3,039,971

United States Patent Office Patiented June 19, 1962

2
ployed as the phosphate builder and the sodium silicate
3,039,971 is employed as an anticorrosion agent. The lauryl alco
HGH-FOAM PASTE DETERGENT COMPOSITION hoi Sulfate is employed as a surfactant, while the carboxy
Leoa E. Coaera, Roselle, N.J., assigner to FMC methyl cellulose is used as an antiredeposition agent. The
Corporation, a corporation of Delaware
No Drawing. Fied June 2, 1958, Ser. No. 738,994 Sodium silicate employed may be any silicate in which
4. Claims. (C. 252-138) the NaO/SiO ratio varies between 1:3.2 to about 1:1.
preferably anhydrous sodium metasilicate, a liquid sili
This invention relates to an improved paste built cate, or sodium metasilicate pentahydrate is employed in
detergent. More particularly, this invention relates to a the formulation. Hereinafter whenever we refer to the
stable high foam paste built detergent. This invention O weight percent of the silicate employed in the formula
also relates to a process for the preparation of the paste tion, it will be understood to have been calculated as
detergent. weight percent silica.
A good built paste detergent should contain all of The formulations of this invention may contain from
the essential ingredients of a good built dry detergent about 18 to about 26 weight percent tetrapotassium pyro
formulation, i.e., a surfactant, a phosphate builder, an 5 phosphate, from about 19 to about 47 percent by weight
anticorrosion agent, and an antiredeposition agent. In lauryl alcohol sulfate and from about 35 to about 55
addition, a foam stabilizer is sometimes necessary when percent by weight water. The amount of silicate employed
a high persistent foam is desirable, and other ingredients may vary, but it is preferable to maintain it in the range
such as optical brighteners, dyes, perfumes, etc. may be of about 0.1 to about 1.7 weight percent calculated as
incorporated where desired. However, it has not been 20 SiO2. The carboxymethyl cellulose may be employed
commercially possible heretofore to incorporate these over wide ranges, but we have found it preferable to
various ingredients into a paste formulation and still ob maintain it from about 0.1 to about 3 weight percent.
tain a stable detergent. Many formulations prepared The amount of carboxymethyl cellulose which can be
heretofore have been physically unstable resulting in employed depends upon the degree of substitution of car
separation of the detergent into two or more incompati 25 boxyl groups in the molecule. The greater the degree of
ble layers, sedimentation, etc. This has been a serious substitution, the more soluble the product. However, at
detriment to commercialization of built paste detergents the higher degree of substitution, the soil antiredeposition
in the past. property may be slightly adversely affected. The carboxy
In efforts to overcome the above-mentioned disadvan methyl cellulose produced by Hercules Powder under
tages, detergent formulators have heretofore resorted to 30 the trade name "Hercules CMC 70 M' has been found to
a number of undesirable devices. Sodium silicate is dif be particularly suitable. The lauryl alcohol sulfate em
ficult to incorporate into detergent formulations and one ployed may be any high assay product, but particularly
common device is to leave out this essential ingredient good results have been obtained by using the product
or to decrease its concentration to much less than that 35
made by Du Pont under the trade name "Dupanol ME
necessary for proper protection of metal surfaces which Dry.” This product is identified in the "Du Pont Products
come in contact with the detergent. This results in exces index' as the dry sodium salt of technical lauryl alcohol
sive corrosion of metal containers and of metal Washing sulfate.
machine parts. Another device is to omit sodium car A preferred formulation of this invention is set forth
boxymethyl cellulose from the formulation resulting in in 40
below in which all of the percents are by weight:
creased greyness of fabrics laundered with such detergents. Percent
Another device is to resort to expensive combinations of Tetrapotassium pyrophosphate------------------ 20.0
specially purified surfactants with unduly large propor Anhydrous sodium metasilicate (equivalent to
tions of solubilizers such as sodium Xylene sulfonate. 1.47% by Weight SiO2---------------------- 3.0
These latter substances increase the cost of built deter 45 Carboxymethylcellulose ----------------------- 0.5
gents without contributing appreciably to detergency. Technical lauryl alcohol Sulfate----------------- 26.5
More expensive potassium containing surfactants have Water -------------------------------------- 500
also been used in place of less Soluble, less expensive so
dium-containing surfactants. It is possible to decrease the This invention also provides a procedure for the prep
cost of these built detergents by decreasing the concentra 50
aration of the desired detergent. If this procedure is not
tion of the expensive specially purified surfactants but the followed, the desired formulation is not obtained in
performance suffers. stable form. According to this process, the tetrapotassium
It is the object of this invention to provide a stable pyrophosphate is dissolved in water and the carboxy
high foam built detergent. It is a further object of this methyl cellulose is then added and is completely dispersed
invention to provide a stable paste detergent which con 55
therein. The anhydrous sodium metasilicate, or other sili
tains all of the essential ingredients of a good dry deter cate, is then added and must be completely dissolved be
gent formulation. It is another object of this invention to fore proceeding any further. Upon the complete dissolu
provide a stable paste detergent employing commercially tion of the silicate, the lauryl alcohol sulfate is added at
cheap available materials. It is another object of this this point and mixing is then continued until a pasty con
invention to provide a paste formulation capable of ex 60
sistency is obtained. After mixing is complete, the paste
trusion from a collapsible tube or for distribution in a will be rather thin and hot. The paste should not be al
jar. Furthermore, it is an object of this invention to lowed to exceed 60 degrees centigrade in temperature.
provide a process for the preparation of this stable high The proper consistency is obtained when the mix cools.
foam built paste detergent. It has been found that the best results are accomplished
with a high-speed mixer, similar in action to the Eppen
According to this invention, these is provided a stable 65 bach Homo-Mixer. This type mixer allows for mixing
high-foam built detergent paste comprising tetrapotassium the ingredients without the entrainment of air. This is
pyrophosphate, a sodium silicate, carboxymethyl cellulose, essential, since the entrainment of air causes the formula
lauryl alcohol sulfate and water. If desired, a foam tion to be unstable.
stabilizer such as fatty acid alkanol amides, water-soluble O
The detergents of this formulation are all-purpose deter
dyes and antitarnishing agents for metal Surfaces may be gents and are suitable for laundering cotton, woolen goods
included in the formulation. and fine fabrics, for cleaning hard surfaces and for other
In the above compositions, the pyrophosphate is en wetting and detergent applications.
 3,039,971
3. 4.
The detergent properties of a stable high-foam paste I claim:
detergent having the following composition 1. A high foam stable built paste detergent composition
Percent which consists essentially of from about 18 to about 26%
Tetrapotassium pyrophosphate------------------ 20.0 by weight of tetrapotassium pyrophosphate, from about
Anhydrous Sodium metasilicate.----------------- 3.0 19 to about 47% by weight of sodium lauryl alcohol
Carboxymethylcellulose ----------------------- 0.5 sulfate, from about 0.1 to about 1.7% by weight of sodi
Technical lauryl alcohol sulfate----------------- 26.5 um silicate calculated as SiO, from about 35 to about
Water -------------------------------------- 50.0 55% by weight of water and about 3% by weight of
carboxymethyl cellulose.
were tested by techniques similar to those described in O 2. A stable high foam built paste detergent composition
the manual "Detergency Evaluation and Testing' by J. C. which consists essentially of about 20% by weight of
Harris (Interscience Publishers, Inc., 1954). A single tetrapotassium pyrophosphate, about 3% by weight of
wash technique is carried out in a Launder-Ometer (Atlas anhydrous sodium metasilicate, about 0.5% by Weight of
Electric Devices Company) at 140° F., using two com carboxymethyl cellulose, about 26.5% by weight of sodi
mercially soiled cotton fabrics (Foster D. Snell Soiled 15 um lauryl alcohol sulfate, and about 50% by weight of
Cotton 159 and American Conditioning House 115) in Water.
distilled water, and with three commercially soiled fabrics 3. The method of preparing a stable high foam built
(Foster D. Snell Soiled Cotton 159, American Condition paste detergent composition consisting essentially of dis
ing House 115, and American Conditioning House 130) solving about 20% by weight of tetrapotassium pyro
in 21 g.p.g. synthetic hard water. Concentration of 20 phosphate in water, adding and completely dispersing
the detergent in the test is 0.50 percent equivalent to 0.25 about 0.5% by weight of carboxymethyl cellulose in said
percent solids content. Duplicate tests are run simul tetrapotassium pyrophosphate solution, adding and com
taneously with a 0.25 percent solution of a commercially pletely dissolving about 3% by weight of anhydrous sodi
available, Solid, spray-dried detergent having the follow um metasilicate in the mixture of carboxymethyl cellulose
ing approximate composition: and tetrapotassium pyrophosphate, and finally adding
Percent about 26.5% by weight of sodium lauryl alcohol sulfate
Sodium tripolyphosphate---------------------- 50.00 with agitation and continuing the agitation until a pasty
Sodium silicate------------------------------ 3.25 consistency is obtained, the temperature being maintained
Anionic Surfactant mixture-------------------- 22.85 30 inder 60 C.
Sodium carboxymethylcellulose---------------- O.20 4. A method for the preparation of a stable high-foam
Sodium sulfate------------------------------ 17.00 built paste detergent composition which consists essential
Water, perfume and other minor ingredients.---- 6.70 ly of dissolving from about 18 to about 26% by weight of
In the following table, numbers represent the increase tetrapotassium pyrophosphate in water, adding and con
in reflectance of the soiled fabrics during the single wash. 35 pletely dispersing from about 0.1 to about 3% by weight
Each number represents the average of six reflectance of carboxymethyl cellulose in the tetrapotassium pyro
readings made on three replicate fabric samples: phosphate Solution, adding and completely dissolving
Detergency Table from about 0.1 to about 1.7% by weight of sodium sili
cate calculated as SiO2, and finally adding from about 19
Water Detergent Spray
40 to about 47% by weight of sodium lauryl alcohol sulfate
Type of Fabric Hardness,
2.9.S.
of
Invention
Dried
Detergent
with agitation, the temperature not being allowed to ex
ceed 60 C.
ACH-115------------------------- O 24.3 23.7
ES-159.
ACE-115
O
2.
26.8
23.
3
19.9
References Cited in the file of this patent
ACH-30- 21 20.3 8.7 UNITED STATES PATENTS
FDS-159------------------------- 21 24, 2 5.9
2,731,420 Sylvester --------------- Jan. 17, 1956