Extraction Techniques for Various Seed Oils

INTRODUCTION

Ever since Man took over at the helm of "science", oil has played a

truly remarkable and overwhelming role. In the midst of the civilization upheaval

the share of oil, from various sources, extended to lightening, food, machineries and

cosmetics and medicinal fields.

The study, research and application of oil as a medicine have been a

part of ' Ayurveda' - the Indian version of natural medicine science. Ayurvedic oils

have had a history of over thousands of years.

There are many sources of oil; one such source is seeds from the

plants. The oils present in seeds amounting less than 20% are termed as essential

oils. Ayurveda has greatly used essential oils for medicinal purposes.

Ayurveda and chemical engineering both have their own methods for

extraction of oil. These methods are both conventional and modern.

Ancient Indian Ayurveda adopted methods like oil extraction by

'charkha' (charak yantram) and pulverization. 'Charkha' or charak yantram was

invented by 'Rishi Charakh’, which was employed for extraction of oil for medicinal

purposes. Another methods for oil extraction are by pulverization of the oil seed.

The pulverization was carried out in such a way that the fibers in the seed glands will

not broken and simultaneously oil is extracted. Pulverization employed an oval

shape vessel with sharp end. The seeds were pulverized with the help of a heavy

roller type equipment which was hand operated. The strokes were in harmony with

C.O.E.&T.Akola. 1
 Extraction Techniques for Various Seed Oils

the breath of the person pulverizing the seeds. This method of pulverization

maintains the oscillations and force such that the fibers are not broken.

Another method is oil extraction is “ Decoction ”. Decoction is the

method in which following procedure is followed. Water about 16 lit and oil seed

about 1/4th part of water are boiled together till the water is reduced to 4 liters. This

is followed by treatment with "til oil". It is notable here that the til oil is used as a

solvent. Another advantage of using til oil is that it works as a smoothening agent.

When this mixture is applied to a wound, the til oil would prevent the rashes on the

skin, which would have been formed by using the concerned medicinal oil alone.

Yet another method worth considering is the wet cloth containing oil

seed held over the boiling water in an enclosed vessel. This method resembles way

much to the modern solvent extraction method. The oil seed are held in the wet cloth

above boiling water enclosed in a vessel. The steam rising through the cloth and

condensing back causes the seed to spill the oil, which is collected.

Ayurveda makes the use of oil seed as a whole while chemical

engineering deals which the oil alone. With the advent of modern technology and

availability of equipments, oil extraction has gained major commercial importance.

The oil seed containing more than 20% of oil content may be extracted by direct

crushing. Most of the edible oils are extracted by direct crushing. The solvent

extraction process is widely used now days. The oil seed are held over a perforated

plate or a mesh (depending upon the size of seeds). The solvent present in the same

vessel is boiled and evaporated.

C.O.E.&T.Akola. 2
 Extraction Techniques for Various Seed Oils

These vapors are condensed and made to fall over the oil seeds. The

solvent thus extracts the oil and is also recovered. The process will be described in

detail in further chapters. The main advantage of using solvent is its recovery, which

is about 98%. Another advantage is that the oil extraction from seeds, which is not

possible by crushing, can be mostly extracted by solvent extraction.

Extraction equipments may be broadly classified as crushing

equipments and solvent extractors. Both ancient and modern sciences use their own

equipments for oil extraction. As stated previously the ancient science (Ayurveda)

made use of 'Charak yantram’, which resembles much with the solvent extraction

and the pulverization, which is direct crushing. Also modern Ayurveda uses the

technique of decoction in which the 'til oil' is used as a solvent.

Modern chemical engineering equipments also employ crushers

(hammer mills, ball mills etc). This process extracts oil from seeds or material

having oil content more than 20%. When oil extraction is not possible by simple

crushing then the solvent extractors are employed. Solvent extractors may be

classified as a continuous or batch mode depending on the type of material handled,

oil content and even economic considerations. The oldest and the most widely used

continuous extractors are the 'bucketed' Ballman's extractor and a Rotocell. The

equipments will be described in detail in further chapters.

The batch extractors are of resent origin. Essential oils have a great

value in market and are costlier. The requirement of essential oils is generally low.

Hence batch extractors prove more economical than continuous extractors as only

C.O.E.&T.Akola. 3
 Extraction Techniques for Various Seed Oils

required quantity of material will be handled as per the order undertaken for

production of oil.

Conventional batch extractors, which are employed for Soybean oil

extraction, are available in two sizes 18 x 8.5 feet and 10 x 4.5 feet. Both these

extractors can handle about 10 to 12 and 2 to 4 tons of material respectively. The oil

extracted by these extractors is as good as 1.5 to 15% of the amount of material

handled.

Many essential oils can also be extracted by using these types of batch

extractors. Here we will deal specifically with the extraction and analysis of Bavanja

(Psoralia corilifolia ) oil.

'Bavanja' i.e. Psoralia corilifolia as it is popularly known is about 30-

180 cm high shrub found almost all over India. Unlike tea or coffee it is not

cultivated anywhere but it is reported to be grown in some parts of Rajasthan due to

its medicinal properties.

It contain a sticky pericarp ( c 12.1 of the seed) a hard seed coat and a

kernel.

The oil from Bavanja oil is of great medicinal use. Bavanja oil is

every useful especially in skin cars. Hence Bavanja oil is finding wide applications

in dealing with skin burns. Researches are also being carried out at various

universities all over the world especially for employing Bavanja oils in treatment of

leprosy.

C.O.E.&T.Akola. 4
 Extraction Techniques for Various Seed Oils

Previous work done :

Already some work was done in our college with respect to extraction

of oil from Palmarosa and Ricebran. But for the first time we have installed a regular

soxlets apparatus which very conveniently and accurately determines the oil content

of various seeds. Initially we decided to study the oil production from orange pills,

and various seed shells and kernels. But because of the large amount of raw of

different types. The actual work would have been probably large and such work

already done in ample measures at other places. We decided to take few different

seeds as raw material. We decided to confine or work only to bavanchi, bitter

almond, nagarmotha and soybean. We found out the oil content in these seeds with

the help of soxlets apparatus. The analysis of oil was also carried out. As such we are

not aware whether any attempt has been previously done, but we thought it to link

ancient Ayurveda and chemical engineering. This may be considered as special

feature of this project.

We are thankful to Dr. Yaddaiya of Akola and Dr. Jyotshi of Nagpur

for helping in the venture. We are also thankful to Dr. Somani of P.K.V., Akola who

guided us in finding the previous work done in P.K.V. regarding our topic.

Though this is a team work one of us Mr. Pankaj Solanki who is an

expert in web designing has already put this project work on the web.

We are sufficiently satisfied that we have taken oil extraction with

new angle.

C.O.E.&T.Akola. 5
 Extraction Techniques for Various Seed Oils

HISTORY OF ESSENTIAL OILS

Essential oils were mankind's first medicine. From Egyptian

hieroglyphics and Chinese manuscripts, we know that priests and physicians have

been using essential oils for thousands of years. In Egypt, essential oils were used in

the embalming process and well preserved oils were found in alabaster jars in King

Tut's tomb. Egyptian temples were dedicated to the production and blending of the

oils and recipes were recorded on the walls in hieroglyphics. There are 188

references to oils in the Bible. Some precious oils, such as frankincense, myrrh,

galbanum, rosemary, hyssop, cassia, cinnamon and spikenard, were used for the

anointing and healing of the sick. Additionally, biblical prophets recognized the use

of essential oils as a protection for their bodies against the ravages of disease.

"And when they were come into the house, they saw the young child

with Mary his mother, and fell down, and worshipped him; and when

they had opened their treasures, they presented unto him gifts; gold,

and frankincense, and myrrh". St. Matthew 2:11

During the Medieval plagues in Europe, it was discovered that thieves

were robbing the dying and the dead and not becoming infected themselves. When

asked their secret, they said they were perfumers and spice traders. Before coming in

contact with the diseased bodies, they rubbed themselves down with essential oils,

such as cinnamon, clove and oregano to avoid infection.

C.O.E.&T.Akola. 6
 Extraction Techniques for Various Seed Oils

High Grade v/s Low Grade Oils

There are three grades of essential oils: Grade A, B and C. Over 90%

of the essential oils in this country are of the lower grades. Only Grade A oils carry

frequency, are labeled therapeutic grade, and have the full health benefits

Pure essential oils are expensive. Often one thousand pounds of plant

are needed to produce one pound of essence. When purchasing

essential oils, it is important to take note of their purity, quality, and

price. While pure, natural essential oils may seem expensive, small

amounts go far, making them cost-effective

Therapeutic grade oils have the highest electrical vibration on the

planet that can be ingested and carried throughout our body. When these oils enter

our bloodstream, which they do easily, both the chemicals and the vibration are

carried to all the cells of the body.

Their oxygenating molecules effectively transport nutrients to the

cells of the body. A nutritional deficiency in the body is often caused by an oxygen

deficiency. Therefore, the oxygenating molecules in the oils can help the body

receive and assimilate nutrients to maintain health.

Vibrations Frequencies and Health

We create our reality from energy we call thought, belief and emotion.

We are comprised of electro-magnetic energy; this energy has a vibrational

C.O.E.&T.Akola. 7
 Extraction Techniques for Various Seed Oils

frequency that attracts similar frequency. We change our reality by taking

responsibility and changing our thoughts and feelings to reflect that which we seek to

attract. By working with high vibrational plant essences, being clear in our intentions

and thoughts, we are better able to attract those conditions that resonate with higher

frequency.

Those of us putting high frequency essential oils into our bloodstream

are finding that our overall emotional, mental and physical frequency resonates at a

higher vibratory level, which then attracts energy that facilitates healing and

strengthens our resolve in the process of personal evolution.

These plant essences are formulated to facilitate deep emotional

release, help us be more receptive to communication and connection with Source,

help clear obstacles that prevent us from moving toward our life's purpose and

enhance our passion for life. The oils work synergistically with spiritual and healing

practices such as massage therapy, reiki, acupressure, acupuncture, light body

activation, shamanic work, and cellular level release work.

C.O.E.&T.Akola. 8
 Extraction Techniques for Various Seed Oils

OILS IN AYURVEDA

Man is the only clever living being that knows how to adapt to the

changing environment of time and space. That genius of him has given to him the

supreme position in the world and enabled him to make progress and utilize all the

new achievement of science in the interest of himself and humanity.

During the oral era of Education (Vedic period), the man compiled

sutra-styled encyclopedic treatises mostly in simple, rhythmic poetry. Oral

transmission was the only method for education at that period and this style being

convenient to memorize was accepted.

During the manuscript era, the man tried to dilate or abridge,

comment or criticize, expound or extract, as writing has been of some help to spread

the knowledge and relieve the extra-ordinary burden of memorizing the totality of

knowledge.

With the advent of printing process, the man gets a powerful means of

expression of his thoughts, ideas and experiences to his full satisfaction. He

becomes relieved of memorizing strain, and science has so enabled him today that he

can print not only the word but record its sound rhythm, style and even passion with

which it is uttered.

With these progressive achievements in the sphere of verbal

knowledge on one side and in the change of concept of generalization and all-round

distribution of medical knowledge on the other side, it is bin natural that there will

C.O.E.&T.Akola. 9
 Extraction Techniques for Various Seed Oils

arise a need for simplifying modification in the writing of medical literature so that

people of various grades of intelligence may have full benefit of this knowledge.

A glance is the history of Ayurveda confirms this process of

modulation of compilation of medical knowledge to suit the existing circumstances.

Medical knowledge began with scattered references in the Vedas. Then there was

compiled Ayurvedic Samhita as a comprehensive tretise on the science of life. It is

said to be a systematized compilation divided in 1000 chapters. Each chapter

containing 100 verses, thus making one hundred thousand verses in all.

bg [kYok;qosZnh

ukeksikaxe/koZosnLFkktqRikpSo iztk%]

Üyksd’krlg[ke/;k;lg[ka p d`rokULopaHkw%A

‘This science known as Ayurveda is a branch of Atharvaveda. The

self-created Brahma before creating men, first formulated this science of life

consisting of a hundred thousand verses and a thousand chapters.

Then came the creation of scientific encyclopaedic treatise divided in

eight branches viz., Charaka Samhita and Sushruta Samhita. This was the creator’s

Age. Vagbhata later on compiled a concise book taking the fundamentals of the

above two books, adding the new knowledge and making the book to suit the time

¼;qxkuq:i½ and be the cream of knowledge of the disease and drugs of the

whole universe ¼foÜoO;k/;kSf/kKkulkj%½- This was the transmuter’s

Age.

C.O.E.&T.Akola. 10
 Extraction Techniques for Various Seed Oils

Then the separate books on various branches of medicine were

compiled viz Madhav-Nidan, Sharangadhar-Samhita; and the last encyclopedic book

Bhav-Prakash was published in the sixteenth century. This was the transmitter’s

Age.

Vagbhats, Madhava, Sharogadhars, Bhavamisra and all other authors

of these periods adopt the method of collecting all the existing literature, extracting

the useful parts and compiling them in a simple classified form.

It is classified in eight different Branches known as ‘Ashtanga

Ayurved’

RkL;k;qosZnL;kM~xkU;IVkS ] r|Fkk

dk;fpfdRlk ] 'kkykd;a ]

'ky;kigr`Zda fo"kxjoSjksf/kdiz’keua ] Hkwrfo|

k]

dkSekjHk`R;da ] jlk;ua] okthdjxfefr AA

pjd lq=LFkku 30A28

Kayachikitsa, Shalakya, shalya, Agadtantra, Mantra, Kaumarbhritya,

Rasayan and Vajikaran are the Ashtanga of Ayurveda. All the Ayurved knowledge is

found in these Ashtang. According to time the Ayurved knowledge increases and so

Ashtanga Ayurved is divided into subclasses (Pravibhaga) like Ras-shastra, Baishjya-

kalpana, strirog vigyana and Prasuti-Tantra etc.

C.O.E.&T.Akola. 11
 Extraction Techniques for Various Seed Oils

In Ras-shastra and Baishjya-Kalpana mainly different Ayurvedic

Medicinal preparation process and their uses in different disease can be described. In

Ras-shastra oil extraction process (Tail-Nishkasan Padhati) can be described in

detailed by using ‘Patalyantra’.

gLrizek.ka fuEua p xrZa d`Rok iz;Rur%A

rfLeu~ Hkka.M p laFkkI; rFkkU;r~

ik=ekgjsr~

rfLeUUkkS"kf/k oxZa p nRok·U;a p 'kjkode~A

eq[ks laLFkkI; fNnzkf.k d`Rok pSo 'kjkodsAA

'kjkolfgra ik=a xrZLFks Hkktus U;lsr~A

laf/kysia rr% d`Rok xrZekiw;Ze`Rlu;ksAA

i'pknfXau p izTokY; LokM~++x'khra

leq)jsr~A

i'pkr~ rr~ ik=e/;LFka ik=a ;qDR;k

lekgjsr~AA

rnarLFka p rr~ rSya x`g~.kh;kr~

fof/kiwoZde~A

C.O.E.&T.Akola. 12
 Extraction Techniques for Various Seed Oils

ikrkyk[;a bna ;a=a Hkkf"kra 'kaHkquk

Lo;e~AA

& jlpaMk'kq ] iwoZ[kaM

610 rs 614

& jlizdk'k lq/kkdj ] v/;k; 10

Dig one hand depth ( Hastapramanam ) pit in ground and placed one

'Mritapatra' in it ( Mritapatra is the special type of soil pot ). At the upper end of this

Mritpatra the other Mritpatra having porous ( Sachhidra ) bottom can be placed. In

this Mritpatra the seeds from that oil can be extracted is kept. Then the joint of two

Mritpatra means the upper end of lower Mritpatra and bottom of upper Mritpatra can

be packed with 'Matkapad' (Matkapad is the special packing process in Ayurveda) on

the upper end of upper Mritpatra inverted 'Sharaw' is placed. The joint of sharaw

and Mritpatra packed with matkapad on the sharaw 'Ranshenya' put and burn it.

From the heat of burning Ranshenya oil extracted from the seeds like

seeds of Bakuchi and collect it in the lower Mritpatra through the porous to present

at the bottom of upper Mritpatra.

To avoid the heat loss during the process the both Mritpatra is placed

underground and source of heat is placed on the ground. So the Yantra used for the

process is known as ' patal yantra'.

Oil extracted in Ayurveda by using this process. In this process

without using any solvent only by heat oil can be extracted.

C.O.E.&T.Akola. 13
 Extraction Techniques for Various Seed Oils

In chemical Engineering oil extracted from seeds by using solvent

like Hexan. In this process the chemical reaction may takes place in between hexan

and the seeds under the influence of heat and oil can be extracted. As the way of

solvent there may be chances of changing in the original property of seeds and its oil

extract.

While oil extraction process of Ayurveda solvent can not be used. Oil

extracted directly from the seeds under the influence of heat. As the solvent can not

be used the property of oil is same as the original property of seeds. In some time

solvent like Til-tail is used. By wing til-tail also the property can not be changed.

Adaspatan Yantra -

vFkks/oZHkktus fyIrLFkkfirL; tys lq/kh%A

nhIrSoZuksiyS% dq;kZn/k%ikra iz;Rura%AA

& j- j- l- v- 9&9

In this procedure the two Ghata ( Soil pot ) is taken as shown in

diagram. In the upper Ghata substance placed at the bottom and at the lower Ghata

water can be taken. On the upper ghata Ranshenya put and burn it. By this heat the

steam of medicinal substance is collected at the bottom of water.

Tiryaka patan Yantra

f{kisnzla ?kVs nh?ksZ urk/kksuky la;qrsA

rUukya fuf{kisnU;?kV dq{;Urjs [kyqAA

r= #/ok e`nk lE;Xonus ?kV;ksjFkA

C.O.E.&T.Akola. 14
 Extraction Techniques for Various Seed Oils

v/kLrknzldqEHkL; Toky;s&rhozikode~AA

brjkfLeU?kVs rks;a izf{kisRLoknq 'khrye~A

fr;Zd~ikruesrf) okfrZdSjfHk/kh;rsAA & j- j-

l- v- 9&10 rs 12

In this type of Yantra two ghata is placed as shown in diagram.

Medicinal substance from that Arka ( extract ) is want is kept in bigger size of ghata

and heat it the steam of medicinal substance is collected in small ghata having

through a tube. Small ghata is placed in water bath.

Valuka Yantra

ljlka xw<oD=ka e`}L=kM~‐xqy?kuko`rke~A

'kksf"krka dkpdy'kha f="kq Hkkxs"kq

iwj;sr~AA

Hkk.Ms forfLrxEHkhjs okyqdklqizfrf"Brke~A

rn~Hkk.Ma iwj;s f=fHkjU;kfHkjoxq.B;sr~AA

Hkk.MoD=a ekf.kd;k laf/ka fyEisUe`nk

ipsr~A

pqYY;ka r`.kL; pknkgkUef.kdk i`"BofrZu%A

,rf) okyqdk;U=a r|U=a yo.kkJ;e~A

iTpk<okyqdkiw.kZaHkk.Ms fuf{kI; ;Rur%A

C.O.E.&T.Akola. 15
 Extraction Techniques for Various Seed Oils

iP;rs jlxksykFkZ okyqdk;U=ehfjre~AA

& j- j- l- v- 9 & 36 rs 39

In this type Mritpatra ( Soil pot ) as shown in fig. is kept this

Mritpatra is fill up with sand. At the centre of this Mritpatra a glass bottle with

medicinal substance is kept. The 3/4th portion of this bottle is placed empty. Then

this Mritpatra heat. After slow heating medicine can be prepared.

C.O.E.&T.Akola. 16
 Extraction Techniques for Various Seed Oils

BAVANCHI THEORY AND MEDICINAL

PROPERTIES

PSORALEA Linn. (Leguminosoe; Paptlionaceae)

A large genus of herbs, shrubs or under shrubs is distributed in

tropical and sub-tropical regions of the world. Four species are found in India of

which one is exotic.

P. corylifolia Linn.

D.E.P.,VI (1),353;111 418; FI. Br. Ind.' II, 103' Kirt of Basu, PI.300A

Sans :- Bakuchi , Kushthanashini , Sugandhaleantale ,

Hindi :- Babchi , bavanchi , bulechi ;

Bengali :- Bavachi , koleuch , Latakasturi ;

Marathi :- Babachi , bavchi ;

Gujarathi :- Babchi , bavchi ;

Telgu :- Baavanchalu, bapunga, bawuchee ;

Tamil :- Kaarboka arisi , karporgam ;

Kannad :- Bavanchigida , karbelehiga ;

Malyyalam :- Karpokkari , Kaurleoalari ;

Oriya :- Bakuchi.

An erect annual, 30-180 cm. high , found almost throughout India.

Leaves broadly - elliptic , incisodentate ; flowers yellow or bluish purple , in dense

C.O.E.&T.Akola. 17
 Extraction Techniques for Various Seed Oils

auxiliary , long - peduncled heads ; pods small , 35 - 4.5 mn x 2.0 - 3.0 mm , avoid

oblong , somewhat compressed, mucronate, dark chocolate to almost block ; seed

one , smooth , adhering to the pericarp.

P. corylifolia is not cultivated on a commercial scale anywhere . It is

reported to be grown to somewhat extent in Rajasthan and the eastern districts of

Punjab adjoining Uttar Pardesh for its seeds Seeds of good quality are produced in

Rajasthan. The plant grows on any average soil. Seed is sown in March - April in

lires, 30 cm. apart , at the rate of 7 kg / hectare. The plant flowers during rains and

seeds mature in November. Under proper care, the plants may continue to grow for

5-7 years ( Luthra Suri , Spec. Bull., Dep. Agric. Punjab , 1936 , 14 ; Luthra , Indian

Fmg , 1950 , 11 , 10 ; Chopra , 1958 , 391 ; Biswas , J. Asiat. Soc. Sci., 1956-57 , 22

, 61 ).

The fruits (seeds) of P. coryifolia consist of a sticky aily pericarp

( c.12% of the seed) , a hard seed coat and kernel. They are odoucess , but on

chewing they emit a pungent odour , and have a bitler , unpleasand and acrid taste.

The seeds contain on essential oil (0.05%), a non-volofile trepenoid oil , a dark

brown resin (8.61) a Pignent (probably a hydrony flavore ) , a monoterpenoid phend

named bakuchial ( C181+240 , b.p/0.7 mm. 145 - 47), a brown fixed oil ( c.10%)

roffinose , and coumarin compounds. viz. psoralen (identical with ficusin ; CuHsO3 ,

m.p. 161 - 620). Isopsoralen ( identical with orgelicin ; mp. 141-42) psoralidin ( C16,

H14 04. m.p. 3150 decomp.) ,isopsoralidin (C16. H14 04. m.p. 283 - 840), and corylifolin

( C17 H18 O3, mp. 1830 ). Later investigations indicated formula of psoralidin to be

C.O.E.&T.Akola. 18
 Extraction Techniques for Various Seed Oils

C20 H10 O3 ( m.p. 290-920 decomp). Fixed oil of the seeds is viscous , bitter in taste

and on keeping deposits psoralen. It contains considerable resin acids (21.5%) ,

stignastered is present in the unsoponifiable matter ( Seshadri Venkatarao, Proc.

Indian Acad. Sci 1937 , 5A , 351 ; I.P.C., 209; Chopra Chotterjee Indian J. med. Res,

1927-28 , 15 ; 49 ; Mehta etal : Tetrahedron Lett., 1966 456 t : Jais et al., J. Indian

chem. Soc., 1933, 10, 4.1 ; Bhattacherji , J. sci , industry Res., 1961 , 20 B , 135 ;

Chakravarti et al , ibid. 1948, 7B , 24 ; Chem. Abstr., 1936 , 30 , 4855 , 7575;

Dattagupta et al, Chem Ind., 1960, 48 ; Siddappa Devi , Boc. Indian Sci , Congr. ,

1957 , pt.III.130 , 1956 , pt III , 126 ; Khastgir et al., Indian J. appl. Chem, 1959, 22 ,

35 ).

The seeds are used in indigenous medicine a lanative, aphrodisiac ,

anthelmintic , diuretic and diphoretic in febrile conditions. They have been specially

recommended in the treatment of leucoderma leprosy , psoriasis and inflammatory

diseases of the skin , and are prescribed both for oral administration and for local

external application in the form of a paste or oinment. The use of seed in the

treatment of leprosy has been more or less abondoned [ Chaopra, 1958 , 391 ;

Mukerji , J. Sci. industr. Res., 1956 , 15A (5) , Suppl., I ].

Extensive clinical trials carried out in India have shown that the seed

and their various preparations are useful in the treatment of leucoderma of non -

syphilitic origin. Psoralen and isopsoralen are considered the theropentically active

constituents of the seeds. The drug appears to have a purely local action, with a

specific effect on the asterioles of the sub-capillary plenuses which are dilated so that

C.O.E.&T.Akola. 19
 Extraction Techniques for Various Seed Oils

plasma is increased in this area. The skin becomes red and the melonoblasts

( pigment - forming cells ) are stimulated. In leucoderma , melonoblasts do not

function properly and their stimulation by the drug leads them to form and exude

pigments which gradually diffuse into the white leucodermic patches. The treatment

by this drug has not been effective in the leucoderma syphilitic group , because in

such uses, in a probability melanoblasts are Lilled, for they are not visible in

histological preparations [ Chapra , 1958. 191-95 ; Mukerji Bhandari , East. Pharm.

1959 , 1 (30), 29 ].

A number of preparations made from the seeds have been tried in

numerous cases of leucoderma and other skin diseases. Oral administration of the

powdered seeds to the patients has generally resulted in side reactions such as

nausea, vomiting , mabisa , headache and sometime , purging. External application

of the essential oil preparations generally proved to be highly irritent to the skin

causing sensitiveness and even blistering. Intraderma injection of the oil , though

effective , was normally accompanied by severe pain with tendency to ulceration.

Local application of the oleoresinous extrat of the seeds has been recommended as a

more suitable preparation. The extract is official in Indian Pharmacopocia as Babchi

Ointment or Application of Psoralea. The strength of the oil or oleoresin

preparations should be so adjusted as not to allow its action to go beyond the state of

redness of the leucodermic patches. The use of these preparations has, however, not

resulted in permanent cure ; there has been even total failure in some cases ( Chopra ,

C.O.E.&T.Akola. 20
 Extraction Techniques for Various Seed Oils

1958 , 391 - 95 ; Mukarji , loc. cit ; I. P. , 60 ; Panja Maplestone , Indian med. Gaz.,

1940, 75 , 93 ).

Trials with the active principles , psoralen and isopsoralen mixture ,

given orally , have shown that this treatment has some value which is not obtainable

by external application of the oil or by the oleoresinous extract. In trials with

patients aged belao 20 and having leucoderma of recent origin , encouraging results

were obtained with the furocoumosin mixture. External application of a a liquid

preparation made from this mixture was also tried on white patches simultaneously

with oral administration. The patches tended to be covered up gradually and the

initial time of response varied between 10 and 30 days. No fresh patches appeared

during the course of treatment and relapses were few. Process of extraction of

psoralen isopsoralen mixture from seeds have been developed and covered by

patents. The furoconmarias are present in the fresh seeds as glycosides of the

corresponding caumarinic acids and cannot be fully extracted out directly. Soaking

the ground seeds in the water for a few days prior to extraction hydralyses the

glycosides thereby releasing the coumasins. Yields of upto 1 per cent of the mixture

have been obtained psoralen is reported to be more patent than other furocoumarias

such as xanthotoxin and begapten. [Mukerji , loc. cit. ; Mukarji Bhandari , loc cit ;

Khastgir et al , Indian. J. appl. Chem., 1959, 22 , 82 ; Rangaswami of Seshadri.

Indian J. Pharma, 194 3 , 5 , 105 ; Chakravarti et al , loc. cit ; Bhattacharya Dhar ,

Indian. Pat., No : 59265 , 59266 and 61772 , 1957 ; DasGupta , Proc. Indian Sci ,

Congr.; 1962; pt - III , 154 ; Sen J. Sci industr. Res , 1963 , 22 , 88 ).

C.O.E.&T.Akola. 21
 Extraction Techniques for Various Seed Oils

The seed extracts inhibit the growth of staphylocodus citreus, S.

aureus and S. albus including strains resistant to penicillins. A highly potent anti

staphylcoccal fraction has been obtaianed from the seeds. The seed posses

anthemintic activity against earthworms, psoralen being the active principle.

Psoralen is also toxic to fish. The essential oil shows a selective activity against the

skin streptococci and the probably accounts for its use in indigenous has marked

action on Paramaceum ; in a dilution of 1 in 10,000 , streptococci and Paramecia are

killed in 10 minutes. It has a distinct stimulant action an voluntary muscles in high

dilution , upto 1 is 100,000. It increases the tone of the uterus and stimulates the

intestinal smooth muscles of the experimental animals. ( Gupta. et. al , Bull , reg.

Res. Lab : Jammu , 1962 , 1 , 59 ; Gaind et al , Indian J. Pharma., 1964 . 26 , 141 ;

1965 , 27, 198 ; Iyengar & Pendise , ibid., 1962 , 24, 289 ; Chopra , 1958 ; 392 - 93 ).

The seeds are used locally in preparation of certain types of medicated

oils and incense preparations. The root is useful in the caries of teeth. Leaves are

used in diarrhoea. [ Krishna & Badhwar, J. Sci., industr. Res ; 1949 , (2). Suppl : 159

; Cooke, I, 342 ; Kirt & Basu , I , 718 ].

The cake left behind after the removal of the fixed oil is rich in

nitrogen (6.7%) and minerals (7.8%) and is stated to be suitable as a feed or manure (

Seshadri & Venkatarao , loc, cit.).

The plant is eatten by cattle in Bundelkhond. The seeds are reported

to be used as an article of food. The whole plant is a good source of nitrogen for

organic mature. Its manurial value is as follow :

C.O.E.&T.Akola. 22
 Extraction Techniques for Various Seed Oils

( Oven - dry basis ) : Organic matter, 87.77; ash , 11.13 ; nitrogen , 3.69 ; Calcium

(CaO), 3.25 ; potassium (k2O), 1.18 ; and phosphorous (P2O5), 0.96 %.

[ Santapau , Rec , bot. Surv. India, 1953 , 16 , 51 ; Patil , Poona agric, Coll , Mag .,

1960-61 , 51 ( 3 & 4 ), 32 ].

P Plicata Delile ( Punjab - Bakhtmal ) is low , much - branched shurb , 30 - 60

cm., high , with trifolio - late leaves , yellow or pale violet flowers and ellipsoid or

oblong - globose , one seeded pods found in Punjab & Delhi.

Camels are fond of this plant. The leaves contain ; crude protein , 9.4

; other extr, 1.5 ; N - free extr., 41.9 ; crude fible , 40.1 ; mineral matter , 7.2 ;

calcium , 1.9; and phosphorous , 0.2 %. The young pods are reported to yield a

yellow dye.

[ Singh et al Indian J. vet. Sci., 1959 , 29 ( 2 & 3 ), 32 ; F L.Delhi ,

134 ].

The seeds are used in indigenous medicine a lanative, aphrodisiac ,

anthelmintic , diuretic and diphoretic in febrile conditions. They have been specially

recommended in the treatment of leucoderma leprosy , psoriasis and inflammatory

diseases of the skin , and are prescribed both for oral administration and for local

external application in the form of a paste or oinment. The use of seed in the

treatment of leprosy has been more or less abondoned [ Chaopra, 1958 , 391 ;

Mukerji , J. Sci. industr. Res., 1956 , 15A (5) , Suppl., I ].

Extensive clinical trials carried out in India have shown that the seed

and their various preparations are useful in the treatment of leucoderma of non -

C.O.E.&T.Akola. 23
 Extraction Techniques for Various Seed Oils

syphilitic origin. Psoralen and isopsoralen are considered the theropentically active

constituents of the seeds. The drug appears to have a purely local action, with a

specific effect on the asterioles of the sub-capillary plenuses which are dilated so that

plasma is increased in this area. The skin becomes red and the melonoblasts

( pigment - forming cells ) are stimulated. In leucoderma , melonoblasts do not

function properly and their stimulation by the drug leads them to form and exude

pigments which gradually diffuse into the white leucodermic patches. The treatment

by this drug has not been effective in the leucoderma syphilitic group , because in

such uses, in a probability melanoblasts are Lilled, for they are not visible in

histological preparations [ Chapra , 1958. 191-95 ; Mukerji Bhandari , East. Pharm.

1959 , 1 (30), 29 ].

A number of preparations made from the seeds have been tried in

numerous cases of leucoderma and other skin diseases. Oral administration of the

powdered seeds to the patients has generally resulted in side reactions such as

nausea, vomiting , mabisa , headache and sometime , purging. External application

of the essential oil preparations generally proved to be highly irritent to the skin

causing sensitiveness and even blistering. Intraderma injection of the oil , though

effective , was normally accompanied by severe pain with tendency to ulceration.

Local application of the oleoresinous extrat of the seeds has been recommended as a

more suitable preparation. The extract is official in Indian Pharmacopocia as Babchi

Ointment or Application of Psoralea. The strength of the oil or oleoresin

preparations should be so adjusted as not to allow its action to go beyond the state of

C.O.E.&T.Akola. 24
 Extraction Techniques for Various Seed Oils

redness of the leucodermic patches. The use of these preparations has, however, not

resulted in permanent cure ; there has been even total failure in some cases ( Chopra ,

1958 , 391 - 95 ; Mukarji , loc. cit ; I. P. , 60 ; Panja Maplestone , Indian med. Gaz.,

1940, 75 , 93 ).

Trials with the active principles , psoralen and isopsoralen mixture ,

given orally , have shown that this treatment has some value which is not obtainable

by external application of the oil or by the oleoresinous extract. In trials with

patients aged belao 20 and having leucoderma of recent origin , encouraging results

were obtained with the furocoumosin mixture. External application of a a liquid

preparation made from this mixture was also tried on white patches simultaneously

with oral administration. The patches tended to be covered up gradually and the

initial time of response varied between 10 and 30 days. No fresh patches appeared

during the course of treatment and relapses were few. Process of extraction of

psoralen isopsoralen mixture from seeds have been developed and covered by

patents.

The root is useful in the caries of teeth. Leaves are used in diarhoea.

C.O.E.&T.Akola. 25
 Extraction Techniques for Various Seed Oils

EXTRACTION THEORY

Extraction Rates

In practice, the design of large-scale solvent extraction apparatus must

be determined by the rate at which equilibrium is attained between a lean miscella

outside the seed particles and oil and solvent within the particles. The attainment of

equilibrium may be quite slow, particularly as the oil content of the seed (on a dry,

solvent-free basis) falls toward the low level (usually below 1.0%) demanded by

efficient commercial operation. Modern investigations indicate that the rate at which

equilibrium is approached (and hence in effect the extraction rate) is influenced by a

number of factors. These include the intrinsic capacity for diffusion of solvent and

oil, which is determined primarily by the viscosities of the two; the size and shape of

the seed particles; their internal structure; and, at low seed oil levels, the rate at

which the solvent dissolves nonglyceride substances which are oil-soluble but

dissolve less readily than the glyceride portion of the oil.

In a homogeneous oil-impregnated material consisting of thin

platelets of uniform thickness whose total surface area is substantially that of the two

faces, the theoretical extraction rate, based upon simple diffusion, has been given by

Boucher and coworkers (13) as follows:

n =∞
8 1
∑ ( 2n + 1 ) ( π / 2 )2 ( D θ / R 2 )
2
E= e −( 2 n +1 )
π2 n =0
2

C.O.E.&T.Akola. 26
 Extraction Techniques for Various Seed Oils

where E w the fraction of the total oil unextracted at the end of time 0, in

hours; A is one-half the plate thickness, in feet; and D is the diffusion

coefficient, in square feet per hour.

Except at low values of θ, the above equation takes the approximate form (82):

8 2
Dθ / 4 R 2
E= 2
e −π
π

Dθ
or log 10 E = −0.091 − 1.07
R2

Hence, at the lover values of E, a plot of log E against θ gives a

straight line with a slope dependent upon the diffusion coefficient and the plate

thickness. It is to be emphasized that the equation is valid only when all platelets

have the same thickness, and average plate thickness cannot be used for a material of

nonuniform thickness.

Working with porous clay plates impregnated with phosphatide free

soybean oil and with tetrachloroethylene as a solvent, Boucher et al. found that

experimentally determined extraction rates checked closely with theory; a typical

theoretical extraction curve is shown (curve A) in figure. A lack of correspondence

between extraction rates and Reynolds number of the flowing solvent, over a wide

range of the latter, indicated that liquid-film resistance to the transfer of oil to the

solvent was inconsequential as compared to resistance to diffusion within the plates.

The diffusion coefficient was found to be simply a function of the product of the

viscosities of solvent and oil; under the particular conditions of their tests it could be

represented by the formula

C.O.E.&T.Akola. 27
 Extraction Techniques for Various Seed Oils

D = 12.96 × 10 −6 ( µ 0 µ 8 ) −0.46

where µ0, and µ8 refer to the viscosities, in centipoises, of oil and solvent,

respectively.

The numerical values in the formula are undoubtedly related to the

structure of the plates and hence can be considered specific only for the lot of plates

used in the tests. Tests involving extraction with solvent-oil mixtures as well as pure

solvents show that the diffusion coefficient is independent of the composition of the

solvent, in terms of relative proportions of solvent and oil. It can, of course, be

C.O.E.&T.Akola. 28
 Extraction Techniques for Various Seed Oils

expected to increase with increase in temperature or with use of a less viscous

solvent than tetrachloroethylene.

The experiments of Fan and coworkers (82) with peanuts carefully

sliced with a microtome show that the relationships developed by Boucher et al. are

also applicable to at least one oil seed, provided that structural considerations are not

complicated by crushing of the seed to form flakes. A typical extraction curve is

shown as curve B of figure. As required by diffusion theory, there is a linear

relationship between the logarithm of the residual oil content and extraction time

after a short period has elapsed. During this period, however, a large proportion of

the oil is extracted very rapidly.

Fan et al. carried out a mathematical analysis which indicated that this

deviation from theory with respect to rapidly extractable oil was caused by the

opening of a certain number of oil-bearing cells in slicing the oil seeds, plus the

occurrence of void spaces in the seeds after drying. Thus they agreed with Osburn

and Katz (84) that the major obstacle to extraction is probably diffusion through the

cell walls and that the initial rapid extraction is to be attributed to cell destruction.

The proportion of easily extractable oil was found to decrease rapidly with increase

in the slice thickness. In the case of curve B of figure, which represents the

extraction of peanut slices 0.026-inch thick, the extraction curve became linear after

about 76% of the oil was extracted; in other experiments with flakes of similar

moisture content, there was linearity with 0.032-inch flakes after about 51% of the

oil was extracted, and linearity with 0.040-inch flakes after about 30% was extracted.

C.O.E.&T.Akola. 29
 Extraction Techniques for Various Seed Oils

With flakes of constant thickness, there was a progressive decrease in the content of

rapidly extractable oil with increase in the moisture content.

Fan and coworkers found that the diffusion coefficient decreased

considerably with increase in the moisture content (in the range of moisture, about

0.4 square centimeter per second per 1 % moisture). With commercial hexane

(Skellysolve B) at 24-260C. and peanut slices with 13% moisture, the calculated

diffusion coefficients averaged about 7 × 10-9 square centimeter per second.

In the extraction of oil seed flakes formed commercially by rolling,

there appear to be factors which still further complicate the extraction rate.

Extraction curves not only reveal a very large fraction of easily extractable oil, but

tend to be continuously concave upward from the time axis; curve C of figure,

constructed from the laboratory data of Wingard and Shand (83), is typical (compare

also figure ). In practice, extraction in the range of about 5.0-0.5 % residual oil (on

the basis of the dry, solvent-free meal) is so slow that it actually controls the overall

extraction rate and extractor design (10). On a semilog plot, the concavity of the

extraction curve is so great in this region that actually, a nearer approximation to a

straight line is obtained with a log-log plot as in figure.

C.O.E.&T.Akola. 30
 Extraction Techniques for Various Seed Oils

A variety of explanations can be offered for the large deviation of

curve C (figure) from the form of curve A or curve B. It has been pointed out by

King et al. (85), as well as by Osburn and Katz (84), that structural heterogeneity

leading to the simultaneous operation of two different diffusion processes with

different diffusion coefficients could account for the shape of the curves. The

analysis of soybean flake extraction curves by Osburn and Katz suggested that at

80°F., 70-90% of the oil was extracted with trichloroethylene with the relatively high

diffusion coefficient of about 4 × 10-6 square foot per hour, while the remaining

10-30% was extracted with the lower diffusion coefficient of about 4 × l0-6 square

foot per hour. It was further suggested that the larger portion of readily available oil

was derived from cells ruptured in rolling, whereas the smaller portion of difficultly

C.O.E.&T.Akola. 31
 Extraction Techniques for Various Seed Oils

extractable oil was in cells that remained intact. It seems unlikely, however, that

such extensive cell destruction could occur; if lack of structural homogeneity is the

proper explanation, it appears that it is probably of a different kind. Other kinds of

heterogeneity can be conceived, including nonuniformity of flake thickness.

As a result of extensive experimental work on the extraction of oil

seed flakes, Karnofsky and coworkers (10, 86) have advanced the hypothesis that the

slow final extraction rate is at least in part the result of decreased solubility of the

last portions of oil. It is well known that oil seeds subjected to repeated extraction

with a solvent yield fractions of oil toward the end of the process that are much

higher in phosphatides and other nonglyceride materials than the first fractions (10,

87); hence these materials are obviously less soluble. That the difficulty of extracting

the last portions of oil from oil seeds may be related to the chemical composition of

the "oil" was suggested previously by Goss (88). The hypothesis of Karnofsky et al.

is supported by the observation (86) that the last portions of oil are removed much

more readily if the oil seeds are first given a "soaking" period, even in relatively

strong miscella, and that no difficulty is encountered in recovering the last portions

of oil from oil seeds reconstituted from extracted oil and oil-free residue.

Acceptance of the "difficultly soluble oil" theory does not vitiate

many of the basic conclusions to be derived from the above theories based upon

simple diffusion with free miscibility of solvent and oil. If free miscibility does not

exist in the latter stages of extraction, this means simply that the effective

concentration of solute is not the concentration of "oil" in the solid seed material but

C.O.E.&T.Akola. 32
 Extraction Techniques for Various Seed Oils

a lower concentration which is limited by the solubility of the "oil" in the solvent.

The rate of diffusion will be less than observed in the earlier stages, not because the

diffusion coefficient has decreased, but because the "oil" content of the solid material

is no longer a proper measure of its instantaneous content of diffusible material. The

diffusion or extraction rate will, for example, still be inversely proportional to the,

square of the flake thickness.

It may be noted that with simple diffusion an increase in the

extraction temperature can be expected to increase the extraction rate by lowering

the viscosities of solvent and oil, but that with incomplete solubility of the oil an

additional effect can be anticipated through an increase in the solubility. This may

account for the great effect of temperature observed by Karnofsky (10); in one case

increasing the temperature from 1000F to 1920F reduced by 80% the time required to

lower the oil content of cottonseed flakes to 3% with heptane. This is rather greater

effect than would be predicted from a simple decrease in viscosity, according to the

data of Boucher et al. (13).

According to Wingard and Phillips (89), the time required to reduce

oil seeds to 1% residual oil content varies with a power of the temperature which,

with cottonseed, soybean, and flaxseed flakes and hexane as a solvent, ranges from –

1.9 to –2.4. Hence a plot of log time versus log temperature yields a straight line.

It is evident in commercial practice, and has been confirmed by

closely controlled laboratory experiments, that different oil seeds differ markedly in

the rate at which flakes of a given thickness can be extracted to a low residual oil

C.O.E.&T.Akola. 33
 Extraction Techniques for Various Seed Oils

content. The relation of particle size oil seed to extraction rate has been clarified by a

laboratory investigation reported by Coats and Wingard (90), who found that the

hexane extraction of soyabeans, cottonseed, flaxseed, and peanuts, as either flaxes or

cracked particles (grits), confirmed to the mathematical formula

T = KDn

Where T= time to reduce the material to a residual oil content of 1.0% (on a

dry, solvent-free basis), D = flake thickness or grit diameter, and K and n are

constants.

Consequently, a plot of T against D on a log-log scale yields a straight

line, with a slope equal to n. Approximate values found for n were, for four samples

of soybean flakes, 2.3 to 2.5; for two samples of cottonseed flakes, 1.5; for one

sample of flaxseed flakes, 7; for one sample of peanut flakes, 3.2; for two samples of

soybean grits, 5.5; for one sample of cottonseed grits, 4; and for one sample of corn

germ grits, 3.4. With T expressed in minutes and D expressed in units of 0.010 inch

each, approximate values for K were, for soybean flakes, 6 to 20; for cottonseed

flakes, 140 and 270; for flaxseed flakes, 3600; for peanut flakes, 1.4; for soyabean

grits, 2.5 and 10; for cottonseed grits, 40; and for corn germ grits, 1.6.

C.O.E.&T.Akola. 34
 Extraction Techniques for Various Seed Oils

Note that K in the above equation is a measure of the case of

extraction (of flakes 0.010-inch thick), whereas n is a measure of the influence of

flake thickness upon the extraction rate. Thus soybean flakes extract more readily

than cottonseed flakes of equivalent thickness, and cottonseed flakes, in turn, extract

more readily than flaxseed flakes (figure). The extraction rate of flaxseed is highly

sensitive to flake or particle thickness, whereas that of soybeans is less so, and

cottonseed are less sensitive to flake thickness than either. Soybean grits of a given

diameter extract more easily than flakes of equivalent thickness, but their extraction

rate is more dependent upon their thickness. The value of n for soybean flakes was

found to be substantially the same for different lots of beans of varying moisture

C.O.E.&T.Akola. 35
 Extraction Techniques for Various Seed Oils

content flaked by different methods, and that the data of King et al. (85) obtained by

trichloroethylene extraction indicated a value for n exactly in line with the results

with hexane, as well as a comparable value for K.

There is evidence (85) that large seed particles rolled to form flakes of

a definite thickness can be extracted more rapidly than small particles, presumably

because they undergo greater internal disruption in the rolling process.

Recently, laboratory and pilot plant work on soybeans by Othmer and

Agarwal (91) has led them to conclude that for hexane extraction of soybeans:

1. The oil extracted, the residual oil, and the rate of extraction are all independent of

the concentration of oil in the solvent; that is, there can be no advantage in

countercurrent extraction.

2. The rate of extraction is proportional to

(a) Residual oil3.5

(b) Flake thickness-3.97; that is, increasing flake thickness by 3 times deceases rate

by 80 times.

Commercial application of point 1 is seen in the "filtration extraction"

process for cottonseed (92) in which a slurry of cooked cottonseed flakes and

miscella is held for a time before the rich miscella is washed off on a continuous

horizontal filter.

A later paper by Othmer and Jaatinen (93) extends their work to other

solvents and shows that solvents other than hexane and acetone do not extract at a

rate independent of miscella concentration.

C.O.E.&T.Akola. 36
 Extraction Techniques for Various Seed Oils

Any review of the literature on extraction uncovers several

inconsistencies and contradictions, which are largely due to the experimental

techniques used. Results obtained under one method may not be obtained under

another, and consequently the conclusions will differ, although each may be

consistent with the data on which it was based. Some investigators mix solvent or

miscella with flaked oil seeds under conditions of good agitation, while others

believe that a percolation-type extraction more closely parallels commercial plant

conditions. Some use pure solvent and others use a combination of miscellas, such as

would be used in the plant. Some prefer to calculate the residual oil content of the

extracted material from the enrichment of the miscella, rather than separate and

analyze the extracted solids. Some consider solvent extraction as consisting of two

parts: extraction proper and washing, washing being considered rather

inconsequential, with primary emphasis on the attainment of equilibrium between oil

seed flakes and miscella. However, efficient washing is a requirement in a

commercial plant, and if washing time is unduly long, it increases the total time the

flakes are in the extractor just the same as if more time were needed for extraction

proper. Future researchers might well consider solvent extraction as including

everything that happens between &e time oil seed flakes are contacted by miscella or

solvent and the time they enter the enter the solvent removal equipment. It would

also seem that actual analysis of spent flakes is to be preferred to any calculations of

what the oil content would be if the flakes were removed from the system and

washed instantaneously.

C.O.E.&T.Akola. 37
 Extraction Techniques for Various Seed Oils

EXTRACTION STANDARDS

Chiefly from experience with soybeans, it is accepted that commercial

solvent extraction must reduce the oil content of the dry solid residue to less than

1.0%, and preferably to about 0.5%, to be efficient. In making guarantees on soybean

extraction equipment, manufacturers usually specify that the analysis be made on

extracted flakes before toasting, since it is generally acknowledged that there is an

increase in the apparent "oil" content (petroleum ether-soluble material) during

toasting. Moreover, since appreciable toasting takes place during the removal of

solvent from extracted flakes- in desolventizer-toasters, the analysis should

preferably be made on spent flakes which have been desolventized without the use of

steam or heat. Unfortunately, this is seldom practical from a safety standpoint; thus

meal analysis is usually relied upon.

In any given installation the objective is usually to reduce the oil in

meal to the lowest possible level; in actual practice this is probably desirable.

However, published evidence shows that the last portions of "oil" (or petroleum

ether-soluble material) in the meal are largely not oil at all but phosphatides and

other nonglyceride impurities. Bull and Hopper (87) have reported a phosphatide

content of 18.62% in the last 1.1% of material extracted from a sample of soybean

flakes with commercial hexane at 40°C. Similarly, Karnofsky (10) has reported that

a similar fraction had a refining loss of 81.5%. More research is needed on the

quality of the total oil extracted versus the degree of extraction.

C.O.E.&T.Akola. 38
 Extraction Techniques for Various Seed Oils

SOLVENTS FOR OIL EXTRACTION

The most common solvents used in the United states for oil and fat

extraction are light paraffinic petroleum fractions. The more popular products are

cuts of fairly narrow boiling range, which are distinguished according to the chain

length of their principal components. One manufacturer lists the following general

ASTM boiling ranges for four types of naphtha: pentane type, 88-97°F.; hexane type,

146-156oF.; heptane type, 194-210°F.; octane type, 215-264o F.; octane type, 215-

264oF. (94). The hexane-type naphtha is the most widely used and the one generally

preferred for oil-seed extraction, although the heptane-type product is also suitable

for use in most modern plants. The pentane type finds limited use in the extraction

of heat-labile products such as pharmaceuticals; the higher-boiling products are

required for the extraction of castor oil, which is not freely miscible with

hydrocarbons except at elevated temperatures.

In Europe, where cyclic hydrocarbons are more commonly available,

the preferred extraction naphtha in the past has been a product consisting

predominantly of cyclohexane, which has a boiling range of about 160-185o F.

A preliminary laboratory study of a number of pure hydrocarbons

with respect to their all-around desirability as solvents for the extraction of

cottonseed has been published by Ayers and Dooley (95), who consider paraffinic

hydrocarbons preferable to cyclic hydrocarbons and find methylpentanes the best of

C.O.E.&T.Akola. 39
 Extraction Techniques for Various Seed Oils

the former group. A commercially available methylpentane type naphtha is listed as

having a typical boiling range of l39-145°F.

Although solvent losses in American plants employing hexanes for

extraction are higher than in European plants using a higher-boiling product, they »re

not excessive and in well-operated soybean extraction plants do not exceed about 2

gallons for each ton of seed processed. At this rate, charges for solvent loss are less

than for labor, power, or steam (75). :

The American-produced extraction naphthas are substantially free

from nitrogen- or sulfur-containing compounds and unsaturated hydrocarbons and

leave a residue upon evaporation of teas than 0.0016%. They are sufficiently stable

to be reused indefinitely, cheap, and available in practically unlimited quantities.

The only serious is advantage to their use is their extreme flammability. Rather

elaborate precautions are required to avoid fire or explosion hazard in the plants in

which they are used. The proper safety measures have been discussed in detail by

Bonotto (96), MacGee (94, 97), and others (98).

The history, composition, and characteristics of American extraction

naphthas have been reviewed by MacGee (94, 97, 99). Detailed analyses of a popular

hexane product have been published by Griswold and coworkers (100) and by

MacGee (99).

Because of the potential fire and explosion hazard involved when

hydrocarbon solvents are used for extraction, there has always been a great deal of

interest in nonflammable solvents. Trichloroethylene, boiling at 188o F., is such a

C.O.E.&T.Akola. 40
 Extraction Techniques for Various Seed Oils

solvent (101, 102). During World War II it was used in one large extraction plant in

England because of its safety, and it is still used there today. In the United States,

however, its use has been confined to a few small soybean extraction plants.

Originally, it was thought that the use of a nonflammable solvent like

trichloroethylene would result in less danger of fire, less need for skilled labor, and

lower initial investment cost. Experience has shown, however, that:

1. Although safe from a fire and explosion standpoint, the toxicity the solvent

requires that it be handled carefully;

2. Its relatively high cost is not counterbalanced by proportionately lower solvent

losses;

3. Corrosion is a serious problem despite attempts at stabilization;

4. Oil produced must be exhaustively stripped of solvent, since small amounts of

residual solvent will interfere with subsequent hydrogenation of the oil unless special

precautions are taken (103), and this requires skilled labor; and

5. The solvent reacts with soybeans in some manner still not completely understood,

despite considerable investigations (104), producing a soybean meal which is toxic

to cattle. As a result of this, all commercial production of trichloroethylene-extracted

soybean meal in the United States has been halted.

At one time carbon disulfide was widely used in Europe for the

extraction of olive press cake, to recover the inedible product termed olive oil "foots"

or "sulfur olive oil." However, carbon disulfide is not a desirable solvent, it has

never been used in the United States, and in Europe its use is rapidly declining in

C.O.E.&T.Akola. 41
 Extraction Techniques for Various Seed Oils

favor of petroleum naphthas which yield an edible extract. Acetone has been used to

some extent for the recovery of oil from wet materials, such as fish livers, as has also

ethyl ether (79).

Interesting recent laboratory developments include oil seed extraction

processes employing isopropyl alcohol (105-107), and ethyl alcohol (108-110) as

solvents. The former, unlike petroleum naphthas, effectively extracts gossypol from

cottonseed and thus offers a possible means of detoxifying the residue from this seed

without the necessity for severe heat treatment. However, the miscella must be

purified of phosphatides, carbohydrates,, and other nonglyceride extractives if it is

to yield a crude oil of low refining loss and good refined color. When cooled

moderately, alcohol miscellas separate into two layers consisting principally of oil

and of solvent; hence, with such a solvent; equipment and steam for the evaporation

and recovery of solvent may be greatly reduced.

Eaves et al. (111) have investigated the extraction of cottonseed by

five commercial solvents (hexane, benzene, ethyl ether, acetone, and butanone) and

concluded that none compared favorably with hexane as an extractant for cottonseed.

A combination of solvent extraction acetone and miscella refining has been described

by Vaccarino (112).

EXTRACTION EQUIPMENTS

TYPES OF EXTRACTOR

Batteries of batch extractors are still in use in Europe for the recovery

of oil from oil seeds or mechanical press residues. In modern plants, however, batch

C.O.E.&T.Akola. 42
 Extraction Techniques for Various Seed Oils

equipment is used principally in the form of small units for the recovery of

pharmaceutical oils or other expensive oils; for the extraction of spent bleaching

earth; for the processing of meat scraps, cracklings, and garbage; or for other

purposes where the tonnage of material handled does not justify the expense of

installing continuous extractors. The largest single use of batch extractors in the

United States at the present time is probably for the processing of castor pomace

remaining from the cold-cage pressing of castor beans.

Batch extractors vary greatly in design. An extractor which is popular

in the castor oil industry consists of a large horizontal drum (18 by 8.5 ft.) mounted

on rollers by means of which the drum can be rotated on its longitudinal axis. Inside

the drum is a horizontal, perforated, metal strainer covered with a filter mat of

burlap, which extends the length of the drum and divides it into two compartments,

one much smaller than the other. The large compartment receives a charge of 10 to

12 tons of solid material through which solvent is percolated to drain into the smaller

compartment by gravity, from which it is continuously pumped during the drainage

period. Four to six successive extractions suffice to reduce the oil content of castor

pomace from about 15% to 1.5%. A common European extractor, somewhat similar,

but of a stationary vertical design with internal mixing arms, has been described by

Goss (88).

C.O.E.&T.Akola. 43
 Extraction Techniques for Various Seed Oils

The extractor commonly used for the extraction of garbage consists of

a vertical cylindrical kettle, with a large ratio of diameter to depth, equipped with a

vapor-tight cover, a steam jacket, and a vertical low speed agitator. The most

popular unit is about 4 ½ feet high and 10 feet in diameter, and takes a charge of 3 to

C.O.E.&T.Akola. 44
 Extraction Techniques for Various Seed Oils

5 tons of material. This extractor is suitable also for the extraction of other relatively

wet materials, as the material may be dried and extracted in the same vessel.

Solvent systems are used to some extent for the extraction of fish liver

oils, as well as fish oil (3, 4). A number of other types of batch extractor have been

described (113). The extraction of miscellaneous oil-containing materials, as well as

oil seeds, has been developed to a much higher degree in Europe than in the United

States.

CONTINUOUS EXTRACTORS (88, 113-118)

The oldest successful continuous oil seed extractor, and one that many

still consider the best type, is the Bollman or Hansa-Muhle extractor (119), otherwise

known as the paternoster or basket type. This extractor was designed and first built

in Germany; the American-built Blaw-Knox and French extractors are very similar.

The basket-type extractor (Figures 15.18 and 15.19) has the

appearance of an enclosed bucket elevator. Unlike the various types of continuous

extractors to be described later, it docs not immerse the oil seed flakes in the solvent

but extracts by percolation of solvent through the flakes while they are held in a

series of baskets with perforated bottoms. To ensure uniform percolation and

drainage, the width and depth of the baskets are usually fixed, and the length is

varied according to the capacity of the extractor; common dimensions are 20-28

inches deep, 30-10 inches wide, and 40-85 inches long (114). The baskets (usually,

38 in the earlier models) are supported on endless chains, within a gastight housing.

C.O.E.&T.Akola. 45
 Extraction Techniques for Various Seed Oils

The flaked oil seeds are conveyed by a screw into a closed charging hopper at the top

of the housing. The completely filled conveyor tube serving as an effective vapor

seal against the solvent vapors inside the extractor. The baskets are continuously and

very slowly raised and lowered at the rate of about 1 revolution per hour. As each

basket starts down the descending side of the apparatus, a charge of seed is

automatically dropped into it from the charging hopper. Extraction is effected by the

percolation of solvent through the seed during their passage from the top to the

bottom and again to the top of the apparatus. As the baskets containing the spent and

drained flakes ascend to the top of the housing on the opposite side from the

charging hopper, they are automatically inverted and the contents are dumped into a

discharge hopper from which they are conveyed by means of screw conveyors to the

meal driers.

Fresh solvent at the rate of approximately I pound of solvent per

pound of seed is sprayed into a basket near the top of the ascending line of baskets,

from which it percolates by gravity through the lower baskets, in countercurrent

flow. The miscella from this side, termed the "half-miscella," is collected in a sump

in the lower part of the housing. A pump continuously withdraws it from the sump

and sprays it into the topmost basket of the descending line. From this basket it

percolates downward through the lower baskets like the fresh solvent introduced on

the other side of the system and is collected in a separate sump as "full-miscella."

The full-miscella is freed from fine seed particles and solvent, to yield the finished

oil, by means which will be described later.

C.O.E.&T.Akola. 46
 Extraction Techniques for Various Seed Oils

Detailed operating data on a modified 400-ton per day Hansa-Muhle

plant processing soybeans have been published by Kenyon, Kruse, and dark (120).

Commercial hexane at a temperature of 136°F. is used as the solvent at the rate of

960 pounds per 1000 pounds of flakes (9.5% moisture content) to reduce the oil

content of the finished meal (containing 8.0% moisture) to 0.6-0.7% and produce a

full-miscella containing 25-28% oil. The extracted and drained flakes leaving the

extractor retain about 35 % of their own weight of entrained solvent. Most of the

basket-type extractors built thus far have been large, with capacities of the order of

200-1000 tons of flakes per day. In recent years the basket extractor has been

modified into square and rectangular (horizontal) types (115) wh8re, in addition to

solvent or miscella draining vertically from one basket to another, it may be pumped

to individual baskets in the horizontal sections. In this way recirculation of miscella

can be used with generally improved efficiency. The horizontal extractor also permits

one-floor operation and can be housed at minimum cost.

Basket filling has also been improved with respect to vapor seals and

may be adapted to preslurrying of flakes with miscella before dumping into the

baskets.

C.O.E.&T.Akola. 47
 Extraction Techniques for Various Seed Oils

The Blaw-Knox Rotocel extractor (figure) (121, 122) is similar in

principle to the basket extractors described above; however, the baskets are carried in

a rotary motion in a single horizontal plane and miscella percolating through the

baskets and falling into compartments in the bottom of the extractor housing is

picked up by a series of pumps and recirculated countercurrently to the flakes. The

first commercial unit placed in operation on soybeans in early 1950 employed 18

cells and six stages of extraction. It operated in a housing 12 feet high and 22 feet in

diameter and had a capacity of 250 tons per day (122). Extractors approximately

four to seven times this capacity are now in operation. These are reported to have all

the advantages of the conventional basket-type extractor without some of its

disadvantages, being more compact and more flexible in operation. The French Oil

Mill Machinery Company has recently announced a stationary basket extractor in

which flakes and major machine parts remain stationary throughout the entire

extraction cycle (123).

Rotocell extractor.

C.O.E.&T.Akola. 48
 Extraction Techniques for Various Seed Oils

The principal advantage of the basket-type extractor is that it yields a

very clean miscella with a minimum content of fines, since the flakes are not

subjected to mechanical disturbance during the extraction period and the descending

baskets form an effective series of filter beds for the half-miscella from-the

ascending baskets where most of the fines production occurs. Its principal

disadvantages are that it permits the possibility of channeling solvent flow through

the seeds and that some oil seeds tend to pack in the baskets and become relatively

impervious to percolation, with the result that the extraction rate becomes slow and

the size of extractor required for a given capacity becomes unduly large. It should be

noted, however, that materials difficult to process in the basket-type extractor

likewise complicate the operation of extractors of other types.

Another early German extractor, the Hildebrandt (124), consists

essentially of two vertical tubes interconnected at the bottom by a third horizontal

tube, with motor-driven screws to propel the flakes down one tube, across, and up

the other tube countercurrent to the flow of solvent. Because of the working given

the flakes by the screws, flake disintegration and fines production are relatively

extensive; for this reason it is unsuitable for seeds such as cottonseed, although it has

been reasonably successful in processing soybeans. A number of installations are in

operation in this country and abroad, but the trend appears to be away from this type

of equipment. The original Hildebrandt extractor is no longer manufactured, nor is

the modified design with screw propulsion of the flakes found in the Ford extractor

(125), or the modern counterpart of the latter apparatus, the Detrex extractor (126).

C.O.E.&T.Akola. 49
 Extraction Techniques for Various Seed Oils

A variation in design consisted in the substitution of a drag-link conveyor for the

flake-propelling screws (102). All of these latter extractors were designed for the use

of a chlorinated solvent and were intended primarily for the small-scale extraction of

soybeans, for example, at the rate of about 25 tons per day. A number of these

extractors, manufactured by the Crown Iron Works, Minneapolis,

Minnesota, are in service in small capacities.

The Bonotto extractor (127) (Figure 15.21) has a column divided into

a number of sections by a revolving assembly of horizontal plates attached to a

central shaft. The plates are provided with a series of staggered slots through which

the flakes, introduced at the top of the column, proceed downward by gravity,

countercurrent to a rising flow of solvent. Stationary scraper arms placed Just above

each plate provide gentle agitation of the flake mass to prevent packing or bridging

and assist in moving the flakes through the slots. The original Bonotto extractor

employed a screw discharge with choke mechanism to compress the spent flakes and

seal the bottom of the column against the escape of solvent. Discharge of the flakes

through such a mechanism has the advantage of squeezing out most of the entrained

solvent. With some seeds, however, it m not mechanically reliable; hence, in

extractors of the Bonotto type operating on seeds than soybeans it has generally been

replaced with an inclined side tube, up which the spent flakes are carried by a Redler

or drag-link conveyor, through a set of squeezing rolls.

C.O.E.&T.Akola. 50
 Extraction Techniques for Various Seed Oils

An improved Bonotto design (128) uses a Redler conveyor within a

closed loop to feed the column and filters the miscella from the column through the

flakes in a portion of the loop before it is discharged. This assists in clarifying the

miscella and also extracts considerable oil from the flakes before they enter the

extractor proper.

C.O.E.&T.Akola. 51
 Extraction Techniques for Various Seed Oils

The Allis-Chalmers and Anderson extractors are modifications of the

Bonotto apparatus; each employs stationary plates or partitions and moving scraper

arms within the column rather than moving plates and stationary arms, and there are

other structural differences, as well as differences in auxiliaries. The Anderson

extractor for soybeans uses a choke or plug-forming flake discharge and has a built-

in mechanically operated device for settling fines out of the miscella; the Allis-

Chalmers extractor uses an inclined side tube discharge for all oil seeds. In present

installations this type of extractor is commonly used with prepressing, thus

minimizing the problem of "fines" in the miscella.

The Kennedy extractor (129) (Figure 15.22) is built in the form of a

long, enclosed trough divided into a number of sections, each of which has a rounded

bottom. An impeller wheel carrying four curved and perforated blades revolves in

each section, with the blade tips closely following the contour of the rounded bottom.

Material introduced into the first section is transferred the length of the trough, from

section to section, by the scooping action of the impeller blades as the solvent flows

through the bottom of each section in a counter direction. As the material is lifted up

the curved section wall above the liquid level, to fall into the succeeding section, it is

compressed slightly between the impeller blade and the wall; this squeezes out some

of the entrained solvent and serves to decrease the carryover of solvent from one

section to another by the flakes. From the final section they are carried up an

inclined tube and out of the extractor by a drag conveyor. This type of extractor has

not found general acceptance.

C.O.E.&T.Akola. 52
 Extraction Techniques for Various Seed Oils

A traveling-belt type of horizontal extractor originated by DeSmet in

Belgium has found only limited use in this country.

The "filtration extraction" process developed at the United States

Department of Agriculture laboratory in New Orleans (92) is now manufactured by

Wurster and Sanger and is used in plants extracting cottonseed. In this process, the

flakes are first "cooked" lightly, quickly air-cooled ("crisped"), and then immersed in

miscella for some time. Following this, the mixture is conveyed to a horizontal

rotary vacuum filter where the flakes are washed with leaner miscellas and finally

with fresh solvent. The process and equipment are reported to be adaptable to a

wide variety of oil-bearing materials, including, some that are difficult to extract in

other types of equipment.

Many other continuous extractor designs have been patented, and a

few have been used commercially in Europe or South America. Of these, these, the

Miag(130) and Fauth (131) extractors deserve particular mention. For some detailed

descriptions of these as well as the more common extractors mentioned previously,

reference should be made to the publications of Goss (88), Werth (113), Alderks

(42), and Langhurst (1).

A plant for the commercial extraction of castor oil (132) departed

from the conventional practice of forming flakes and striving to maintain the flake

structure throughout the extraction process by grinding the seed and extracting the

finely disintegrated material in three successive stages, in which it was alternately

mixed with the counter flowing solvent and separated by centrifugation in

C.O.E.&T.Akola. 53
 Extraction Techniques for Various Seed Oils

continuous Bird centrifugals. Heptane was used as the solvent at a temperature of

170°F. According to Pascal (133), miscellas containing oil in the range of 8-22% can

advantageously be separated by cooling into an oil-rich and an oil-poor phase with

the latter being reused as a solvent without distillation. Commercial heptane und

castor oil arc miscible in all proportions above about 310C., which is well below the

preferred extraction temperature of 50'C.; but good separation occurs upon cooling a

20% miscella, for example, to20°C. It is understood that this plant has or is being

converted to prepress conventional continuous extraction (118).

RECOVERY OF SOLVENT

Recovery from Miscella:

Normally, miscella from the solvent extractor is freed of finely

divided solid material before it is processed for oil recovery. Although it is possible

to clarify the oil after the solvent is removed (77), the presence of fines complicates

C.O.E.&T.Akola. 54
 Extraction Techniques for Various Seed Oils

the operation of packed distillation columns, and this method also leads to excessive

losses of oil entrained in the fines, unless the letter are well washed. It is generally

not considered advantageous to recycle a large amount of separated fines through the

extraction equipment. Recently, however, increasingly widespread use of “disk and

doughnut”- type stripping columns has made the handling of miscellas containing

fines much easier and has decreased emphasis on complete removal of fines from

miscella before distillation.

The amount of fines to be handled varies greatly with different oil

seeds and different types of extractors. Basket-type or percolation extractors

processing soybeans produce very little fines and the miscella is simply filtered,

usually through leaf-type filters, which must be cleaned only occasionally. In

processing nonprepressed seed, such as cottonseed, through extractors of the

immersion type a considerable proportion of fines is obtained. It must be handled

with special equipment and washed to reduce the oil content if a high overall

extraction efficiency is to be maintained. Here the tendency was to rely upon

continuous centrifuges of the Bird type to remove most of the solid material and

filtration to provide the final clarification. None of the clarification systems thus far

introduced appears to be altogether satisfactory where large amounts of fines are to

be handled; current problems in the extraction of high-oil-content seeds are largely a

matter of fines prevention or efficient fines handling rather than a matter of difficulty

in reducing the oil content of the seed.

C.O.E.&T.Akola. 55
 Extraction Techniques for Various Seed Oils

It has been reported (134) that 0.15-0.30% of fines in the miscella

have been successfully removed on a commercial scale by injecting 1-4% water plus

a wetting agent to effect hydration of the fines and separation of the hydrated

material plus a small quantity of emulsion in centrifuges of the fixed-nozzle or

automatic valve type.

The original Hansa-Muhle plant effected recovery of solvent from the

oil in three stages. The miscella containing 20-25% oil was passed in screw through

two steam-heated pot stills to reduce the solvent content to about 50%, then through

a falling film evaporator, where it was reduced to 5-10%, and finally through one or

two steam stripping columns of the packed type, where the last portions were

removed. In the American-built plants the pot stills have been replaced by miscella

preheaters and rising film evaporators with entrainment separators. In some cases

the falling film evaporator has been retained or replaced with a small rising film

evaporator operated with sparging steam; in others, miscella from the first large

rising film evaporator goes direct to the stripping column. Usually the stripping

column is maintained under reduced pressure with a steam ejector. The American

equipment is more compact, and with it the miscella a kept hot for a shorter period.

In the extraction of cottonseed oil, in particular, prolonged heating of the oil or

miscella will "set" the color and produce a permanently dark oil (135). However, no

difficulty in this respect has been encountered in plants using the rapid evaporation

equipment described above.

C.O.E.&T.Akola. 56
 Extraction Techniques for Various Seed Oils

Many soybean processors operate degumming and lecithin recovery

plants in connection with solvent extraction plants. In the past, some plants have

purposely allowed some condensation of stripping steam to occur in the

stripping column to hydrate the phosphatides and deliver an oil ready for passage

through the degumming centrifuges.

Systems comprising a fatty oil and hexane or other hydrocarbon

solvent exhibit a considerable negative deviation from ideality; that is, the vapor

pressure of the solvent is lower than calculated from it molar concentration in the

miscella and the vapor pressure of the pure solvent upon the basis of Raoult's law.

Below a solvent concentration of about 10% by weight, the boiling point becomes so

high that steam a stripping is essential in the final stages of solvent recovery.

Boiling point and vapor pressure data on mixtures of commercial

hexane with cottonseed and peanut oils have been published by Pollard et al. (136).

Values for the boiling points of cottonseed-hexane mixtures at different pressures, as

derived from Pollard's smoothed data, are shown in Table.

Figure plots vapor pressure curves for pure hexane, for commercial

hexane experimentally determined, and for a 10% commercial hexane miscella, both

as calculated for an ideal solution and as actually determined. The plots are on the

conventional basis of log vapor pressure versus reciprocal of the absolute

C.O.E.&T.Akola. 57
 Extraction Techniques for Various Seed Oils

temperature, to give straight lines. It will be seen that below a temperature of about

200°F. (corresponding to a value of l/T of 15.16), the actual vapor pressure curve of

the miscella is a straight line, with a slope equal to that of the vapor pressure curve of

the pure solvent or of the ideal curve but considerably below the latter. Assuming an

average molecular weight for the oil of 865 and for the solvent of 86, the mol.

percent of solvent in a mixture containing 10% solvent by weight is 52.8; hence the

ideal vapor pressure is at any temperature 52.8% of that of the solvent alone. The

activity coefficient or ratio of actual vapor pressure to ideal vapor pressure over the

linear portion of the actual vapor pressure curve may be determined from the figure;

at a value of 1/T of 16, for example, the actual vapor pressure is 310mm., whereas

the ideal pressure is 520 mm.; the activity coefficient is 310/520 = 0.60.

Table : Boiling points (degrees Fahrenheit) of mixtures of cottonseed oil and

commercial hexane (136).

Oil in Pressure (mm)

mixture
(wt %) 760 610 460 310 160

C.O.E.&T.Akola. 58
 Extraction Techniques for Various Seed Oils

0 152 10 124 105 80

50 158 145 130 111 82
60 162 150 133 114 85
70 171 157 140 120 91
80 186 172 154 132 102
85 201 186 167 144 113
90 231 210 189 163 129
92 248 226 203 177 142
94 273 250 224 192 156
95 289 268 238 203 165
96 - - 254 215 177
97 - - 271 230 190
98 - - - 248 207
99 - - - 272 229

Similar plots and calculations may be made for miscellas of other

concentrations where experimental values have been determined at temperatures

below 200°F.; the graphical data are shown in figure. In figure activity coefficients

are shown in terms of the composition of the miscella. Data subsequently published

by Smith and Wechter (137) on the vapor pressures of mixtures of soybean oil with a

practical grade of hexane in the range of 75-120°C. and 2-36 mol. percent or 0.2.5-

5.25 weight percent (figure) indicate activity coefficients generally between 0.50 and

0.60. For leaner miscellas, where boiling occurs at reasonable temperatures and

steam stripping is not required, the data in Table 15.5 are directly applicable. The

values from which the table was derived were determined in a laboratory apparatus

with vigorous stirring to prevent superheating of the solvent. In ordinary apparatus

considerable superheating may be expected.

The effect of differences in boiling points of various hexanes on vapor

pressures of the solvent or solvent fraction in a miscella has been studied by Smith

C.O.E.&T.Akola. 59
 Extraction Techniques for Various Seed Oils

(138), who has also determined the vapor pressure of hexane-soybean oil solutions at

high solvent concentrations(139).

In making practical stripping calculations, it should be recognized that

the last portions of solvent consist in part of heavy end of lower volatility than the

original solvent.

Recent improvements in recovery of solvent from miscella have

included double-effect and dual evaporation systems. Generally speaking, these two

systems make use of hot vapors from other parts of the oil and meal recovery

equipment so as to obtain maximum efficiency from the steam used and reduce

steam consumption to a fraction of that previously required (140).

C.O.E.&T.Akola. 60
 Extraction Techniques for Various Seed Oils

RECOVERY FROM EXTRACTED FLAKES

Formerly the standard equipment, originally of German design, for

desolventizing of the extracted flakes consisted of a series of horizontal steam-

jacketed tubes ("Schneckens") through which the flakes were propelled by screws.

For the final removal of the last traces of solvent or "deodorization" of the flakes, a

similar but larger tube was provided through which the flakes passed countercurrent

to a current of stripping steam. In recent years this type of meal desolventizing has

been largely replaced by "desol-ventizer-toasters,” similar to stack cookers, in which

both live and indirect steam are used (141). In this equipment live steam is injected

into the top and often also into lower kettles, where it evaporates most of the hexane

as it, in turn, is condensed. This adds moistures to the meal, minimizing dust

carryover to the condenser, and results in a combination of solvent removal and

toasting. From an operating standpoint this system is generally preferred to the

“Schneckens” originally employed.

In some cases desolventizing is accomplished by superheated solvent

vapors. This and "flash" desolventizing (112) are of interest mainly where it is

desired to avoid toasting and to minimize of denaturation of the protein.

When hydrocarbon solvents are used, the separation of condensed

solvent and condensed stripping steam from the "deodorizer" and from the miscella

stripping column is facilitated by the comparative immiscibility of the solvent and

water; a continuous decanter or settling tank is used to separate the solvent, which is

reused without further treatment.

C.O.E.&T.Akola. 61
 Extraction Techniques for Various Seed Oils

The extractor proper, all solvent and miscella tanks, and the various

solvent condensers are all vented to a vent condenser or condensers which are

protected by special means from loss of solvents. In some plants the vent condensers

are refrigerated; in others, they communicate with the atmosphere through charcoal-

C.O.E.&T.Akola. 62
 Extraction Techniques for Various Seed Oils

filled adsorbers which are periodically steamed for the recovery of solvent or

through a packed column down which a small side stream of oil is diverted as an

adsorbing agent. As indicated previously, solvent losses in the more efficient plants

operating with a hexane-type solvent do not exceed 2 gallons of solvent (about 11.5

pounds) for each short ton of flakes extracted.

Vapors from the "deodorizer" and air from a final meal cooler may

carry considerable dust, lint, etc., particularly if the extracted material is inclined to

powder. Scrubbers, cyclone separators, etc., of various designs are used to collect

dust and avoid fouling of the condensers and other portions of the solvent recovery

system, as well as the formation of emulsions in the solvent-steam condensate

separator.

Auxiliary Equipment :

C.O.E.&T.Akola. 63
 Extraction Techniques for Various Seed Oils

Auxiliary equipment for pretreating the seed before they enter the

extractor and for treating the desolventized and deodorized flakes after they leave the

extraction system is shown for a typical soybean plant in figure. The flake toaster

shown in the figure is a stack cooker similar to that depicted in figure. However,

many plants employ a more compact apparatus in which toasting is conducted under

steam pressure.

Recovery of oil from fruit pulps:

The only fruit pulp oils of commercial importance are olive oil and

palm oil. These oils must be recovered by techniques somewhat different from those

employed for the treatment of either fatty animal tissues or oil seeds. The extraction

of these oils will, therefore, be considered apart from the different processes which

have been discussed previously.

Extraction of olive oil.

The extraction of olive oil is in general carried out by less efficient

and legs modern methods than most other vegetable oils, since the industry is highly

decentralized and is distributed throughout the growing countries in many small

establishments.

Notwithstanding the fact that olives are seldom transported long

distances from the producing groves to the extraction plants, they are often subjected

to considerable abuse prior .to being processed. The rather general practice of

bruising the fruit during harvesting, and later storing it for protracted periods,

accounts for the fact that olive oil usually has a rather high content of free fatty acids.

C.O.E.&T.Akola. 64
 Extraction Techniques for Various Seed Oils

The equipment used for processing olives for oil varies greatly from

one country to another and even from mill to mill within the same country. Perhaps

the most common method of preparing the pulp for expression comprises putting the

fruit through mills of the edge runner type without cracking the fruit pits. The

macerated-pulp is then transferred to woven baskets or "scourtins," and the oil and

water are expressed in a hydraulic press. The presses used for this purpose generally

develop considerably less pressure than those used for the expression of oil seeds,

since the fluid nature of the pulp mass pre-eludes the application of very high

pressures.

Pressing is carried out in two or more stages with the first pressing

yielding the highest grade, so-called "virgin" olive oil, and each subsequent pressing

yielding a lower grade. Prior to the last pressing the cake is sometimes broken up

and moistened with water, and in some cases it is subjected to a more thorough

milling with cracking of the olive pits. In all cases, heat treatment of the pulp or

cake is avoided.

In the United States, hydraulic box presses arc generally used for the

recovery of olive oil although there is some use of screw presses. It is reported to be

possible to press olive pomace mechanically to a residual oil content of 8%, although

much of that produced in California runs as high as 12-13% oil (143). The press

cake or pomace is extracted with a hydrocarbon solvent usually of the hexane type;

and the extracted oil is refined, bleached, and deodorized, after which it is blended

with other oil in the preparation of the grade of oil termed “pure olive oil.” A similar

C.O.E.&T.Akola. 65
 Extraction Techniques for Various Seed Oils

method of processing is now also becoming common in the olive-producing section

of the Mediterranean region.

Extraction of palm oil:

At one time, most of the palm oil on the market was extracted by

African natives by exceedingly primitive methods. In recent years, however, the

production of oil from wild-growing trees has been much exceeded by that from the

plantations of Indonesia, Malaysia, and the Republics of the Congo. The plantation

oil has generally been extracted by modern methods and is much superior in duality

to the older African oil. Good plantation oil consistently runs lower than 5 % in free

fatty acids, whereas native-produced oil was not commonly as high as 15, 25, or

even 50% in free fatty acid content.

The sequence of operation in a plant designed and constructed in 1949

(144) is as follows: The fruit is first sterilized with low-pressure steam. This

destroys enzyme action while at the same time loosening the fruits from the stalks. A

stripping machine completes the separation of fruits from the stalks. A stripping

machine completes the separation of fruits from the stalks by a threshing action. The

loose fruits are next conveyed to a steam-jacketed digester where they are heated and

agitated to disintegrate the pericarp and form a mash. Large centrifugal extractors

remove 90-93% of the oil from the pericarp. Crude oil produced is run into tanks

where it is heated with open; steam, settled, and recentrifuged.

C.O.E.&T.Akola. 66
 Extraction Techniques for Various Seed Oils

Palm nuts are not broken by this processing and pass from the large

centrifuges to a revolving screen where the nuts are separated from the kernels and

then sacked for shipment.

With adequate preparation and cooking of raw material to be

processed, the capacity of an expeller or screw press is a function of the shaft

arrangement and the shaft speed. For example, the meats from 25 to 100 tons of

cottonseed per day can be expressed leaving cakes containing 3.0 to 9% oil,

depending upon the shaft speed and worm arrangement. Moreover, 68 a rule, no loss

in extraction efficiency if experienced in going from the old capacity of about 20 to

25 tons of cottonseed per day to the much higher rate of 45 to 50 tons.

Despite the use of special alloys and manufacturing techniques

designed to make expeller parts as hard as possible, shafts do wear with usage and

tonnage normally drops. Some modern machines are manufactured with provisions

for rapid gear change, making it possible to increase the revolutions per minute and

the tonnage with only a very short down time. New or newly built-up shafts may be

expected to process the meats from about I ton of cottonseed per revolution per

minute with high efficiency. Where only a prepressing action is desired, 100 tone

per day can be obtained with approximately 45 r.p.m. Tonnage may also be increased

without loss in efficiency by having a minimum amount of bulls in the expeller feed.

Since the expeller appears to-handle a certain volume of feed, removal of hulls

makes it possible to increase capacity by removing essentially nonextractable

material from the feed. This also minimizes wear from the highly abrasive hulls.

C.O.E.&T.Akola. 67
 Extraction Techniques for Various Seed Oils

This increased tonnage with high efficiency naturally increases the power

requirements with motor horsepowers up to 125 now being used as compared to 40

to 60 of a few years ago. Suitably strengthened gear boxes, etc., are also required.

With the high capacity and efficiency thus possible, coupler with lower installed

equipment cost as compared to solvent extraction, expeller operations compare

favorably in many cases with the more efficient solvent extraction.

In addition to the general literature references on the continuous

pressing of oil seeds (63), there are also references dealing specifically with screw

presses (64-69), expellers (70, 71), and product quality (66,72).

LOW-PRESSURE PRESSING

For the prepressing of oil seeds prior to extraction, ordinary high

pressure screw presses may be operated at low pressure and at increased capacity.

Specially designed machines are much more satisfactory, however; in new

installations these are normally used.

In this country, most of the plants solvent-extracting cottonseed do so

via the prepress route. At first this was probably the result of problems m handling

"fines" and difficulties in detoxifying the extracted flakes when direct extraction was

used. Other advantages of prepressing include the need for only a minimum-sized

solvent plant, since moat of the oil is removed in the prepressing step, and the

production of meal of high protein quality. Disadvantages are higher initial

equipment coats if, for example, soybeans must also be proc-eased in equivalent

tonnage in the same plant and, normally, higher power requirements and repairs.

C.O.E.&T.Akola. 68
 Extraction Techniques for Various Seed Oils

Prepress solvent extraction of cottonseed has been discussed by Pons et al. (73) and

by Rea and Wamble (69). The nutritional value of the meal has been discussed by

Chang et al. (74). Prepress extraction of soybeans is described by Dunning and

Terstage (71).

Expellers and screw pleases of the same design as those used for oil

seeds are sometimes used for pressing whale or seal flesh or fish, and for processing

meat scraps, .but these materials are more commonly handled in screw presses

specially designed for the purpose.These are generally of lighter construction than

the machines built for oil seed extraction and are operated under lower pressure.

Centrifugal Expression

The removal of oil from an oil-bearing by centrifugation has been a

standard method only in the case of palm fruit. However, recent developments in the

rendering of animal fats make full use of centrifugal separation of oil. The

centrifugal recovery of palm oil will be discussed in a later part of this chapter.

Solvent Extraction

Application:

While extraction with solvents constituents the most efficient method

for the recovery of oil from any oil-bearing material, it is relatively the most

advantageous in the processing of seeds or other material low in oil. The minimum

oil content to winch oil cake can be reduced by mechanical expression is

approximately the same for all oil seeds, that is, about 2 to 3%. Consequently, the oil

unrecoverable by mechanical expression, in terms of percentage of the total oil,

C.O.E.&T.Akola. 69
 Extraction Techniques for Various Seed Oils

increases progressively as the oil content of the seed decreases. Comparative yields

of oil from representative seeds of low, medium, and high oil content by the two

methods of processing are shown in table. Substitution of solvent extraction for

pressing methods increases the yield of oil from soybeans by 12.1%, whereas in the

processing of cottonseed the increase is 11.5% and in the case of flaxseed only 5.3

%. These figures, it should be noted, are industry-wide averages. The increase of oil

yield for soybeans and cottonseed by solvent extraction over the most efficient

mechanical processing today is appreciably less.

Table : Comparison of solvent extraction with mechanical pressing in the United

States, 1957-1958 (75)

Flaxseed
Soybeans Cottonseed
(Estimated)
Oil yield per ton
Hydraulic b 308 None
Continuous screw press 300 327 674
Solvent extraction 362 376 710
Total, United States 358 339 699
Percent increased oil yield
Solvent over screw press 12.1 11.5 5.3
Solvent over hydraulic - 22.1 -

Of all the common oil seeds, soybeans are solvent-extracted most

easily. In the crop year 1957-1958 it was estimated by the Production and Marketing

C.O.E.&T.Akola. 70
 Extraction Techniques for Various Seed Oils

Administration of the United States Department of Agriculture (75) that 93.2% of the

soybeans processed were solvent extracted, with an average yield of 362 pounds of

oil per ton, as compared with 6.8% screw pressed, with an oil yield of 300 pounds

per ton.

Cottonseed flakes disintegrate more readily and occasion more

trouble from the production of fines, whereas peanuts and flaxseed disintegrate very

badly. By "prepressing" or "forepressing" the seed in low-pressure screw presses to

remove a portion of the oil it is possible subsequently to solvent-extract high-oil-

content seeds that are difficult or impossible to handle in their original form in

conventional equipment. In Europe and where European practices have prevailed, it

is the general practice to extract whole soybeans but to prepress other oil seeds. In

the United States prepressing is used commercially on cottonseed, flaxseed, peanuts,

and corn germ.

Solvent extraction finds some use in the recovery of animal fats. The

tankage or cracklings from dry rendering are often solvent extracted, usually in batch

extractors. The recovery of fat from garbage is frequently carried out by means of

solvent extraction since the low fat content of this material makes other methods of

recovery difficult. Garbage is extracted in batch equipment of special design.

Materials containing scarce or expensive oil are often solvent

extracted even when the operation is relatively difficult. Examples are castor oil,

olive oil and wheat germ oil residues from mechanical pressing. Solvent extraction

may be wed to obtain a fat-free residue or a residue in which proteins are not heat

C.O.E.&T.Akola. 71
 Extraction Techniques for Various Seed Oils

denatured, rather than for the primary purpose of improving the yield of oil. Thus,

for example, cocoa is solvent extracted in order to produce a residue which may

serve as a source of the bromine. Solvent-extracted meal is preferred for the

manufacture of protein adhesives, fibers, or plastics, since there is much less

denaturation of the protein in this meal than in that obtained by cooking and

mechanical pressing.

Since minimum heat treatment is involved, oil produced by solvent

extraction is of maximum quality, and the meal contains protein subjected to a

minimum of damage due to the effects of heat. On the other hand, there are several

disadvantages:

(a) Solvent extraction equipment is relatively expensive compared to other extraction

systems;

(b) Except where nonflammable solvents can be used, there is the ever-present

danger of fire and explosion;

(c) Low-oil-content meal tends to be dusty, with attendant problems; and

(d) As in the case of cottonseed, unheated flakes from the direct extraction of raw

flakes may contain material that is toxic to nonruminants and is not removed or

inactivated by the relatively mild processing, thus requiring further treatment.

PRINCIPLES AND THEORY :

Methods of Achieving Contact with Solvent.

C.O.E.&T.Akola. 72
 Extraction Techniques for Various Seed Oils

The laboratory extraction of an oil-bearing material in an ordinary

Butt extraction tube is an example of solvent extraction in its simplest form. In this

extraction procedure, the pure solvent is delivered continuously to the top of the

mass of material to be extracted and is percolated through the mass by gravity until

the removal of oil is substantially complete. Although this method is effective in the

laboratory, it is highly insufficient. Complete extraction can be accomplished only

by the use of a large volume of solvent relative to the volume of oil extracted, and

this solvent must eventually be recovered from the oil. Even in the most efficient

extraction plants, charges for steam and water for solvent recovery constitute a

substantial part of the operating costs (76); if the ratio of solvent to oil is high, such

charges may easily become prohibitive. A prime object in modern solvent extraction

practice is, therefore, to reduce the solvent content of the final miscella or oil-solvent

mixture to the lowest possible figure. In the best continuous soybean extraction

plants the solvent-oil ratio may be as low as 1 to 1 by weight, whereas by simple

percolation an equivalent extraction could hardly be accomplished with several times

as much solvent.

Efficiency is somewhat improved if the continuous percolation of

fresh solvent is replaced by prolonged treatment of the oil seeds or other material

with successive portions of solvent. Each portion is recirculated through the material

being extracted until equilibrium or near-equilibrium is established between the oil

content of the solid material and that of the solvent; that is, until free miscella is as

rich in oil as the miscella absorbed within the solid particles. When this condition is

C.O.E.&T.Akola. 73
 Extraction Techniques for Various Seed Oils

attained, the free miscella is drained off, a fresh batch of solvent is brought into the

system, and the operation is repeated. Extraction is thus continued in successive

cycles of recirculation and drainage until the oil content of the material is reduced to

the value desired.

Although batch extraction by means of percolation is satisfactory for

some materials, it is not generally adaptable to the large-scale processing of oil

seeds. It is virtually impossible to charge large extraction chambers with oil seed

flakes without uneven compacting of the material and consequent channeling and

incomplete extraction. Hence batch extractors for oil seeds are generally provided

with some means of mechanically mixing the solvent and the seed particles.

However, from the standpoint of efficiency in maintaining a low solvent-oil ratio it is

immaterial whether the solvent and the oil seeds are brought into equilibrium with

respect to oil content by circulating the solvent through the seeds while the latter are

contained in a tower or by simply intermixing the solvent and seeds in a chamber of

suitable design. The system of extraction by means of successive batches of pure

solvent is generally referred to as "multiple extraction."

The last portions of miscella recovered in the multiple extraction

process will naturally be very lean in oil; hence these portions may well be

substituted for fresh solvent in the initial treatment of fresh seed. In this way each

portion of solvent is made to perform a double duty, and the amount of solvent to be

recovered eventually from the oil is decreased accordingly. A batch extraction system

set up in such a manner as to utilize the principle of solvent reuse to the best possible

C.O.E.&T.Akola. 74
 Extraction Techniques for Various Seed Oils

advantage is designated as a "batch countercurrent system." In this system a battery

of extractors is provided and the solvent is used to treat the contents of each extractor

in succession. Each time a batch of miscella is drained from an extractor, it is used to

treat a batch of seeds which have previously been extracted with a richer miscella.

On the other hand, the drained seeds are each time extracted with a leaner miscella.

Thus the seeds are treated with batches of solvent of progressively decreasing oil

content, until they are finally extracted with fresh solvent and discharged while the

solvent is brought into contact with batches of seed of progressively increasing oil

content until it finally encounters fresh seed and is then discharged as the finished

miscella. In this way the miscella is brought out of the system at a uniformly high

oil content. If there are a large number of extractors in the battery, the effect

approximate that of mixing the solvent and oil in continuously moving

countercurrent streams.

Although batch countercurrent extraction may theoretically be

brought to an efficiency approaching that of continuous countercurrent extraction by

sufficiently increasing the number of extractors, the system thereby becomes

unnecessarily cumbersome. In practice, therefore, solvent extraction is carried out

on the largest scale only in continuous systems which are entirely automatic in

operation. Such systems achieve the highest economy of steam, power, labor, and

materials. Their adaptabilities is limited only by the mechanical difficulties involved

in moving the seed mass and the miscella in opposite direction a with free

intermixing and in effecting a final separation of the miscella and the seed particles.

C.O.E.&T.Akola. 75
 Extraction Techniques for Various Seed Oils

If it is assumed in batch extraction that a constant volume of miscella

is retained by the seeds after each drainage period, and this volume is known, one

may calculate the number of extractions required to reduce the oil content of the

seeds to any given level (77, 78), in the case of either multiple or batch

countercurrent extraction. Actually, however, the retention of miscella is not usually

constant but is variable for different solvent-oil ratios, presumably because of the

effect on drainage of such factors as viscosity and surface tension of the miscella.

This circumstance renders calculations highly involved, but Ravenscroft (79) has

introduced a graphical method for estimating the number of extractions required for

a given recovery of oil which is applicable in the was of variable oil retention.

DESIGN OF EXTRACTOR

DESIGN OF VERTICAL OIL EXTRACTOR :-

The design of the vertical oil extraction is done by considering oil

yield from soybean grits or grit :

Basis : The basis for the design has been taken as 4000 kg of Soyabean grit for the

extraction. (i.e.) 4000 kg of material handled per batch in the extraction.

The percentage of soybean oil extracted = 15% of the total grit feed.

= 600 kg of oil extracted per batch.

Batch Time taken for the extraction of the 600 kg of oil = 4 hrs.

Calculating the volume of grit handled above the perforated plate@mesh.

Now as we know :

C.O.E.&T.Akola. 76
 Extraction Techniques for Various Seed Oils

Volume (v) =

Density of Soyabean Seed = 919 kg@m3

V = 4000/919

V = 4.85 m3

= 4.85 m3 × 1.1 = 5.335 m3

This is the volume of grit handled above the plate mesh = 5.335 m3

Material used = Stainless steel.

Design of Extraction shell:

Now :

Where ; d = diameter of plate = 1.63 m

L = length of the extraction shell = 2.44 m

L 2.44
Now ; = = 1.49 ≈ 1.50
d 1.63

L = 1.50 d

π 2
v= d × 1.5d
4

d = 1.63 m.

This is the diameter of the extractor shell for the soyabean grit.

For the length of extractor we got to find it by geometrical method.

L = 2.44 m. ( By geometrical method)

The shell thickness = 1 inch according to std. Nomenclature.

∴Length of Extractor = 4.88 m

C.O.E.&T.Akola. 77
 Extraction Techniques for Various Seed Oils

Design of the Strainer:

The strainer is inclined at any angle of 100 with the shell for the

proper flow of the oil.

The length of strainer considering it as x mts.

1.63
∴ cos 10 =
x

∴ x = 1.65 m

The top end of the strainer is at the centre of the whole length of the

shell lies nearly at 0.795 m from bottom in top of shell. Now the mesh used is made

of stainless steel.

The mesh can be taken as of 0.1 mm from the standard nomenclature.

Design of the Down-Comer:-

The diameter of the down comes is assumed as 3 cm.

The length is also assumed, so that the down comer is immersed in

solvent.

The length has been taken as (more than) 0.376 m.

Design of the shell containing oil:

It is 2@3rd of the total shell

= 3.08/8 = 1.778 m from the bottom of shell.

Design of the solvent Distributor:

C.O.E.&T.Akola. 78
 Extraction Techniques for Various Seed Oils

The material used is stainless steel. This distributor is spread all over

the diameter of the shell. Hence the diameter of the solvent distributor = dia. of the

shell = 1.63 m.

It is perforated for proper flow of the solvent into the grit. The dia. of

each perforation can be taken as 5 mm.

The distributor is placed at the top of the shell below the head cover.

Design of the steam coil :

The steam coil is made of stainless steel material.

The coil is placed 25 cm above the shell and it is attached with a

steam heater out of the shell.

Design of the head covers:

The head covers are close to either end of the cylindrical shell. This

can be attached to the shell by welded, riveted or bolted construction.

The choice of the head covers is made depending on the pressure

handled. Depending upon the depth of dishing & its shape these are classified as

shallow dished, ared & dished, spherical, elliptical, hemispherical & conical.

For the design of the head covers of the vertical extraction we use is

top spherical head cover because the pressure handled is between 1 to 15 kg@cm2

gauge.

Height of head cover = 1/3 × length = 1.62 m

The thickness of this head cover is equal to that of the shell = 1 inch = 2.25 cm.

Design of the Inlet & outlets & provisions.

C.O.E.&T.Akola. 79
 Extraction Techniques for Various Seed Oils

An inlet of 10 cm is provided for the feed of the grit in the shell.

It is placed at 40 cm above from the strainer.

Another outlet is provided for solvent which is also taken of 10 cm

dia. above 38 cm above the shell bottom.

Outlet is provided in the bottom cover for removal of oil. This outlet

is provided with a valve.

An inlet of 10 cm is provided on the top head over for the feed of

solvent (hexane).

The inlet of the feed is provided on the manhole. The manhole is

provided for cleaning and withdrawing leached solid i.e. seed from the extractor.

SOXLET'S ANALYSIS

Analysis of Soxlet's apparatus:

Theory :

This apparatus is generally divided into 3 sections or part which can

be detached. As the three parts can be removed or identified sequentially. These part

are at the bottom flask which is used to handled solvent-oil mixture. Heating is

provided to this flask. The second section is a centrally placed delicate tube i.e.

extract tube where the necessary operation i.e. extraction of oil from the seeds take

place. This tube is seen as a big test tube but it has an extra arrangement for solvent

C.O.E.&T.Akola. 80
 Extraction Techniques for Various Seed Oils

seperation after getting contact with the seeds placed in a inner section of this tube.

The seeds are placed in a seed holder called as thumble which is made up of

permeable material like blotting paper which allows liquid hexane and oil to charge

out of the thumble without interference of seed particles which may block the small

tube used for transportation of solvent oil mix from the centre tube to the round

bottom flask. The upper section consists of condensers tube which condense the

vapour solvent into liquid phase so that it can come in contact with the seeds placed

in thumble beneath it. This tube generally handelds dry seed from which oil is

extracted. If seeds are in powered forms they are generally wrapped in a filter paper

and then placed straight in the tube.

The third section or part is called condenser where solvent in

continuously condensed and dropped in the extract tube by circulating a external

water stream. The water used for circulation should be cold and the flow rate should

be fast.

All three parts can be fitted into each other and assembles to a single

apparatus. In each of the three section separate process occurs. At the bottom heating

occurs, at the middle section extraction occurs whereas at the top section cooling or

condesing occurs.

C.O.E.&T.Akola. 81
 Extraction Techniques for Various Seed Oils

Procedure :

1. Take a quantity of petroleum solvent (hexane) say 100 ml in the round bottom

flask.

2. Now crush the sample seed into powder form and then weight it to 10 gm

approximately. Note that during crushing of seed the oil from the seeds should

not expel out.

3. The seed used should be completely dry.

4. Now prepare a cone of a filter paper such that it can be easily placed in the

extraction tube. Fill the cone with 10 gms of crushed powder and then place the

cone in the extract tube properly in straight position.

C.O.E.&T.Akola. 82
 Extraction Techniques for Various Seed Oils

5. Now fit the condensing tube with inlet and outlet long pipe and allow the cold

water to flow through inlet pipe.

6. Maintain the flow of cold water so that maximum cooling of hexane occurs.

7. The cold water flows from inlet pipe & through condenser, after condensing

hexane if leaves through the outlet pipe.

8. After completion of preliminary arrangements, the hexane in the flask is heated

with the help of burner approximately upto 1 hr so that complete recovery of oil

from the seed is obtained.

9. The procedure occurs in this way that on heating the hexane, the vapours of

hexane rises in condensing tube.

10. A condensing tube where hexane is condensed by water and the liquid hexane

falls into the extraction tube.

11. After extraction, the mixture of oil & hexane is passed into the flask by a side

tube. The extraction is carried out till a faint colour of oil in the hexane appears.

This could approximate take one hour.

12. After all oil is extracted from seed, heating is stopped.

13. Oil and hexane mixture is allowed to cool.

14. The sample is then weighted.

15. The cake is also weighted.

16. The hexane and oil mixture is then separated by evaporating hexane from the oil.

17. The separation can be done either by heating the mixture in water bath by

distillation or by sun drying till the smell of hexane from oil disappears.

C.O.E.&T.Akola. 83
 Extraction Techniques for Various Seed Oils

18. The separation is also performed in the same soxlet apparatus. This could be

done by heating the mixture in the flask after which the hexane evaporates from

oil it is condensed and collected in an extraction tube till the height just below the

inside tube because if the condensate passes the height of side it will again go

back to the flask and mix with the oil.

19. While doing so, care must be taken so that oil must not burn due to excessive

heating.

20. The hexane collected in extract tube and the oil in the flask both are weighted

and percent oil extracted is calculated.

Resultant Analysis

After oil has been extract the oil are studied for the following analysis

S.No. Name of the Seed Acid value SAP value Iodine Value
1. Neem oil 0.4 193 66.4
2. Nagarmotha 0.28 190 209
3. Bitter Almond 0.23 184 113
4. Soybean 0.3 185 124
5. Bavanchi 0.5 187 153

Sr. No. Name of Seeds Gram of Seeds used Oil extracted in %

1. Neem oil 10 gm 12 -16
2. Nagarmotha 10 gm 8 - 10
3. Bitter Almond 10 gm 15 - 19
4. Soybean 10 gm 13 - 16
5. Bavanchi 10 gm 12 - 15

C.O.E.&T.Akola. 84
 Extraction Techniques for Various Seed Oils

SOLVENT EXTRACTION OF SOYBEAN OIL

Soybeans are subjected to preliminary cleaning and milling operations

as usual. The soy meal is then cooked. But the cooking of meal by heat treatment is

done under mild conditions. The heat treated meals are then converted into flakes

using smooth flaking rolls. Solvent extraction of the cooked flakes can be done

batch wise or continuously. In continuous extraction method countercurrent solvent

flow is preferred. The oil from the miscella is separated by distillation and stripping

under vacuum. The extracted meal is desolventized by heating with live steam in a

desolventizer. The solvent from the distillation and stripping columns as well as

from the desolventizer is condensed and recovered and stored in the solvent storage

tank. The oil, separated from the miscella in the distillation column goes to oil

storage tank after cooling. The flow sheet for a continuous solvent extraction

process of soybean is shown, in fig. The deoiled cake contains about 1% residual

oil.

C.O.E.&T.Akola. 85
 Extraction Techniques for Various Seed Oils

C.O.E.&T.Akola. 86
 Extraction Techniques for Various Seed Oils

Soybean Production & area 2000-01

Area Production (m.t.) Productivity(kg/ha)

World 73553 162480 2209

(1000 ha) (1000 m.t.)

India 5700 5400 947

(1000 ha) (1000 m.t.)

Maharashtra 6.8 Lakh ha 8.8 Lakh ha. 1287

Complication : Protein 40%

oil - 20%

Vitamin B complex

Biotin, folic acid,

Pyridoxin & vitamin E

Ref : - Post Harvest Technology-

A. Chakraverty

C.O.E.&T.Akola. 87
 Extraction Techniques for Various Seed Oils

MARKETING

The oil extracted by solvent extraction is an essential oil and has

heavy demand for medicine purpose. As we all known soybean is a high protein,

carbohydrate diet and the oil extracted from it is also used for medicine purpose.

The oil of Psuropoba is used in avoidable as a medicine for skin diseases and in hair

care shampoos etc. The oil of Psuroples is extracted by Bhadnath and is marketed

as Babach-tale costing 40 Rs per 50 ml. It comes in three packing 50 ml, 100 ml and

250 ml only. The neem oil is also an important oil exported to Australia, china,

Japan, Malaysia and other countries as a bio fertilizer as well as insecticide. It is also

used for manufacturing medicines for diabetic person as well as for neem soap

manufacturing. The seeds containing 12 to 20 % of oil are selected for solvent

extraction. This is because crushing and other conventional methods for extraction

would be ineffective and less yield is obtained.

C.O.E.&T.Akola. 88
 Extraction Techniques for Various Seed Oils

RELATION BETWEEN AYURVEDA AND

CHEMICAL ENGINEERING

Man is the only clever living being that knows how to adapt to the

changing environment of time and space. That genius of him has given to him the

supreme position in the world and enabled him to make progress and utilize all the

new achievement of science in the interest of himself and humanity.

During the oral era of Education ( Vedic period ), the man compiled

sutra-styled encyclopaedic treatises mostly in simple, rhythmic poetry. Oral

transmission was the only method for education at that period and this style being

convenient to memorize was accepted.

During the manuscript era, the man tried to dilate or abridge,

comment or criticize, expound or extract, as writing has been of some help to spread

the knowledge and relieve the extra-ordinary burden of memorizing the totality of

knowledge.

With the advent of printing process, the man gets a powerful means of

expression of his thoughts, ideas and experiences to his full satisfaction. He

C.O.E.&T.Akola. 89
 Extraction Techniques for Various Seed Oils

becomes relieved of memorizing strain, and science has so enabled him today that he

can print not only the word but record its sound rhythm, style and even passion with

which it is uttered.

With these progressive achievements in the sphere of verbal

knowledge on one side and in the change of concept of generalization and all-round

distribution of medical knowledge on the other side, it is bin natural that there will

arise a need for simplifying modification in the writing of medical literature so that

people of various grades of intelligence may have full benefit of this knowledge.

A glance is the history of Ayurveda confirms this process of

modulation of compilation of medical knowledge to suit the existing circumstances.

Medical knowledge began with scattered references in the Vedas. Then there was

compiled Ayurvedic Samhita as a comprehensive tretise on the science of life. It is

said to be a systematized compilation divided in 1000 chapters. Each chapter

containing 100 verses, thus making one hundred thousand verses in all.

bg [kYok;qosZnh

ukeksikaxe/koZosnLFkktqRikpSo iztk%]

Üyksd’krlg[ke/;k;lg[ka p d`rokULopaHkw%A

‘This science known as Ayurveda is a branch of Atharvaveda. The

self-created Brahma before creating men, first formulated this science of life

consisting of a hundred thousand verses and a thousand chapters.

Then came the creation of scientific encyclopaedic treatise divided in

eight branches viz., Charaka Samhita and Sushruta Samhita. This was the creator’s

C.O.E.&T.Akola. 90
 Extraction Techniques for Various Seed Oils

Age. Vagbhata later on compiled a concise book taking the fundamentals of the

above two books, adding the new knowledge and making the book to suit the time

¼;qxkuq:i½ and be the cream of knowledge of the disease and drugs of the

whole universe ¼foÜoO;k/;kSf/kKkulkj%½- This was the transmuter’s

Age.

Then the separate books on various branches of medicine were

compiled viz Madhav-Nidan, Sharangadhar-Samhita; and the last encyclopedic book

Bhav-Prakash was published in the sixteenth century. This was the transmitter’s

Age.

Vagbhats, Madhava, Sharogadhars, Bhavamisra and all other authors

of these periods adopt the method of collecting all the existing literature, extracting

the useful parts and compiling them in a simple classified form.

It is classified in eight different Branches known as ‘Ashtanga

Ayurved’

RkL;k;qosZnL;kM~xkU;IVkS ] r|Fkk

dk;fpfdRlk ] 'kkykd;a ]

'ky;kigr`Zda fo"kxjoSjksf/kdiz’keua ] Hkwrfo|

k]

dkSekjHk`R;da ] jlk;ua] okthdjxfefr AA

pjd lq=LFkku 30A28

C.O.E.&T.Akola. 91
 Extraction Techniques for Various Seed Oils

Kayachikitsa, Shalakya, shalya, Agadtantra, Mantra, Kaumarbhritya,

Rasayan and Vajikaran are the Ashtanga of Ayurveda. All the Ayurved knowledge is

found in these Ashtang. According to time the Ayurved knowledge increases and so

Ashtanga Ayurved is divided into subclasses (Pravibhaga) like Ras-shastra, Baishjya-

kalpana, strirog vigyana and Prasuti-Tantra etc.

In Ras-shastra and Baishjya-Kalpana mainly different Ayurvedic

Medicinal preparation process and their uses in different disease can be described. In

Ras-shastra oil extraction process (Tail-Nishkasan Padhati) can be described in

detailed by using ‘Patalyantra’.

gLrizek.ka fuEua p xrZa d`Rok iz;Rur%A

rfLeu~ Hkka.M p laFkkI; rFkkU;r~

ik=ekgjsr~

rfLeUUkkS"kf/k oxZa p nRok·U;a p 'kjkode~A

eq[ks laLFkkI; fNnzkf.k d`Rok pSo 'kjkodsAA

'kjkolfgra ik=a xrZLFks Hkktus U;lsr~A

laf/kysia rr% d`Rok xrZekiw;Ze`Rlu;ksAA

i'pknfXau p izTokY; LokM~++x'khra

leq)jsr~A

C.O.E.&T.Akola. 92
 Extraction Techniques for Various Seed Oils

i'pkr~ rr~ ik=e/;LFka ik=a ;qDR;k

lekgjsr~AA

rnarLFka p rr~ rSya x`g~.kh;kr~

fof/kiwoZde~A

ikrkyk[;a bna ;a=a Hkkf"kra 'kaHkquk

Lo;e~AA

& jlpaMk'kq ] iwoZ[kaM

610 rs 614

& jlizdk'k lq/kkdj ] v/;k; 10

Dig one hand depth ( Hastapramanam ) pit in ground and placed one

'Mritapatra' in it ( Mritapatra is the special type of soil pot ). At the upper end of this

Mritpatra the other Mritpatra having porous ( Sachhidra ) bottom can be placed. In

this Mritpatra the seeds from that oil can be extracted is kept. Then the joint of two

Mritpatra means the upper end of lower Mritpatra and bottom of upper Mritpatra can

be packed with 'Matkapad' (Matkapad is the special packing process in Ayurveda) on

C.O.E.&T.Akola. 93
 Extraction Techniques for Various Seed Oils

the upper end of upper Mritpatra inverted 'Sharaw' is placed. The joint of sharaw

and Mritpatra packed with matkapad on the sharaw 'Ranshenya' put and burn it.

From the heat of burning Ranshenya oil extracted from the seeds like seeds of

Bakuchi and collect it in the lower Mritpatra through the porous to present at the

bottom of upper Mritpatra.

To avoid the heat loss during the process the both Mritpatra is placed

underground and source of heat is placed on the ground. So the Yantra used for the

process is known as ' patal yantra'.

Oil extracted in Ayurveda by using this process. In this process

without using any solvent only by heat oil can be extracted.

In chemical Engineering oil extracted from seeds by using solvent

like Hexan. In this process the chemical reaction may takes place in between hexan

and the seeds under the influence of heat and oil can be extracted. As the way of

solvent there may be chances of changing in the original property of seeds and its oil

extract.

While oil extraction process of Ayurveda solvent cannot be used. Oil

extracted directly from the seeds under the influence of heat. As the solvent cannot

be used the property of oil is same as the original property of seeds. In some time

solvent like Til-tail is used. By wing til-tail also the property can not be changed.

FAQ’S

C.O.E.&T.Akola. 94
 Extraction Techniques for Various Seed Oils

Q.l You are the leading exponent of " Panchakarma Chikitsa" and you have also

written books on it. We shall be very happy if you give us some message relating

Ayurveda and Chemical engineering.

Ans: Ayurveda and chemical engineering are two sides of on coin in term

of extraction by distillation. But if you are company it on solvent extraction basis

they are very much different. In solvent extraction it resin and other chemical

components get damaged which an of great use to as in Ayurveda we use plant as a

whole.

But in near future we can use chemical engineering process for

extracting oils which will not affect the basic properties of the oil.

Q.2 Is there any relation between Ayurvedic medicine extracting and chemical

engineering ?

Ans: Yes, there is a relationship between Ayurvedic medicine extraction

and chemical Engineering because they have extracted the active principle from

herbs of different useful parts such as roots, flowers, leaves, seeds and whole plant

material from this extract different tyspes of medicinal preparation such as oil can be

prepared. Even by using this process the active principle of any drug can be

extracted and collected in particular season when what drug is fully growth. Even

drug contain 8 - 10% moisture due to this moisture than can undergo spoilage if we

extrocted active principle we can avoid the useful part of that drug.

C.O.E.&T.Akola. 95
 Extraction Techniques for Various Seed Oils

According to Ayurveda oil extraction process is known as 'Tail

Nishkasan padhati. In this process by using 'Bhudhar Yantra' oil can be extracted

from seeds e.g. oil extraction from 'Bhallatak Beef'.

This process consists of a pit of size 3 feet deep dug in the earth such

that two large size earthen pots are placed one upon other. The seeds are implanted

on the bottom of upper pot which is perforated by providing multiholes on it. On the

upper portion of upper earthen pot, heat is generated by burning natural fuel like

dungcake and dry grass. The heat get into the upper earthen pot and the oil is

extracted from the seed which then by the effect of gravity falls in the lower pot. In

this way oil is extracted from seeds by thermal effect in Ayurveda.

Q.3 Can we use solvent extracting process in Ayurveda ?

Ans: Up till now we had not used any of solvent rather than our oils. But if

the solvent is not affecting the properties and chemical compaction than this is no

harm in very it. But its chemical analysis of solvent should be known.

Q.4 Will, Using solvent extraction be against Ayurvedic principles ?

Ans: I can't justify it as I had now used it but if the solvent used is not

charmful as work's as a catalystic i.e. without taking part in the reaction than it is O

kay.

C.O.E.&T.Akola. 96
 Extraction Techniques for Various Seed Oils

In our Ayurvedic process the principle applied is to nulify the

unwanted effect of the oil for example we use babach oil for treatment of skin

diseases. We use it with till oil to nullify the itching effect of Bavanchi.

Q.5 If the solvent is 100% separated at the end of process, will it be economical?

Ans: It is economical offcourse but, as I previously mentioned it should not

disturb the properties of oil. We give more stress of quality than on quantity.

Q.6 The rotocell, Kenedy extractor. Ballman extractor are modern equipments for

obtaining oil from seeds ( Miscuea ). Are they being used for Ayurvedic

preparations?

Ans: We are using our conventional method but for large scale production

company like Baidyanath may use this process.

Q.7 Kindly tell us something about Bawanja oil extraction and Kadu Badam oil

extraction and its various uses.

Ans: Bavanchi and Kadu Badam oil is used as medicines for skin diseases.

The powder of Bavanchi is used in soap for skin care and kadubadam is used in

herbal shampoos for hair care.

Q 8 Kindly explain in brief oil extraction method in Ayurveda.

Ans: Dig one hand depth (Hastapreamanam) pit in ground and placed one

‘Mritpatra’ in it. Mritpatra is the special type of soil pot. At the upper end of this

C.O.E.&T.Akola. 97
 Extraction Techniques for Various Seed Oils

Mritpatra the Mritpatra having porous (Sachhidr) bottom can be placed. In this

Mritpatra the seeds from that oil can be extracted is kept. Then the joint of two

Mritpatra means the upper Mritpatra can be packed with ‘Matkapad’ (Matkapad is

the special packing process in Ayurveda) on the upper end of upper Mritpatra

inverted ‘Sharaw’ is packed. The joint of sharaw and Mritpatra packed with

Matkapad on the Sharaw ‘Ranshenya’ put and burn it. From the heat of burning

Ranshenya oil extracted from the seeds like seeds of Bakuchi and collect it in the

lower Mritpatra through the porous present at the bottom of upper Mritpatra.

Q.9 Is there any research paper published for the above mentioned oil extraction?

Ans: First of all we prepare the decoction by taking 16 parts water and 4

parts seeds and evaporate it till the solution becomes 4 parts and then treat it with til

oil.

Q.10 There are many methods for calculating yield, number of stages of oil

extraction in chemical engineering. These are both graphical and analytical.

Can these be used for large scale extraction of oil from seeds?

Ans: Yet not published specially for this type of research.

Q.11 What are " Asavas " and " Arishtas"?

Ans: The kwath or swaras of a drug is subjected to Sandhan Karma so that

the drug can be used for longer time. In the Sandhan Karma of decoction of a drug is

filtered, after that gud and dhatki flower is added and kept untouched for 1 month the

result is called as Arishta.

C.O.E.&T.Akola. 98
 Extraction Techniques for Various Seed Oils

The swaras is used instead of decoction then the resultant is called as

Asvas.

In this process various chemical constituents including alcohol I

generated.

Q.12 Adaspaban Yantra, Triyak patan yantra, Valuka yantram were the batch

distillation methods of earlier days. In Chemical Engineering most modern and

highly aumated equipments are used. Can you throw some light on this aspect.

Ans: 1. Adaspatan Yantra -

vFkks/oZHkktus fyIrLFkkfirL; tys lq/kh%A

nhIrSoZuksiyS% dq;kZn/k%ikra iz;Rura%AA

& j- j- l- v- 9&9

In this procedure the two Ghata ( Soil pot ) is taken as shown in

diagram. In the upper Ghata substance placed at the bottom and at the lower Ghata

water can be taken. On the upper ghata Ranshenya put and burn it. By this heat the

steam of medicinal substance is collected at the bottom of water.

C.O.E.&T.Akola. 99
 Extraction Techniques for Various Seed Oils

2. Tiryaka patan Yantra

f{kisnzla ?kVs nh?ksZ urk/kksuky la;qrsA

rUukya fuf{kisnU;?kV dq{;Urjs [kyqAA

r= #/ok e`nk lE;Xonus ?kV;ksjFkA

v/kLrknzldqEHkL; Toky;s&rhozikode~AA

brjkfLeU?kVs rks;a izf{kisRLoknq 'khrye~A

fr;Zd~ikruesrf) okfrZdSjfHk/kh;rsAA & j- j-

l- v- 9&10 rs 12

In this type of Yantra two ghata is placed as shown in diagram.

Medicinal substance from that Arka ( extract ) is want is kept in bigger size of ghata

and heat it the steam of medicinal substance is collected in small ghata having

through a tube. Small ghata is placed in water bath.

C.O.E.&T.Akola. 100
 Extraction Techniques for Various Seed Oils

3. Valuka Yantra

ljlka xw<oD=ka e`}L=kM~‐xqy?kuko`rke~A

'kksf"krka dkpdy'kha f="kq Hkkxs"kq

iwj;sr~AA

Hkk.Ms forfLrxEHkhjs okyqdklqizfrf"Brke~A

rn~Hkk.Ma iwj;s f=fHkjU;kfHkjoxq.B;sr~AA

Hkk.MoD=a ekf.kd;k laf/ka fyEisUe`nk

ipsr~A

pqYY;ka r`.kL; pknkgkUef.kdk i`"BofrZu%A

,rf) okyqdk;U=a r|U=a yo.kkJ;e~A

iTpk<okyqdkiw.kZaHkk.Ms fuf{kI; ;Rur%A

iP;rs jlxksykFkZ okyqdk;U=ehfjre~AA

& j- j- l- v- 9 & 36 rs 39

In this type Mritpatra ( Soil pot ) as shown in fig. is kept this

Mritpatra is fill up with sand. At the centre of this Mritpatra a glass bottle with

medicinal substance is kept. The 3/4th portion of this bottle is placed empty. Then

this Mritpatra heat. After slow heating medicine can be prepared.

C.O.E.&T.Akola. 101
 Extraction Techniques for Various Seed Oils

Q.13 Can Students of Chemical engineering ( Final Year) take up project work in

collaboration with R T Ayurvedic College?

Ans: Yes. We will definitely help them.

CONCLUSION

“Necessity is the mother of invention”, as it is rightly said, this project

work tries to justify it. In growing urbanization and pollution, health problems such

as skin diseases are causing increased threats.

As described previously some essential oils like bavanchi can prove

to be a great boon in future. These essential oils can be lifelong sources for different

medicines.

We have tried to apply chemical engineering methods, especially

solvent extraction for the extraction of different oils. Ayurvedic oils and other

medicines have had an advantage over allopathic medicines.

Thus this project was undertaken with a foresight to support

Ayurvedic medicines using modern chemical engineering methods.

C.O.E.&T.Akola. 102
 Extraction Techniques for Various Seed Oils

BIBLIOGRAPHY

1. Industrial oils and fats – Volume 3 -------Bailey

2. Wealth of India- Volume 3,5 & 7.

3. Dravyagoon Vidnyan ------Acharya Priyvrat Sharma

4. Rasshatra------Dr. S. S. Vaidya.

5. Chemical Reaction Engineering - Vol . 7

6. Machine Design ------ M.V.Joshi

7. www.essentialoils.com.

C.O.E.&T.Akola. 103