(12) INTERNATIONAL APPLICATION PUBLISHED UNDER THE PATENT COOPERATION TREATY (PCT)

(19) World Intellectual Property Organization

International Bureau
(10) International Publication Number
(43) International Publication Date
24 June 2010 (24.06.2010) WO 2010/069028 Al

(51) International Patent Classification: (81) Designated States (unless otherwise indicated, for every
A61K 8/73 (2006.01) A61K 8/99 (2006.01) kind of national protection available): AE, AG, AL, AM,
A61K 8/97 (2006.01) A61Q 13/00 (2006.01) AO, AT, AU, AZ, BA, BB, BG, BH, BR, BW, BY, BZ,
A61K 8/98 (2006.01) BOlD 21/01 (2006.01) CA, CH, CL, CN, CO, CR, CU, CZ, DE, DK, DM, DO,
DZ, EC, EE, EG, ES, FI, GB, GD, GE, GH, GM, GT,
(21) International Application Number: HN, HR, HU, ID, IL, IN, IS, JP, KE, KG, KM, KN, KP,
PCT/BR2009/000437 KR, KZ, LA, LC, LK, LR, LS, LT, LU, LY, MA, MD,
(22) International Filing Date: ME, MG, MK, MN, MW, MX, MY, MZ, NA, NG, NI,
18 December 2009 (18.12.2009) NO, NZ, OM, PE, PG, PH, PL, PT, RO, RS, RU, SC, SD,
SE, SG, SK, SL, SM, ST, SV, SY, TJ, TM, TN, TR, TT,
(25) Filing Language: English TZ, UA, UG, US, UZ, VC, VN, ZA, ZM, ZW.
(26) Publication Language: English
(84) Designated States (unless otherwise indicated, for every
(30) Priority Data: kind of regional protection available): ARIPO (BW, GH,
PI 0809061-0 18 December 2008 (18. 12.2008) BR GM, KE, LS, MW, MZ, NA, SD, SL, SZ, TZ, UG, ZM,
ZW), Eurasian (AM, AZ, BY, KG, KZ, MD, RU, TJ,
(71) Applicant (for all designated States except US): ASSES- TM), European (AT, BE, BG, CH, CY, CZ, DE, DK, EE,
SA INDUSTRIA COMERCIO E EXPORTACAO ES, FI, FR, GB, GR, HR, HU, IE, IS, IT, LT, LU, LV,
LTDA [BR/BR]; Rua Cardoso Quintao, N° 110 - Thomas MC, MK, MT, NL, NO, PL, PT, RO, SE, SI, SK, SM,
Coelho, 2 1381-460 Rio de Janeiro (BR). TR), OAPI (BF, BJ, CF, CG, CI, CM, GA, GN, GQ, GW,
ML, MR, NE, SN, TD, TG).
(72) Inventor: BARRETO, Daniel, Weingart; Rua Marques
de Sao Vicente, N° 208, Gavea, 2245 1-040 Rio de Janeiro Declarations under Rule 4.17:
(BR).
— as to the identity of the inventor (Rule 4.17 (ϊ))
(74) Agent: CELIA NOVAES & ASSOCIADOS S/C
Published:
LTDA; Rua pedro Lessa, N° 35, Gr 1201-1206, Centra,
20030-030 Rio de Janeiro (BR). — with international search report (Art. 21(3))

(54) Title: PROCESS FOR MANUFACTURING PERFUMES AND COLOGNES AND FOR PURIFYING AND POLISHING
ALCOHOL

Filter media Filter media

FIG. 1A
FIG. 1B

(57) Abstract: A process for obtaining perfumes, colognes and purified alcohol based on the utilization of compositions contain
ing natural hydri-colloid-forming polysaccharides obtained from animal, plant and microbial sources as well as polysaccharides
that are modified chemically or physically which added to hydro-alcoholic solutions, in combinations or not, lead to the floccula-
tion and improvement of sensorial characteristics of the end product, reducing the time taken for maturing and allowing the pro
cess to be performed at room temperature and improving the removal of substances that interfere on the perception of the scent
notes of the fragrance. The composition may be applied in the manufacture of perfumes, hydro-alcoholic solutions, alcohol for
special uses and other solutions and are particularly useful for accelerating the polishing and maturing of perfumes and colognes.
 PROCESS FOR MANUFACTURING PERFUMES AND COLOGNES AND
FOR PURIFYING AND POLISHING ALCOHOL
Field of the invention
This invention involves a new process for producing perfumes and
colognes and for purifying and polishing alcohol with natural hydrocolloids
obtained from animal, plant or microbes to be used as clarifying agents and
for improving the sensorial aspects of hydro-alcoholic solutions. The product
have particularly wide application in the perfume industry and can be used for
the removal of undesirable substances though preserving the essential
characteristics of the final product.
Background of the invention
Until present the procedure for manufacturing perfumes generally
starts with the extraction of scents from flowers, fruits, barks, seeds,
exudates and other plant parts and products. The extract may be later
subjected to purification procedures. These natural extracts and synthetic
substances are combined at specific proportions by professional perfumers,
in order to reach the right sensorial effect, resulting in the creation of
exclusive formulas, having unique fragrances defined by the perception of
scent notes. The final product is the result of the dilution of this formula of
scented ingredients in a mixture of ethanol and water in concentrations that
can vary between 2 and 20 % of the concentrated formula. Other non-
scented components may also be added to the mixture in order to alter its
original color, improve its stability or add other properties to the product.
Many of the natural components of the perfume formulas contain a
series of impurities which need to be removed from the final product so that
the perfume reaches the level of purity, the scent quality and the level of
transparency that are required.
When the fragrance concentrate is added to the polar mixture of
ethanol and water the non-polar impurities precipitate as very fine particles
that tend to form a stable suspension. The composition of such particles
depends on the concentration of the concentrate and its physical and
chemical properties may vary significantly. Frequently the impurity particles
appear as paste matters or as liquid droplets. The usual procedure adopted
for the removal of such particles is through filtration which may be done by
different techniques and with the use of various equipments. When the
impurities appears as paste or liquid materials its removal may require a
cooling stage which may take a few hours or up to several days. This leads
to the aggregation and solidifying or the particles allowing for an easier
retention in the filters. The removal of non-soluble, finely spread particles in a
suspension is also known as the polishing of the solution.
Besides the non-soluble impurities the solution containing the scented
ingredients in water and ethanol also contain molecules having odors that
interfere in the final perception of the fragrance. The removal of such
molecules is achieved through traditional techniques involving the
maintenance of the solution in still conditions for a certain period of time
allowing for the progression of reactions of condensation and oxidation which
leads to chemical changes of these molecules preventing the, otherwise,
resulting interference on the perception of the different fragrance components
which were originally planned by the perfumer. This procedure is known as
fragrance maturing and may also involve the refrigeration of the mixture.
Therefore, traditional techniques used in perfume manufacturing
involve stages of scent concentrate preparation, solubilization of the formula
components in a hydro-alcoholic mixture, resting (maturing), refrigeration,
filtration and bottling. Conditions adopted for each stage are determined by
the manufacturer, taking into consideration the perfume composition and the
quality requirements as defined by the manufacturer and the market. Stages
of maturing and refrigeration are critical for the process and may be highly
costly for the manufacturer, as they involve investing in the acquisition of
expensive equipment, keeping the product that is being manufactured in
storage for long periods of time, as well as significant expenses in energy for
refrigeration.
Prior Art
Several clarification products have been utilized in the beverage
industry which faces problems that are similar to those faced by the perfume
industry.
The Brazilian patent document Pl 9700752-8 describes a composition
obtained from seaweeds of the class RHODOPHYCEAE, which is rich in
polyeiectrolyte biopolymers, which, when added to hydro-alcoholic solutions
that are contaminated with waxes, resins or phospholipids, triggers a
flocculation process through polymeric bridges and, in the conditions found at
hydro-alcoholic medium, forms a micro-net that is responsible for the sweep-
fiocculation leading to the clarification and polishing of the solution. Such
mechanism, acting in combination with the results obtained experimentally,
indicate a wide range of potential applications of these products in many
different areas of knowledge.
The patent document WO 98/000519 describes the use of a colloidal
composition as a clarification agent and finishing of beverages produced by
fermentation such as various kinds of beer, wines, low alcohol content
beverages and their by products. The addition of Isinglass (collagen
produced from fish) to beer is commonly used as a manner to promote its
clarification and improving the efficacy of filtration. The composition
described in that document includes polysaccharides such as pectin and may
contain cooperating agents such as silicates. Those substances have
nevertheless proven to be harmful as they may provoke allergic responses to
the consumers and they also alter the original characteristics of the
beverage.
The patent document WO 2006/032088 describes a special kind of
pectin, obtained from plants, a non-allergenic polysaccharide which when
added to beverages promotes their clarification at a level equivalent or even
superior to that obtained through the use of Isinglass. The technique involves
the use of this pectin combined with an SO2 donor, such as sodium or
potassium metabisulfrde, at a proportion of 3,5 to 7,5 : 1, preferentially at 5:1.
Nevertheless, these clarification agents, in most cases interfere on the
characteristics of the final product, modifying its aroma, taste or color.
The objective of the present invention is of introducing a new process
for manufacturing perfumes and colognes as well as purifying the alcohol
used in their manufacturing. This process is capable of promoting their
clarification within a short period of time, at room temperature, and is also
capable of improve the removal of undesirable components that interfere in
the fragrance without altering the sensorial features planned for the perfume
or cologne.
Summary of the invention
This invention involves a process of obtaining perfumes and colognes
and is based in the use of natural hydro-colloid-forming polysaccharides,
which are obtained from animal, plant or microbial sources as well as from
polysaccharides chemically or physically modified which are added to hydro-
alcoholic solutions in combinations or not and act as flocculation agents and
improving the sensorial features of the product, reducing the maturing time
to a few hours even under ambient temperatures and helping with the
removal of substances thai interfere in the perception of the scent notes of
the fragrances. In cases where the addition of different hydrocolloids in the
solution, the first product may have the purpose of removing the undesirable
components that are dissolved or suspended in the solution whereas the
second product may serve as inducing agent leading to the formation of
denser and more consistent flakes which are easier to remove from the
solution.
The components that are the object of the present invention may be
applied in the manufacture of perfumes, hydro-alcoholic solutions, alcohol for
special uses, as well as other solutions, and are particularly useful at
accelerating the polishing and maturing of perfumes and colognes.
Brief Description of the Figures
Figure 1 shows a scheme representing the removal of particles
comparing the mechanisms involved in the traditional method (FIG. 1A) with
the new process that utilizes hydrocolloids (FIG. 1B).
Figures 2A and 2B show Graphs 1 and 2 which compare the results
obtained with the traditional process (Graph 1) with those obtained through
the application of the newly invented process (Graph 2).
Figure 3 shows the chromatograms where the composition of a
perfume prepared traditionally (FIG. 3A) is compared with that of a perfume
produced by utilizing the newly invented method involving hydrocolloids (FIG.
3B).
Detailed Description of the Invention
The process for obtaining the hydro-colloid compositions are not part
of the invention but will be described herein in order to illustrate the
properties and the general characteristics of the products involved.
In order to obtain the hydrocolloids from seaweeds, the algae are
firstly washed and dried and subjected to a cleaning treatment with nitric acid
or hydrochloric acid in concentrations which may vary from 0.5% to 5.0%, for
a period of at least 10 minutes, under temperatures which may vary from 50C
to 4 O0C , depending on the degree of calcification of the algae. These are
later washed in a neutralizing solution containing a selected hydroxide which
may be calcium, sodium, potash or ammonium or their respective carbonates
or bicarbonates at concentrations that may vary from 0.2% to 5.0%, for
minimum periods of 10 minutes, under temperatures that may vary from 50C
to 400C. The excess of neutralizing agent is removed in flowing water and the
algae are then subjected to the extraction process by utilizing pure water as
the solvent or water solutions containing mineral salts, alcohols or glycols in
proportions that may vary according to the algae to be treated under
temperatures which may vary from 5 O0C to 1200C, for periods varying from
20 minutes up to 2 hours. The volume of the extracting liquid is kept
constant, if necessary through condensation and reflux. The resulting extract
is then filtered or centrifuged for the removal of insoluble residues.
Hydrocolloids from animal sources may be obtained from shrimp and
similar crustacean, usually as residues from seafood processing industries.
This raw material is treated in order to remove coarser residues and is
subjected to a demineraiization treatment with an acid solution at
concentrations ranging from 2.5 % to 10.0 %. The calcium-rich acid solution
is discarded and the demineralized residue is then extracted with a solution
of sodium hydroxide at 5 % for the removal of the proteins. The alkaline
protein solution is removed, the solid materials are washed with water until a
neutral pH is reached and is then treated with a sodium hypochlorite solution
containing 0.3 to 6 % of active chlorine for the removal of color and odor. The
polysaccharide hence obtained is chitin which is then treated with a
concentrated sodium hydroxide solution at 600C for 2-4 hours until its
deacetylation. The raw chitosan is dissolved into an aqueous acetic acid
solution, the non-soluble impurities are removed by filtration and the clear
solution is precipitated by adding a 8% sodium hydroxide solution to it. The
pure chitosan that precipitates is washed in water until a neutral pH is
reached. This is then dried and ground. The chitosan solution used in the
newly described process can be prepared by adding water or acid solutions
to the dried chitosan at concentrations that are adequate for obtaining the
solution that is needed.
Pectin hydrocolloids can also be obtained from fruits such as apples -
whole fruits, apple peels and residues obtained from the apple juice industry
may serve as raw material. The dry materials are treated with a hot acid
solution at temperatures that may vary from 60 to 100 0C. The acid solution
may be prepared from mineral or organic acids and should have a pH
between 1.5 and 3.5. Depending on the conditions of the raw material and
the characteristics needed for the pectin the extraction may take 30 minutes
up to several hours. Subsequently the material is filtered through activated
charcoal for color removal, it is vacuum concentrated and is then precipitated
in ethanol. The precipitated pectin is removed by filtration, washed in ethanol
and left to dry. The dry pectin is ground and, depending on the intended end
use, mixed with calcium salts or organic acids. The pectin solution utilized in
the newly invented process may be prepared by simply adding water to dry
pectin readily available in the market at the appropriate concentrations.
In order to obtain hydrocolloids from gum Arabic or gum acacia the
raw gum obtained from the exudate from trunks of acacia tree (Acacia
Senegal) is dissolved in water and filtered for the removal of insoluble
impurities, clarified with activated charcoal and filtered once again as to
obtain a transparent solution. This solution can be used directly in the
process of fragrance production or it can be spray-dried or concentrated and
precipitated with ethanol, filtered and dried. The gum arabic solution is used
in the newly invented process by the simple addition of water to the gum at
concentrations that are adequate for obtaining the hydro-colloid solution
needed for the process.
Obtaining hydrocolloids from guar seeds {Cyamopsis tetragonolobus)
involves removing the hulls, grinding and sieving them in order to obtain a
powder. The fine powder is then suspended in ethanol for removal of
additional impurities, filtered and dried. The solution of gum guar used in the
newly invented process may be prepared by simply adding water to the dried
gum at concentrations that are adequate for obtaining a solution of
hydrocolloids adequate for the process.
In order to obtain hydrocolloids from the bacterium Xanthomonas
campestris, a culture medium containing an aquous solution of sucrose,
peptone, urea, potassium hydrogen phosphate, iron chelated with EDTA and
magnesium salts is seeded with a suspension of X. campestris and left to
ferment in aerated conditions under continuous agitation under a temperature
of 28°C for 5 days. The gum produced by the bacterium is precipitated with
ethanol 98°GL, and is then dried and ground. The solution of xanthan gum
used in the newly invented process may be prepared by simply adding water
to the dried gum at adequate concentrations in order to prepare the hydro-
colloid solution to be used.
The particle removal mechanism is presented in Fig. 1, included in this
report as one of its parts and illustrates how the traditional and the newly
invented process compare.
When the filtering medium is placed transversally to the direction of
the flow and the traditional method is used (FIG. 1A), smaller particles pass
through the filter pores and "soft" particles clog the filter pores or deform and
pass through the filter media.
When hydrocolloids are used the particles are captured by the
polymeric net and are trapped in the flakes allowing them to be intercepted
by the filters (FIG. 1B).
The compositions obtained, according to the newly invented process,
act in hydro-alcoholic perfume solutions or in alcohol for removal of particles
in suspension as double-effect flocculating agents, hydrocolloids such as
those previously mentioned as examples as well as others that are also
adequate but haven't been mentioned form a complex mesh with waxes,
phytoesterols and other non-scented components that are present in the
fragrance raw materials and flocculation occurs due to the intra-molecular
polymeric bonds, combined with the formation of an immobilizing micro-net.
As a result the particles are incorporated in the polymeric flakes and dragged
to the bottom of the maturing tank and can then be removed by filtration.
The performance of the compositions produced according to the
process of the present invention removing odorous molecules which interfere
with the final perception of the fragrance from the scented water-alcohol
solutions or from the alcohol used their formula can be explained by two
possible mechanisms: the formation of charge complexes between the
odorous molecules and the functional groups of the hydrocolloids or the
formation of chemical derivatives between low-molecular weight odorous
molecules such as acetaldehyde, present in ethyl alcohol, and functional
groups present in the hydro-colloid molecules. Aldehydes such as
acetaldehyde may form polymeric ketals or other derivatives with the
hydroxyI groups of the hydro-colloid. Removal of the flakes formed by the
insoluble hydrocolloids then leads to the removal of the odorous molecules
which interfere on the perception of the notes from the perfume solution or
from the alcohol. This invention then makes it unnecessary the long periods
of maturing of the mixture that leads to the removal of such molecules,
mainly by oxidation of aldehydes, which are traditionally utilized.
Fragrance formula compositions vary significantly between different
perfumes and so does the quality of the alcohol provided by each
manufacturer. Therefore the amount of the components included in the
composition of the new invention required for the removal of impurities needs
to be determined experimentally for each product being treated. Quantities of
hydrocolloids between 0.5% and 3% in relation to the hydro-alcoholic solution
have been shown to be sufficient in most cases. When the addition of two
different hydrocolloids is necessary amounts of the first component between
0.5 to 3% and of around 5% of the second component measured in relation
to the first component have been shown to be sufficient in most cases.

In order to have the efficiency and benefits of the newly invented

process properly evaluated some of the experiments that have been
performed will be presented next as examples. These serve only to illustrate
the invention and do not represent any form of limitation to the invention.
Similarly, examples are presented of applications of the newly invented
process.

Example 1: Increase in the efficiency of removal of suspended insoluble

particles through the application of the newly invented process.
The efficiency of the process involving the utilization of the
composition of the present invention was demonstrated through a series of
experiments where it was possible to evaluate and compare the efficiency of
the traditional method with the new process that utilizes the addition of
hydrocolloids for the removal of insoluble particles that are responsible for
the final turbidity in perfumes.
A perfume was produced by utilizing the traditional system by
adding 10 grams of the aroma concentrate to 90 mL of a hydro-alcoholic
solution with 85 % of alcohol and 15 % of water. The resulting mixture was
homogenized and then filtered through a conventional filter lined with two 3µ
filter paper sheets and then through two 1µ filter paper sheets. The resulting
filtrate was then placed under refrigeration at 4°C in order to evaluate the
possible occurrence of precipitation after the filtration.
For the perfume produced with the composition described in the new
invention 10 grams of the aroma concentrate to 90 mL of a hydro-alcoholic
solution with 85 % of alcohol and 15 % of water and then 2 grams of a
solution of hydro-colloid obtained from red seaweeds were added to the
mixture. The mixture was then homogenized and 0.1 grams of a saline
solution of hydrocoHoids obtained from brown seaweeds were added. The
resulting mixture was homogenized and then filtered through a conventional
filter lined with two 3µ filter paper sheets followed by filtering through two 1µ
filter paper sheets. The resulting filtrate was then placed under refrigeration
at 4°C in order to evaluate the possible occurrence of precipitation after the
filtration.
Turbidity of the two solutions was then analyzed through
spectrophotometry by evaluating their absorbance under different times of
maturing. Absorbance measurements were made with a spectrophotometer
HACH mod. 4000U, at 265 nm.
Graphs shown in Figures 2A and 2B show the benefits that were
reached when the process and composition of the present invention was
utilized. Figure 2A ( Graph 1) shows the results of the experiment obtained
without the use of the composition of the invent and Figure 2B (Graph 2)
shows the results of the experiment where the newly invented process was
used.

Even after a month of rest under refrigeration, when the traditional

method of maturing was used (Graph 1) the solution still had a turbidity of
70%. On the other hand, when the newly invented process was used
(Graph 2) a significantly more efficient removal of the impurities occurred
immediately after the treatment. It is also noteworthy that samples that were
submitted to the conventional process still had a cloudy appearance after
four months of having been manufactured.

Example 2: Preservation of the components of the perfume after the

application of the newly invented process
The purpose of this assay was that of verifying the state of
preservation of the perfume components after processing with the
hydrocolloids as described in the invention.
The comparative analysis of the perfume composition prepared with
the traditional process with that obtained by applying the hydro-colloid
composition and the process described in the new invention was made with
High Resolution Gas Cromatography. A cromatograph HP 5890 series II,
equipped with a column DB-1 of 30 m , film thickness of 1 µm and internal
diameter of 0.25 mm, with Helium as carrier gas at a 50 cm/min flow rate was
utilized. Analysis were performed with temperature starting at 100 0C and the
rate of temperature increase was of 10°C/min until reaching a maximum of
250 0C, with maintenance at this temperature.
Resulting chromatograms can be seen in FIGS 3A and 3B included in
this report.

As can be observed when the chromatogram resulting from the

analysis of the composition of the perfume manufactured traditionally (FIG.
3A) is compared with that obtained for the perfume prepared with the hydro-
colloid composition, as described in the new invention (FIG. 3B) it is clearly
demonstrated that the use of the newly invented process removes the
insoluble components from the hydro-alcoholic mixture but does not alter the
composition of the volatile components which are essential for the perfume.

Example 3: Efficiency of the application of the newly invented process

on the perfume stability
The purpose of this essay was checking the efficiency of the hydro-
colloid composition, as described in the new invention, regarding the
parameters of stability of the end products. Table I (see below) shows the
results of the comparative analysis of the stability of a perfume prepared by
following the traditional process and those of a perfume prepared by utilizing
the hydro-colloid composition as described in the newly invented process.
Perfume stability tests were performed under different conditions and
any changes in perfume properties were recorded for the time lapse since
manufacturing when it occurred. Results have clearly shown that the
preparation of a perfume involving the use of the newly invented process with
hydrocolloids generates a transparent and stable perfume under a range
storage conditions as early as 24 hours after manufacturing whereas the
perfume prepared following the traditional procedure remained cloudy even
after 90 days of it having been manufactured.
 TABLE (I)

Example 4: Sensorial performance of the perfume after the application

of the newly invented process
The objective of this essay was that of verifying the sensorial
performance of a perfume prepared by using the newly invented process
involving hydrocolloids that provoke flocculation and hence accelerate
perfume maturing.
For this particular study three traditional scent families were included.
These are known by perfumists as "Fresh Fougere", "Fresh Floral Fresco
with Green and Woody notes" and " Floral Floral", and are regarded as
representing various fine perfumes. Perfumes were prepared by using
identical preparations of each of the perfume concentrates belonging to each
of the three scent families. These perfumes were prepared either by following
the traditional technique or by following the newly invented process. Scent
attributes were evaluated by a panel including trained experts and
perfumists. The results are presented below in Table II.
TABLE (II)

The results that were obtained demonstrate that the preparation of a

perfume that follows the newly invented process yields products that have a
better olfactory performance and preserves and highlights the most valuable
olfactory notes giving the perfume a higher degree of harmony.

Example 5: Sensorial performance of perfumes prepared with alcohol of

different origins and degrees of purify after being subjected to the
newly invented polishing process
One of the critical aspects in the production of high quality perfumes is
the choice of the alcohol to be used in the perfume formulation. It is known
that the level of purity in the alcohol that is chosen affects directly the
olfactory performance of the perfume. This limitation causes many problems
for the perfume manufacturers which are often restricted to a rather limited
range of choices for this fundamental raw material.
This study deals with the evaluation of the influence of the treatment of
alcohol with the newly invented process on the sensorial performance of
perfumes prepared with alcohol of different origins and degrees of purify.
For this study two traditional scent families were chosen. These are
known by the perfumers as "Fresh Fougere" and " Floral Floral", and are
regarded as representative of numerous fine perfumes.
Perfumes were prepared by using identical preparations of each of
the perfume concentrates belonging to each of the two scent families. These
perfumes were prepared with alcohol of three different sources, named
manufacturers 1, 2 and 3 . Experts ranked the alcohol produced by the three
manufactures in a decreasing order of sensorial quality for the production of
fine perfumes, in terms of presence of interfering odorous substances.
Therefore alcohol from manufacturer 1 was regarded as "premium" alcohol,
alcohol from manufacturer 2 was considered as slightly inferior or "second
choice" whereas the alcohol from manufacturer 3 was considered as inferior
and inadequate for the production of fine perfumes. These were prepared
either by following the traditional technique or by following the newly invented
process. Scent attributes were evaluated by a panel including experienced
evaluators and perfumers. The results are presented below in Boxes 1 and 2
below.
The results obtained for this essay clearly shows that the preparation
of a perfume involving the use of the newly invented process improves the
olfactory performance of the perfume removing the sharp notes that usually
remains from the impurities contained in poor quality alcohol preserving the
valuable olfactory notes and upgrading the perfume harmony even when
such low quality alcohol are used in their preparation.
 Box 1

Box 2

The following examples have the purpose of illustrating several

possibilities of applications of the newly invented process.

Example 6: Perfume manufacturing process based on the utilization of

a flocculation system promoted by seaweed hydrocoHoϊ ds
The adoption of the newly invented system is rather simple and allow
increasing perfume production even in smaller scale, in simpler and less
expensive manufacturing plants it reduces the need of further investing in
equipment and reduces the energy expenses for refrigeration of the solution
during production. Besides that, the process allows the manufacturer to
preserve the original composition of the perfume, to maintain and highlight
the valuable scent notes and also improves the perfume harmony. The new
process also helps the experts involved in formulation by reducing the
restrictions related to the type of alcohol that may be used in the perfume
manufacture.

The fragrance concentrate is placed in a tank where it is mixed with

water and alcohol. 20 ml_ of a solution of hydrocolloids obtained from red
seaweeds are added under continuous agitation for each liter of the perfume
solution as well as 1 ml_ of a solution of brown seaweed hydrocolloids. The
solution is left to rest at room temperature. Depending on the fragrance the
time needed for complete formation of the flakes can vary from 2 to 12 hours.
After the flake-forming process ends the raw product is filtered through a
common filter lined with 14 micra porosity filter paper. The transparent
perfume is then bottled. As an alternative, and depending on the fragrance
that is being used filter papers with porosity varying between 0.5 and 30
micra may be used. Depending on the production scale of the perfume or
colony different filtration industrial equipments may be used such as bag
filters, press filters, cartridge filters, basket filters and the like, as well as
associations of these different equipments.

Example 7: Perfume manufacturing process based on the utilization of

a flocculation system promoted by apple pectin

The fragrance concentrate is placed in a tank where it is mixed with

water and alcohol. To the perfume solution 30 mL of an aqueous solution of
apple pectin at 1% for each liter of the perfume solution are added under
continuous agitation. The solution is left to rest at room temperature.
Depending on the fragrance the time needed for complete formation of the
flakes can vary from 2 to 12 hours. After the flake-forming process ends the
raw product is filtered through a common filter lined with 14 micra porosity
filter paper. The transparent perfume is then bottled. As an alternative, and
depending on the fragrance that is being used filter papers with porosity
varying between 0.5 and 30 micra may be used. Depending on the
production scale of the perfume or colony different filtration industrial
equipments may be used such as bag filters, press filters, cartridge filters,
basket filters and the like, as well as associations of these different
equipments.

Example 8: Perfume manufacturing process based on the utilization of

a flocculation system promoted by Xanthomonas campestris (xanthan
gum) hydrocolloids

The fragrance concentrate is placed in a tank where it is mixed with

water and alcohol. To the perfume solution 10 ml_ of an aquous solution of
Xanthan Gum at 1%for each liter of the perfume solution are added under
continuous agitation. The solution is left to rest at room temperature.
Depending on the fragrance the time needed for complete formation of the
flakes can vary from 2 to 12 hours. After the flake-forming process ends the
raw product is filtered through a basket filter equipped with a filter media with
a porosity of 30 microns, followed by a cartridge filter with a porosity of 1
micron, for the complete removal of the flakes that are formed. The
transparent perfume is then bottled.

Exemple 9: Manufacturing process of alcohol - perfume manufacturing

degree - through the application of a system involving flocculation with
seaweed hydrocolloids
The use of this process on low quality alcohols allows the alcohol
manufacturer or the perfume manufacturer to purify alcohol, removing
impurities that occur at low quantities in alcohol such as aldehydes, but that
interfere in the perception of fragrances in a perfume. Alcohol obtained
through this treatment has an appropriate sensorial performance and this
leads to its upgrade to perfume application degree.
Alcohol is taken to a tank where hydro-colloid solutions are added for
treatment. 30 mL of a red seaweed hydro-colloid solution is added for each
liter of alcohol under continuous agitation followed by 1.5 mL of brown
seaweed hydrocolloids. This mixture is left to rest at room temperature for 4
hours. After the flake-forming process ends the alcohol is filtered through a
basket filter with a porosity of 25 microns for complete removal of flakes.
Alcohol obtained through this process has a smoother odor and may be used
in perfume manufacturing without restrictions.
 CLAIMS
I. PROCESS FOR MANUFACTURING PERFUMES AND COLOGNES
utilizing natural hydrocolloids characterized by such hydrocolloids being
incorporated to hydro-alcoholic solutions as a clarification agent and for
improvement of the sensorial features of such hydro-alcoholic solutions.
2. PROCESS FOR MANUFACTURING PERFUMES AND COLOGNES
as in claim 1 , characterized by such hydrocolloids being obtained from
animal, plant or microbial sources.
3. PROCESS FOR MANUFACTURING PERFUMES AND COLOGNES
as in claim 1, characterized bv such hydrocolloids being obtained from
seaweeds.
4. PROCESS FOR MANUFACTURING PERFUMES AND COLOGNES
as in claim 3 , characterized bv such seaweeds being selected from red and
brown algae.
5. PROCESS FOR MANUFACTURING PERFUMES AND COLOGNES
as in claim 2 , characterized bv such hydrocolloids being obtained from
Xanthomonas campestris.
6. PROCESS FOR MANUFACTURING PERFUMES AND COLOGNES
as in claim 2 , characterized bv such hydrocolloids being obtained from
fruits, fruit parts and seeds.
7. PROCESS FOR MANUFACTURING PERFUMES AND COLOGNES
as in claim 1, characterized bv pectin from fruits, particularly from apple
being utilized as flocculating agents.
8. PROCESS FOR MANUFACTURING PERFUMES AND COLOGNES
as in claim 1 , characterized bv chitosan obtained from animals, chitosan
from crustacean sources in particular, being used as a flocculating agent.
9. PROCESS FOR MANUFACTURING PERFUMES AND COLOGNES
as in claim 1, characterized bv guar gum being used as flocculating agent.
10. PROCESS FOR MANUFACTURING PERFUMES AND COLOGNES
as in claim 1 , characterized by xanthan gum being used as flocculating
agent.
II. PROCESS FOR MANUFACTURING PERFUMES AND COLOGNES
as in claim 1, characterized bv such hydrocolloids added to hydro-alcoholic
mixtures leading to the removal of insoluble components from the hydro-
alcoholic mixture without altering its composition in terms of volatile
components of importance for the perfume.
12. PROCESS FOR MANUFACTURING PERFUMES AND COLOGNES
as in claim 1, characterized bv the addition of such hydrocolloids yielding
products which are clearer and more stable under storage.
13. PROCESS FOR MANUFACTURING PERFUMES AND COLOGNES
as in claim 1, characterized bv the addition of such hydrocolloids resulting in
products that have a better olfactory performance, preserving and
highlighting the valuable scent notes and providing a higher level of harmony
to the perfumes.
14. PROCESS FOR PURIFYING ALCOHOL characterized bv the use of
natural hydrocolloids obtained from animal, plant or microbial sources that
act as flocculating agents and lead to an improvement of sensorial
characteristics and by such hydrocolloids when added to poor quality alcohol
allowing for an upgrade of its properties to a standard that is adequate for
use in perfume manufacturing.
 INTERNATIONAL SEARCH REPORT International application N 0

PCT/BR2009/000437
A. CLASSIFICATION O F SU BJ ECT M ATTER

IPC (2010.01) A61 K 8/73 A61K8/97 A61K8/98 A61K8/99 A61Q13/00 B01D21/01

According t o International Patent Classification (IPQ or t o both national classification and IPC
B. FIELDS SEARCHED
Minimum documentation searched (classification system followed by classification symbols)

IPC (2010.01) A61K A61Q B01D

Documentation searched other than minimum documentation t o the extent that such documents are included in the fields searched

Electronic data base consulted during the international search (name o f data base and, where practicable, search terms used )

EPODOC, MEDLINE, SCIELO, BIOSYS, CHEMICAL ABSTRACTS, EMBASE 1 ELSEVIER BIOBASE, SCISEARCH

C . DOCUM ENTS CONSIDERED T O BE RELEVANT

Category* Citation o f document, with indication, where appropriate, o f the relevant passages Relevant to claims

X BR 9700752 A (BARRETO DAMIEL WEINGART [BR]) 1-3, 12, 14

08 December 1998 (1998-12-08)
Y See whole document. 4-11, 33

Y BARRETO, D.W. et al. "O uso de extratos complexos de algas Claims -14
marinhas em perfumaria". In: ASSOC Ϊ ACAO BRASILEIRA DE
COSMETOLOGIA, 1O0 ENCONTRO BRASILEIRO D E
QUIMlCOS COSMETICOS. SAO PAULO, 1996, p. 40.
See whole document.

FR 2829025 A l (OREAL[FR]) Claims 1-7, 10-

07 March 2003 (2003-03-07) 14
See p.5, 1.1 0-p.6, 1.21.

ES 2164566 Al (LIPOTEC SA [ES]) Claims 1-14

16 February 2002 (2002-02-16)
See col.2, 1.42-52.

Further documents arc listed in the continuation o f Box C . Sec patent family anne

♦ Special categories o f cited documents: "T" later document published after the internationa filing date o r
"A" document defining state o f the art which is not considered to be priority date and not in conflict with the application but cited
o f particular relevance to understand the principle o r theory underlying the invention
"E" earlier application o r patent but published o n or after the 'X" document o f particular relevance; the claimed invention cannot
international filing date be considered novel or cannot be considered to involve an
L" document which may throwdoubts o n priority claim(s) or which inventive step when the document is taken alone
is cited to statiiish the publication date of another citation or 'Y" document o f particular relevance; the claimed invention cannot
other special reason (as specified) be considered to involve an inventive step when the document
O" document referring to an oral disclosure, use, exhibition o r other is combined with one o r more other such documents, such
means combination being obvius to a person skilled in the art
"P" document published prior Io the international filing date but later "&" document member o t the same patent family
than the priority claimed '
Date of the actual completion of the international search Date o f mailingof the international search report

26 March 2010 3/M JQtO

Name and mailing address of the ISA/BR Authorized officer

1P INSTITUTO NAClONAL DA
PROPRIEDADE INDUSTRIAL
Rua MayrinkVeiga n°S, 18°andar Mauricio da Silva Martins Almeida
cep: 20090-050, Centra - RIo de Ja πelro/R J
Facsimile N": +55 2 1 2139-3663 Telephone N°: +55 2 1 2139-3686/3742
Form PCT/ISA/210 (second sheet) (July 2009)
 INTERNATIONAL SEARCH REPORT International application N°

PCT/BR2009/000437
C . DOCUM ENTS CONSIDEkKD T O B B RELEVANT

Category* Citation o f document, with indication, where appropriaic. o f the relevant passages Relevant t o claims N 0

US 5008108 A (MASSACHUSETTS INST TECHNOLOGY [US]) Claims 1-7, 9-14

16April 1991 (1991-04-16)
See whole document.

Form PCT/ISA/2 10 (continuation of second sheet) (July 2009)

 INTERNATIONAL SEARCH REPORT International application N°
Information on patent family members
PCT/BR2009/000437
Patent documents
Publication date Patent family members Publication date
cited in search report

BR 9700752 A 1998-12-08 None

FR 2829025 A l 2003-03-07 None

ES 2164566 A l 2002-02-16 ES 2164566 B l 2003-04-16

US 5008 108 A 1991-04-16 EP 0326550 A l 1989-08-09

JP 1500443 T 1989-02-16
US 4851393 A 1989-07-25
WO 8800952 A l 1988-02-11

Form PCT/ISA/2I0 (patent family annex) (July 2009)