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Патент USA US3043787

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United States Patent 0
W‘
_
3,043,778
Patented July 10, 1962
2
1
contain up to 60% coconut soap when su?‘icient free
3,043,778
SOAP BAR COMPOSITIONS
William A. Kelly, Teaneck, N.J., assignor to Lever‘
gathers Company, New York, N.Y., a corporation of
ame
No Drawing. Filed Feb. 20, 1958, Ser. No. 716,273
9 Claims. (Cl. 252-107)
fatty acid is incorporated. The preferred range of coco
nut soap content is between 15% and 40%, because bars
containing more than 40% coconut soap tend to develop
sand-like granules upon aging for about six weeks. These
granules do not interfere with the useful properties of
the bar, but they are aesthetically objectionable.
It has been discovered that in order to obtain satis
factory lathering properties it is not only necessary that
This invention relates to a novel soap bar which will
disperse a soap scum when used in hard water. More 10 the bar contain 15 to 60% of coconut soap, but also from
particularly, it relates to a soap bar comprising certain
proportions of alkali metal salt of fatty acid methyl tau
rate, free fatty acid, and coconut soap.
2 to 25% free fatty acids.
Fatty acid overcomes the
suds depressing effect of taurate on soap, even though it
replaces soap in ‘a ?nished bar formula.
Surprisingly,
the inclusion of at least 2% free fatty acids'greatly in
salts of fatty acid methyl taurate possess the property of 15 creases the lathering ability of the bar. Compositions
dispersing the precipitate formed when soap is used in
containing more than 25% free fatty acids tends to be
hard water. This fact was disclosed as early as 1933 in
soft and mushy, especially when used. ‘The free fatty
acid reduces the pH of the bar from about 10 to 10.5
US. Patent No.‘ 1,932,180. Examples 31-34, 37, 38
and 42 of this patent disclose the preparation of sodium,
to 8.6 to 9.4. It ‘has been discovered that in this range
potassium, and amine salts of fatty acid methyl taurates
the lathering, mildness and scum‘ dispersing properties
' For many years it has been known that alkali metal
and their use as wetting agents in solutions which are
not rendered turbid by the presence of insoluble calcium
' salts. Despite the fact that this property has been known
for many years, until the present invention, no one has
of the bar are improved. Free fatty acid also improves
the feel and “slip” qualities. This is especially notice
able in cool water. A soap taurate mixture tends to drag
and be rough when rotated in the hands during washing,
succeeded in making a commercially acceptable soap bar 25 whereas the taurate, soap, fatty acid mixtures are smooth
wherein this property of dispersing soap scum has been
and slip easily in the hands during use.
One of the most surprising discoveries concerning the
In order to be commercially acceptable in the present
soap, ‘taurate, free fatty acid combinations was that the
day market, a soap bar must meet many requirements.
fatty acid improves the lather without contributing to
It must give good detergency in both cold ‘and hot water. 30 scum formation in hard water.
It must have good lathering properties, but not be irritat
It is advantageous to use free fatty acids which have
ing or injurious to the skin. It must have pleasant ap- _
been hydrogenated to a very lowiodine value, preferably
pearance, odor and feel, and maintain these character
less than about 5. The use of free fatty acids of iodine
istics during and after use. In addition, it must be ca
value no greater than 5 tends to prevent rancidity upon
pable of being formulated and compacted with equip 35 long storage. The chain length of the free fatty acid
ment that would make the product commercially prac
may be from about C12 to about C20. Myristic acid
tical. Until the present invention, no one has succeeded
(C14), palmitic acid (C16) and stearic acid (C18), alone
in making a bar of soap which contains enough taurate
or in combination are preferred. The development of
to disperse hard water soap precipitate and which meets
rancidity may be substantially reduced when unsaturated
all of the above necessary requirements for commercial
acids ‘are present by incorporating butylated hydroxy
usefulness.
' toluene or butylated hydroxy anisol at .02 to 0.5%.
These and other problems are solved by the present
The remaining portions of the bar may comprise soap
invention which pertains to a bar of soap comprising from
of chain length longer than that in coconut soap, e.g. tal
5 to 25% alkali metal salt of fatty acid methyl taurate,
low soap, moisture, and ingredients such as perfume, pig
from 2 to 25% free fatty acids, and from 15 to 60% 45 ment, preservatives and germicides in minor amounts.
coconut soap. The above percentages ‘are by weight andv
Of course, small ‘amounts of various substances such as
utilized.
-
.
are based on the weight of the entire bar. The pH of
the bar as measured in 10% solutions is between 8.6~9.4.
The properties of a bar are mutually dependent func
tions of the type and amounts of the ingredients present.
A change in the composition or amount of any one in
gredient may improve one property, but generally only
at the expense of one or more of the other properties.
methyl taurine, dimethyl taurine, glycerol, salt, etc. are
present in the taurate or soap, and are carried through to
the ?nished bar.
.
.
'
3,4’,S-trihalosalicylanilide having like halogens (e.g.
3,4’,5-tribromosalicylanilide), and tetrahalosalicylanilides
having like halogens, three of which are in the 3,4',5-posi_
tions, have been found to be effective germicideswhen
incorporated in the bar ‘at levels of about 0.1% to 1.0%,
Thus, if there is serious departure from the above stated
ranges of compositions, the resulting bar will be de? 55 preferably about 0.5 %.
cient in one or more respects. Within the ranges stated,
Taurates from fatty acids of 12 to 20 carbon atoms such
it is possible to design bars for various desired character
as described in the aforementioned US. Patent No. 1,932,
istics. For example when a bar is to be used in rela
180 may be used, but it has been discovered that in order
tively soft water, i.e., up to 50 -p.p.m., a bar containing
to have maximum soap curd dispersing action, it is pref~
tallow soap with only 5% of taurate, about 20% coco 60 erable to use relatively long chain fatty acid taurates, e.g.
nut soap and 3% free fatty acid will have good lime
the C16 and C18 compounds from tallow, which have
soap dispersing properties, lather well, and ‘be mild.
considerably ‘greater dispersing action than the corre
‘When the bar is to be used in 300 p.p.m. hard water, at
sponding compounds from coconut oil. It has also been
least about 18% taurate would be required, along with
discovered
that the occurrence of sand like‘ granules is
higher coconut soap and free fatty acid contents to dis 65
perse the lime soap scum, lather well and be mild.
It is not economically feasible to go above 25% taurate
concentration, since optimum dispersion effects are ob
tained below that ?gure, and since the taurate is the most
minimized by the use of taurate made from tallow which
has not been hydrogenated below an iodine value of 10.
For optimum results the iodine value of the fatty acid
portion of the taurate should be about 40.
In order that the bars have a good texture and be
expensive ingredient.
.
70
smooth ‘to the touch during use, it is preferred that the
The soap bar should contain at least 15% coconut
bar contain as little electrolyte as possible. Generally a
soap in order to have good lathering action, and may
3,043,778
3
fatty acid methyl taurate can be made by either of two
reactions. One involves reacting a fatty acid chloride
with the sodium salt of N-methyl taurine in the presence
of caustic. The product of this reaction contains one
' Example N0. 2
This is an example of embodiments of the invention
at lower levels of taurate in ‘bars containing coconut soap
and free fatty acid Within the ranges stated in the speci?ca
tion. Bars were made containing 5, 10, 15 and 18%
mole of salt for every mole of taurate formed, and un
less this salt is removed, ‘for example by ion exchange, a
bar containing the product will be extremely rough when
used after an aging period. The preferred method of
tallow (40 I. V.) methyl taurate by mixing the taurate,
manufacture of the taurate involves reacting an excess of
fatty acid with N-methyl taurine. The product of this 10
kettle soap and stearic acid in a heavy duty jacketed Pater
son'mixer and heating until dried to about 7% moisture.
The complete compositions of the bars are as follows:
reaction contains free fatty acid and taurate but no salt,
and can be used to produce a bar having the desired prop
erties.
The soap portion of the bar will normally be sodium
soap, although minor amounts of potassium soap may be
40 I.V. Tallow methyl taurate _______ ._
Na Coco Soap _____________________ ._
Na Tallow Soap ___________________ ._
0
5
16
70
50
22
10
5O
16
l5
33
35
38
29
incorporated.
Misc. salts, pigments, H2O, etc ____ __~__
14
13
14
13
14
Free Stearic Acid (Grade used in ex
0
10
10
4
6
Percent
'
ample 1) __________________________ __
It has been stated above thatfrom 15 to 60% of the
weight of the soap bar should be coconut soap. It is to
18
These bars were tested as follows:
be understood, however, that soaps derived from other
A wash bowl was ?lled with water of the desired
_ sources, but having approximately the same composition 20
hardness and then used to quench lather ‘formed on the
as coconut soap,'are also acceptable. As is well known
inv the art, the fatty acids of coconut oil comprise about
hand by rotating the wetted bar being tested.
‘9% caprylic acid, 10% capric acid, 45% lauric acid, and
amount of lime soap scum that was formed was estimated
The
20% myristic acid. Thus about. 84% of the fatty acids
are those of relatively short (C8 to C14) chain length.
Soaps can be made from palm kernel oil, babassu oil and/
or ucuhuba fat which approximate this composition, and
by sliding a black tile, about 2" x 4", under the surface‘
of the water to obtain contrast. The following observa
tions were made:
which are equivalent to coconut soap.
A preferred embodiment of the present invention com
Water Hardness, p.p.m.
prises 33% sodium coconut, soap, 18% sodium tallow
(40 I.V.) methyl taurate, and 6% saturated ‘free fatty
acids of C14 to C18 chain length. Water comprises about
6% of the Weight of the bar, and the remaining portions
30
Percent
Taurate
‘50
Heavy scum
N0 scum____
__
are fallow soap (about 30%) and minor amounts of addi
100
180
__.___.___-_.___ ..-1. __________ _.
Heavy scum_. ______________ __
Slight ‘scum-.. Heavy scum__
N0 scum
tives such as germicide, tallow alcohol, perfume, pigment 35
and the like, along with the minor amounts of salt and
_ 150
18 ___________ __do_, ________ __do _______ __
_
Slight scum..- Heavy scum.
No scum ____ __
No scum.
Ex’ample N0. 3
cal reactions involved in the preparation of the soap bar.
This is an example showing the effect of free fatty
Soap bars of the above composition give satisfactory scum
acid on the sudsing of taurate and soap combinations.
40
dispersion even in very hard water, and also have all the
For this ‘test solutions were made so that the ingredients
miscellaneous materials present as a result of the chemi
other desirable properties of good quality soap.
Example N0. 1
would be‘in the same proportion to each other as in
the preferred embodiment of the invention as shown in
Example No. l. The basis used was 5 gms. of soap in .
the proportion of 33 parts sodium coconut soap to 29
parts of sodium tallow soap in 100 ml. of water of about
110 ppm. hardness. Thus when the lathering of taurate
This is an example of a preferred embodiment of the ‘
inventiom Kettle soap,‘ taurate, caustic and ‘free fatty
acid were charged to a cnltcher in the proper proportions
so that :when dried and mixed with perfumes, pigment
etc., and milled and plodded, a bar was produced having
and soap was tested 5 gms. of soap, and 1.46 gms. of
taurate were dissolved in 100 ml. of water, and the rela
tionship of taurate to soap would be 18 parts'of taurate
to 62 parts of soap, or the same as in ?nished bar product
the following composition‘:
.
Percent
in Example No. l.
Tallow methyl taurate from tallow fatty acids hav- '
ing an iodine value of 41 ________________ ______
18
‘ For the tests, 100 ml. of solution was placed in a 500
Na coconut oil soap _________________ __' _____ __
33
Na tallow soap ____ __' ______________________ __
29
ml. graduated cylinder and agitated by inverting the
s'toppered cylinder 10 times in succession, then waiting
Miscellaneous impurities associated with the above
7
H20
'
____________________________ __
5
10 seconds to allow any large bubbles to break, and then
inverting twice more. The volume of the foam was read
___________________ -g _______________ __
6
using the calibration on the cylinder. The following re
components
Free stearic acid (a commercial grade comprising
55% palrnitic-45% stearic)___r____, ____ _r_____
Perfume, pigments ______________ __"_ __,_V_____
3,4’,5-tribromosalicylanilide ____________ __‘___~_
sults were obtained:
6
1.5 60
.5
Sample
Volume of
Suds, ml.
Fatty alcohol (62.0% cetyl, 34.1% stearyl 3.9%
(C14 and C20)) __________ -h. ____________ __
Soap alone
1
100 65
400
Soap-i-tallow (40 I.V.) methyl ‘taurate ___________ __,_______ .-
300
Soap+tallow (40 I.V.) methyl taurate+stearic acid ‘(grade
,
used in Example #1) ___________________________________ -_
Taurate alone
375
300
iThe crutcher mix as made contained about 32-34%
water. The batch was tubular dried to 7% ‘water, chilled
These results show the foam depressing action of taurate
on soap, ‘and indicate that the use of free fatty acid in
perfumes etc. and then milled, plodded, and stamped 70 combination with the taurate and soap improves the
- and formed into ribbons on a chill 'roll, mixed with dyes,
into bars, using regular soapy?nishing equipment. In
sudsing to a point almost equal to the soap alone and
greater than the taurate alone.
300 .p.p.m. hard water, the ?nished bar lathered =Wel'l, dis
persed lime soap and vwas‘ milder than commercial toilet
soap bars.
9.0.
Example N0. 4
The pH ‘of this bar in a ‘10% solution was
.
'
75
_
This is an example showing the degrees of improve
aoaa'rvs
,
6
5
ment in lathering-obtained by using free fatty acid in
methyl taurine in the presence of caustic soda, was made
combinations with a ?xed amount of coconut soap and
tallow soap. For this test a 1% solution of a bar con
in a Paterson mixer; The composition of the bar was as
taining 19% Ernersol '132 (55% palmitic-45% stearic)
follows: 17% POMT, 12% myristic acid, 40% Na coco
soap, 5% sodium stearate, about 2% NaCl, 11% sodium
methyl taurate, 34% Na coco soap, 23% Na tallow soap,
tallow soap and about 13% water. This bar lathered well
14% Na Emersol 132 soap, and the balance water and
miscellaneous perfume, pigments etc. was prepared. Var-'
and- dispersed lime soap scum. However, on aging the
bar became rough textured when used, due to the high
ious percentages of lauric fatty acid were added to 100
ml. aliquots of the solution and these were tested for
salt content.
The fact that salt tends to induce a sandy feel was
demonstrated by making two bars of the approximately
same composition as in Example No. 1, but including 1%
NaCl in one. The bar with the salt became “sandy” after
Percent fatty acid:
Height of foam, ml.
aging about 6 weeks, whereas the bar with no salt re
0 ___________________________________ __ 315
mained
smooth.
2 ___________________________________ __ 340
Example N0. 8
15
6 ___________________________________ __ 385
A bar containing 18% unhardened 51 LV. tallow
8 ___________________________________ __ 380
methyl taurate, 10% free stearic acid (as in Example No.
lathering using the cylinder test described in Example
No. 3. The results were as follows:
4
__
___
_____ __
360
10
___________________________________ __ 375
1), 33% Na coco soap, 26% Na tallow soap and the
15
___________________________________ __ 360
25
___________________________________ ___.
balance miscellaneous materials, pigments, dyes, per
20
fume, water, etc. was made by mixing in a Paterson mixer
and milling and plodding. This bar lathered well, dis
380
Example N0. 5
This is an example to show the effect of free fatty acid
on lime soap dispersion. Two bars were made by the
processes described ‘both containing 18% stearic taurate
and 50% sodium coconut soap. The ?rst bar contained
persed lime soap and had a smooth texture when used.
Example N0. 9
A bar containing 21.0% tallow methyl taurate, 2.5%
20% free stearic acid (grade used in Example No. 1)
Na coco soap, 37.0% K-coco soap, 7.5% Na tallow soap,
and the balance sodium soap with small amounts of per
fume and dyes. The second 'bar was the same except
Attasorb (a diatomaceous earth) and 8.0% Water was
the fatty acid ‘was replaced by sodium tallow soap. These
bars were tested for the amount of lime soap scum by a
titration method published in J .A.O.C.S., vol. 33, No. 3,
pages ll3~1l6. The 'bar containing the free acid pro
4.0% stearic acid (grade used in Example No. l), 20%
made by blending the ingredients in a small heavy duty
mixer (Readco) and then milling and plodding. The
?nished bar was smooth, lathered well and dispersed
lime soap scum.
Example N0. 10
duced only 1.3% scum in 300 ppm. hard water while
the bar containing no free fatty acid produced 4.7%
A bar containing 18% tallow methyl taurate (40 I.V.),
scum.
15% Na coco soap, 6% stearic acid (grade used in Ex- .
The bar with the free fatty acid pH 8.8, was mild
whereas the bar with no free fatty acid, pH 9.8, Was
quite harsh. The bar with the fatty acid was also much
superior in lather. Thus the free fatty acid not only im
proves the mildness and lathering of the bar, but also re
duces the amount of scum produced. Both these bars
made ‘with the saturated taurate and high coconut soap
content had a somewhat sandy feel when used.
ample No. 1), 46% Na tallow soap and the balance mis
cellaneous salts, pigments, perfume, and water was made
by mixing the ingredients in a Paterson mixer and then
milling and plodding. The bar lathered well, and dis
‘ Example No. 6
_This is an example showing'the dispersing effect of
persed lime soap scum.
What is claimed is:
1., A bar of soap which disperses soap scum in hard
water and consists essentially of, by weight based on the
weight of the entire "bar, (a) from 5 to 25% of an alkali
metal salt of a fatty acid methyl taurate, said fatty acid
containing from 12 to 20 carbon atoms and the cationic
portion of said alkali metal salt being selected from the
group consisting of sodium and potassium; (b) from 15
tallow methyl taurate on a ?xed weight of soap and
fatty acid. Solutions were made so that 10 ml. contained
0.0035 gm. of Na coco soap, 0.0025 gm. of tallow soap 50 to 60% of a water soluble alkali metal coconut soap, and
and 0.0010 gm. of stearic acid. Tallow methyl taurate
(c) from 2 to 25% of free fatty acid containing from
was added to each solution so that a speci?c percentage
of taurate based on the weight of the soap and fatty acid
was obtained. The concentration of the combination was
in a 10% aqueous solution of about 8.6 to 9.4.
equal to 0.1%. These percentages were 0, 2, 5, 10, 14
portion of the tau-rate contains 16 to 18 carbon atoms.
and 18. These were tested in 300 p.p.m. water for dis
persing ability by the titration method used in Example
No. 5. The following results were obtained.
Percent of bar as
nondispersed scum
Percent taurate:
0 ____________________________________ __ 20.8
2
5
________ __
16.3
_____ __
7.2
__
4.8
_
3.2
_
8.7
10
14 __
18
___
/
_
This test shows that the ?rst ?ve percent of taurate is
the most effective per unit in dispersing lime soap scum,
and that at least 5% taurate should be included in a
bar to get maximum dispersing per unit of taurate.
Example N0. 7
12 to 20 carbon atoms, said bar having a pH as measured
2. The bar of soap of claim 1 wherein the fatty acid
3. The bar of soap of claim 1 wherein the‘ fatty acid
portion of the taurate has an iodine value greater than
10.
4. The bar of soap of claim 1 wherein the free fatty
acid has an iodine value no greater than 5.
5. The bar of soap of claim 1 which also contains from
0.1 to 1.0% of 3,4’,5-tribromosalicylanilide.
6. The bar of soap of claim 1 wherein the alkali metal
salt of a fatty acid methyl taurate is substantially free
65 of sodium chloride.
7
7. A bar of soap which disperses soap scum in hard
water and consists essentially of, by weight based on the
weight of the entire bar, (a) from 5 to 25% of the
' sodium salt of unhydrogenated tallow fatty acid methyl
taurate; (b) from 15 to 40% of a water soluble alkali
metal coconut soap, and ('c) from 2‘ to 25% of ‘free fatty
acid containing from 14 to 18 carbon atoms and having
aniodine value no greater than 5, said bar having a pH
A bar containing 17% palmitic-oleic methyl taurate
‘as measured in a 10% aqueous solution of about 8.6 to
(POMT), made by reacting fatty acid chloride with N 75 9.4.
3,043,778
7
References Cited in the ?le of this patent
8. A'bar of soap which disperses soap scum in hard
water and consists essentially of, by weight based on the I
weight of the entire bar, (a) about 18% of sodium fatty
‘acid methyl taurate, said fatty acid containing 16 to 18
carbon atoms and having an iodine value of about 40‘; (b)
about 33% of sodiumtcoconut soap; (0) about 6% of
free fatty acid containing from '14 to 18 carbon atoms and
having an iodine value no greater than 5 and (d) about
29% of sodium tallow soap, said bar having a pH as
measured in a 10% aqueous solution of about 8.6 to 9.4. 10
9. The bar of soap of claim 8 which also contains about
0.5% of 3,4’,S-tribromosalicylanilide.
UNITED STATES ' PATENTS
,
1,906,484
Neusslein ____________ ..- May 2, 1933
2,462,758
Malkemus __-_. ________ __ Feb. 22, 1949
Jelinek et a1." _________ __ Feb. 12, 1957
2,781,320
2,802,029
Schuler ______________ __ Aug. 6, 1957
2,868,731
2,894,812
Henderson et a1 ________ _._ Jan. 13, .1959
Geitz _______________ __ July 14, 1959
1,059,351
France ______________ __ Nov. 10, 1953
FOREIGN PATENTS
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