Note: Descriptions are shown in the official language in which they were submitted.
WO 92/1661)9 2 1 ~ 5 0 ~ O PCI-/US92/01~689
LOW P~ MILD PERSONAL CLEANSIN~ BAR
TECHNI~AL FIELD
This invention relates to mild personal cleansing bars and to
processes of making them.
BACKGROUND OF THE INVENTION
Personal cleansing with mild surface-active cleansing bar
preparations has become a focus of great interest. The processa-
bility of such bars has also become a focus of great interest.
The smear properties of such bars have become a focus of even
greater interest.
Some of the problems associated with mild bars comprised of
synthetic detergents are bar processability, firmness, smear and
mildness. The problems of formulating such bars are not limited
to the performance characteristics of the finished bars. Most
bars which are made with certain mild surfactants are very dif-
ficult to fabricate.
In contrast, the fabrication of relatively pure "soap" bars
is .a well-worked-out &ngineering procedure involving milling,
plodding and molding. Coco/tallow soap becomes quite plastic when
warmed and can be easily plodded and molded under relatively low
pressures.
Most synthetic detergents and detergent-filler combinations
do not become plastic and the machinery for fabrication must be
specially designed. See U.S. Pat. No. 2,678,921, J.A.V. Turck.
Jr., issued May 18, 1954.
Ideal processing should be fast and problem free in terms of
milling, plodding and molding toilet bar formation. Most mild bar
processings fall short in this respect.
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The development of soap-synthetic bars dates back to World
War II. U.S. Pat. No. 2,432,169, Hoyt, describes a bar having
soap and alkyl benzene sulfonate as the active and a substantial
proportion of corn starch as a binder; and U.S. Pat. 2,988,511,
Mills and Korpi, issued June 13, 1961, describes a nonsmearing bar
comprising alkyl glyceryl ether sulfonate, sodium and magnesium
soaps and binder. U.S. Pat. No. 2,982,735, Blinka and Grounds,
Jr, issued May 2, 1961, discloses a detergent milled bar com-
prising soap, anionic detergent and starch.
U.S. Pat. No. 2,7B1,321, Mayhew et al., issued Feb. 12, 1957,
discloses (Example 19) a 50% Mg stearate all purpose detergent bar
with 20% gum, etc. The surfactant system includes dodecylbenzene
sulfonate in Examples 26-30, which is a relatively harsh sur-
factant. STPP is used at levels of 10-15% in Mayhew et al.'s
examples.
; U.S. Pat. No. 3,070,547, Chaffee, issued Dec. 25, 1962, also
discloses a potassium synthetic soap-synthetic bar containing
magnesium soap. There appears to be no free fatty acid in the
Chaffee exemplified bars, and the pH's of his surfactant systems
used in those examples are not disclosed, but are normally rela-
tively high,
U.S. Pat. No. 2,987,484, Lundberg and Blinka, issued June 6,
;1961, discloses a closed die injection molded detergent bar
comprising alkyl glyceryl ether sulfonate and acyl isethionate.
Some other uses and procedures for making alkyl glyceryl ether
sulfonate are disclosed in U.S. Pat. Nos.: 2,094,489, Hulter.
issued Sept. 28, 1937; 2,427,576, Smith, issued Sept. 16, 1947:
2,427,577, Smith, issued Sept. 16, 1947; 2,989,547, Whyte, issued
June 20, 1961; 2,999tO68, Pilcher et al., issued Sept. 5, 1961:
and 3,024,273, Whyte et al., issued Mar. 6, 1962, all of said
patents incorporated herein by reference.
It is noted that surfactant mildness can be measured by a
skin barrier destruction test which is used to assess the irri-
tancy potential of surfactants. In this test the milder the
surfactant, the less the skin barrier is destroyed. Skin barrier
destruction is measured by the relative amount of radio-labele~
water (3H-H20~ which passes from the test solution through the
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W O 92/16609 210 5 0 9 PCTtUS92/00689
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skin epidermis into the physiological buffer contained in the
diffusate chamber. This test is described by T. J. Franz in the
J. Invest Derma ol., 1975, 64, pp. 190-195; in U.S. Pat. No.
4~673~525, Small et al., issued June 16, 1987, and in copending
U.S. Pat. Application Ser. No. 294~832, Small et al., filed
Jan. 9, 1989, incorporated herein by reference.
U.S. Pat. No. 2,894,912, Geitz, issued July 14~ 195g, for
"Isethionate Detergent Bar," discloses a detergent bar consisting
essentially of from 30-70% of water-soluble alkali metal detergent
salts of esters of isethionic acid with mixed aliphatic fatty
acids having from 6 to 18 carbon atoms and an iodine value of less
than 20~ of which mixed acids at least 75% have from 12 to 18
carbon atoms and up to 2S% have from 6 to 10 carbon atoms, from
2-10% of at least one water-soluble suds-boosting detergent salt
selected from the group consisting of alkali metal and organic
amine higher aliphatic fatty alcohol sulfates, alkyl aryl sul-
fonates, and higher aliphatic fatty acid taurides, from about 1%
to about 9% water, from about 2.5~o to about 25% of water-soluble
higher fatty acid soap, and from 10-40% of at least one higher
fatty acid having from about 12 to about 25 carbon atoms as a
binder and plasticizer, said bar having a pH within the range from
6 to 8, measured as a 10% aqueous solution of the bar composition
at 35C. No magnesium soap is used.
U.S. Pat. No. 4,180,470t Tokosh et al., issued Dec. 25~ 1979.
discloses a method for making improved 30-70% acyl isethionate
detergent bars with from 2-6% of sodium alkoxy hydroxy propane
sulfonate (a synonym for alkyl glyceryl ether sulfonate) with
alkyl chains of from 8 to 22 carbon atoms in conjunction with a
small amount of sodium chloride. C1g alkyl glyceryl ether sul-
fonate at 5% is used in an example. The added alkyl glyceryl
ether sulfonate and salt are used to improve bar wear rate without
adversely affecting its lathering characteristics.
U.S. Pat. No. 4~234,464~ Morshauser, issued Nov. 18, 1980.
for "Detergent Bar Composition and Binder Therefor," discloses a
detergent bar in Example 6 which comprises: 45% sodium cocoyl
isethionate, 5% alkyl amide, 37.5% stearic acid, 5.0% hydrogenated
tallow glycerides, and 1% Polymer JR. Morshauser teaches that his
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WO 92/16609 PCI/US92/00~89
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detergent bars can contain up to 5% soap "without substantial
detriment."
U.S. Pat. No. 4,012,341, Orshitzer et al., issued Mar. 15,
1977, for a "Unique All Synthetic Detergent Shampoo Bar," dis-
closes a bar comprising a mixture of anionic and nonionic deter-
gents. The Examples are primarily based on sodium lauryl sulfate.
which is an unacceptably harsh primary surfactant for the present
invention.
U.S. Pat. No. 3,761,418, Parran, Jr., issued Sept. 25, 1973,
for "Detergent Compositions Containing Particle Deposition Enhanc-
ing Agents," discloses detergent compositions including a bar,
whose main surfactant is alkyl sulfate, which is unacceptable for
the mild skin cleanser of the present invention.
Major drawbacks of most synthetic surfactant toilet bar
formulations are harshness, poor lather, poor smear, and poor
processability due to stickiness. The use of high sudsing anionic
; surfactants can yield acceptable lather volume. Unfortunately,
the highest sudsing anionic surfactants are, in fact, poor in
processability. While some prior art mild blends of sodium coco-
nut/tallow alkyl glyceryl ether sulfonate (AGS) are relatively
good in lather potential, they are not so easy to process because
of their stickiness or hygroscopicity. It will be appreciated
that processability, firmness, smear, mildness, lather, and
rinsability make surfactant selection for mild personal cleansing
bars a delicate balancing act. Thus, it will be appreciated that
rather stringent requirements for formulating mild personal
cleansing bars limit the choice of surfactants, and final formu-
lations represent some degree of compromise. Mildness is often
obtained at the expense of processability, effective cleansing,
lathering, or rinsing, or vice versa. Processability is often
obtained at the expense of smear.
Needless to say, a superior processable mild personal
cleansing bar formulation with good mildness, good smear. good
lather potential and good rinsability is difficult to formulate.
OBJECTS OF THE INVENTION
An object of the present invention is to provide a stamped.
mild personal cleansing bar which has improved processability.
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WO 92/16609 2 1 ~ 5 ~) 9 0 PCI/US92/00689
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;~ Another object of the present invention is to provide a mild
bar with excellent smear.
Yet another object is to formulate a mild personal cleansing
bar with a relatively low level of free fatty acids to improve bar
smear and bar firmness.
Other objects will become apparent from the detailed de-
scription below.
SUMMARY_OF_THE INVENTION
This invention is a mild personal cleansing bar comprising:
from about ZO% to about 50% lathering mild synthetic surfactant
and from about 5% to about 50% of magnesium soap; wherein the
ratio of said lathering mild synthetic surfactant to said soap is
from about 10:1 to about 0.4:1i said bar having a pH of from about
6.5 to about 8.5 in a 1% aqueous solution at 25~C.
DETAIL~D DESCRIPTION OF THE INVENTION
The invention relates to a mild personal cleansing bar made
from a mix of from about 20% to about 50% of a lathering mild
synthetic detergent surfactant and from about 5% to about 50%,
preferably from about 10% to about 45%, magnesium soap. The mild
personal cleansing bar has a pH of from about 6.5 to about 8.5.
The pH of the bar is preferably from 7 to 8, and is preferably
adjusted with a carboxylic acid. The pH is measured as a 1%
aqueous solution at about 25'C.
The ratio of lathering mild synthetic surfactant to the
magnesium soap is from about 10:1 to about 0.4:1, preferably from
about 5:1 to about 0.5:1, more preferably from about 4:1 to about
0.6:1.
The term "lathering mild synthetic surfactant" as used herein
means any surfactant which lathers at least about as well as the
"mild standard alkyl glyceryl ether sulfonate (AGS)," as defined
herein, which contains a substantial amount of C12 and C14 alkyl
chains, specifically about 68% C12; 25% C14; and 7% C1ç AGS.
A "non-lathering, non-soil-load-diluent, surfactant" is
defined as a surfactant which has a "low" lather on the order of a
C16-C1g alkyl glyceryl ether sulfonate, and other C16-C1g syn-
thetic surfactants, e.g., C16-C1g alkyl sulfates, etc. These
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w O 9~/16609 2 1 0 5 0 ~ O PCT/VS92/00689
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surfactants do not contribute to the lather in any app~ ciable
way, but they also do not detract from the lather in any
significant way. They are, however, especially effective in
improving the ability of the bar to have a good grade in the Flex
Test as described more fully hereinafter. They also are useful in
improving the smear characteristics of the bars.
The terms "soil load diluent" and "hydrophobic material" as
used herein are synonymous and mean any diluent which is a soil
load on the order of free fatty acid, paraffin wax, fatty alcohol~
or triglyceride. Some of these materials, like paraffin wax, are
very effective in improving the Flex Test grades. Other
materials, like free fatty acid, help plasticize the formula for
processability.
The magnesium (Mg~ soap can be made by usina selected fatty
matter (free fatty acids and soaps) having an Iodine Value of from
zero to about 50, preferably below 15, and more preferably from
about zero to about 3. The titer (in C) can be as low as about
15, however, the preferred fatty matter of the soap and free fatty
acid have a titer of from about 60 to 80, preferably from about 35
to 75, and more preferably from about 50 to about 70.
The chemical properties of some preferred pure saturated
acids are set out below in the Pure Acid Table.
Pure Acid Table
Chain Acid Molecular Titer
Acid Lenqth Value Weiqht _ C
Decanoic C-10 326 172
Lauric C-12 280 200 44.2
Myristic C-14 246 228 54.4
Pentadecanoic C-15 231 242
Palmitic C-16 219 256 62.9
Margaric C-17 207 270
Stearic C-18 197 284 69.6
NonadecanoicC-19 188 298
Arachidic C-20 180 312
Behenic C-22 165 340
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.; Palm Kernel Acid Ta~le (T~Dicall
Acid Chain Lenqth Wt.%
Saturated:
Octanoic C-8 3
Decanoic C-10 3
Lauric C-12 50
. Myristic C-14 18
Palmitic C-16 8
Stearic C-18 2
Unsaturated:
Oleic C-18 = 1 14
Linoleic C-18 ~ 2 2
lodine Value: Low 14
High 23
lS Saponification Value: Low 245
High 255
Titer, C (Fatty Acid): Low 20
High 28
Palm Kernel Acid, Coconut Acid and Tallow Acid Tables show some
chemical properties of those acids.
Coconut Acid Table (TyDical)
Acid Chain Lenqth Wt.%
Saturated:
Octanoic C-8 7
Decanoic C-10 6
Lauric C-12 SO
Myristic C-14 18
Palmitic . C-16 a.5
Stearic C-18 3
Unsaturated:
Oleic C-18 = 1 6
Linoleic C-18 = 2 1 ;
:, Linolenic C-18 = 3 0.5
Iodine Value: Low 7.5
: 35 High 10.5
Saponification Value: Low 250
High 264
Titer, C (Fatty Acid): Low 20
High 24
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Tallow BFT Table fTypical)
Acid Chain lenqthWt.%
Saturated:
Myristic C-l~ 3
Pentadecanoic C-15 0.5
Palmitic C-16 24
Margaric C-17 1.5
Stearic C-18 20
Unsaturated:
Myristoleic C-14 - 1 1
Palmitoleic C-16 = 1 2.5
Oleic C-18 = l 43
Linoleic C-18 = 2 4
Linolenic C-18 = 3 0.5
Iodine Value: Low 45
High 50
Saponification Value: Low 192
: High 20Z
Titer, C (Fatty Acid): Low 40
High 45
The free fatty acid (and other soil load diluents) in the
mild personal cleansing bar of the present invention can be
surprisingly low. The Mg soap to FFA ratio can be from about 50:1
to about 0.5:1, preferably from about 30:1 to about l:l, and more
preferably from about 15:1 to about 2:1. The level of FFA is
preferably from about 1% to about 10%, preferably from about 2% to
about 9%, more preferably from about 3% to about 8%, of the bar.
The hydrophobic material (soil load diluents) can be present
in the bars of this invention at a level of from zero up to about
40%, but is preferably used at a level of from about 5% to about
20%. The other hydrophobic material including free fatty acids
containing from about 8 to about 18 carbon atoms; mono-, di-, and
triglycerides; fatty alcohols containing from about 8 to about ~8
carbon atoms; and mixtures thereof; wherein said composition
contains about 25% maximum of said waxes and about 15% maximum of
said other hydrophobic material. Triglycerides (Cg-Clg acyl
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chain) can be used up to about 10% without adversely affecting
acceptable lather performance.
The preferred hydrophobic material is a wax having a melting
point tM.P.) of from about 120'F to about 185F (49'-85C),
preferably from about 125'F to about 175'F (52--79'C). A pre-
ferred paraffin wax is a fully refined petroleum wax having a
melting point ranging from about 130'F to about 140-F (49-607C).
This wax is odorless and tasteless and meets FDA requirements for
use as coatings for food and food packages. Such paraffins are
readily available commercially. A very suitable paraffin can be
obtained, for example, from The Standard Oil Company of Ohio under
the trade name Factowax R-133.
Other suitable waxes are sold by the National Wax Co. under
the trade names of 9182 and 6971, respectively having melting
points of 131F and 130-F (-55-C).
The paraffin preferably is present in the bar in an amount
ranging from about 5% to about 20% by weight. The paraffin
ingredient is used in the product to impart skin mildness, plas-
ticity, firmness, and processability. It also provides a glossy
look and smooth feel to the bar.
The paraffin ingredient is optionally supplemented by a
microcrystalline wax. A suitable microcrystalline wax has a
melting point ranging, for example, from about 140F (60~C) to
about 185'F (85-C), preferably from about 145'F (62-C) to about
175F (79C). The wax preferably should meet the FDA requirements
for food grade microcrystalline waxes. A very suitable micro-
crystalline wax is obtained from Witco Chemical Company under the
trade name Multiwax X-145A. The microcrystalline wax preferably
is present in the bar in an amount ranging from about 0.5X to
about 5% by weight. The microcrystalline wax ingredient imparts
pliability to the bar at room temperatures.
The non-soil-load, surfactant diluent can be used at a level
of from 0% to about 40%, preferably from about 5% to about 407
and more preferably from about 10% to about 35%. The latter level
range is highly preferred for Flex Test mildness.
The water level is from about 2~o to about 15%, prefera31
from about 4% to about 10~/0.
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The total non-surfactant electrolyte (organic and inorganic)
level is from about 1% to about 10%, preferably from about 2% to
about 8%, more preferably from about 2% to about 5%, by weight of
the bar.
Numerous examples of surfactants are disclosed in the patents
incorporated herein by reference. They include alkyl sulfates7
anionic acyl sarcosinates, methyl acyl taurates, N-acyl gluta-
mates, alkyl sulfosuccinates, alkyl phosphate esters, ethoxylated
alkyl phosphate esters, trideceth sulfates, protein condensates,
mixtures of ethoxylated alkyl sulfates and alkyl amine oxides,
betaines, sultaines, and mixtures thereof. Included in the sur-
factants are the alkyl ether sulfates with 1 to 12 ethoxy groups,
especially ammonium and sodium lauryl ether sulfates.
Alkyl chains for these surfactants are Cg-C22, preferably
C12-C14 for lathering mild surfactants, and C16-C1g for non-
lathering non-soil-load diluents.
The term "alkyl glyceryl ether sulfonate" as used herein
means, in general, a mixture of alkyl glyceryl ether sulfonate
(AGS) surfactants having alkyl chains of from 8-22 carbon atoms,
preferably from 10-20 carbon atoms, and more preferably from 12-14
carbon atoms.
Alkyl glyceryl ether sulfonates are derived from corres-
ponding ethers consisting of straight alkyl chains which are in
turn derived from their corresponding synthetic or natural
alcohols.
Commonly assigned U.S. Pat. No. 4,673,525, Small et al
suDra, discloses a mild alkyl glyceryl ether sulfonate surfactant
based mild personal cleansing bar comprising alkyl glyceryl ether
sulfonate. The mild personal cleansing bars of this invention
; 30 exhibit improved processability over the exemplified mild personal
cleansing bars disclosed in Small et al. In other words, the
improved bars of this invention also exhibit a processability
improvement over comparable AGS soap bars. The bars of this
invention are also better in terms of bar firmness and smears.
Alkyl glycosides and methyl glucose esters are preferred mild
nonionics which may be mixed with at least one of said mild
anionic or amphoteric surfactants in the compositions of this
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WO 92/16609 21~ ~i O 9 (~ PC~/US92/00689
invention.
A preferred ingredient i5 acyl isethionate. Acyl isethi-
onates are a1iphatic higher fatty acid esters of an alkali metal
isethionic acid salt and can be defined by the following general
formula: RCOOCH2CH2S03M wherein R is an aliphatic radical or mixed
aliphatic radical of a higher fatty acid or mixture thereof,
having from about 6 to about 20 carbon atoms, preferably from
about 8 to about 18 carbon atoms, e.g., cocoyl or an approximately
equivalent distribution of chain lengths, the longer chains (I6
I0 and 18) being more preferred as non-lathering, non-soil-load
diluents and medium chain (C12-CI4) being more preferred as
lathering synthetic surfactants; and wherein M is an alkali metal
cation such as sodium, potassium, or ammonium, or an organic amine
base such as triethanolamine, triisopropanolamine, diethanolamine
and ethanolamine. The preferred cation in the AGS and the acyl
isethionate salts is sodium.
A preferred milled bar for Flex Test mildness comprises: (1)
from about 5% to about 25%, preferably from about 10% to about
20%, of C16-C18 alkyl (chain) sulfates and (2) from about 5% to
about 50%, preferably from about 10% to about 30% magnesium soap
by weight of the soap bar. E.g., Example 7 disclosed hereinbelow.
Lathering mild synthetic surfactants are also required in this
preferred bar. The ratio of the alkyl sulfates to magnesium soap
can be from about 3:1 to about l:fi, preferably from about 1:2 to
about 1:4. This non-soil-load, non-lathering, synthetic sur-
factant diluent is a surprisingly and unexpectedly excellent or
superior diluent for lathering ultra mild synthetic surfactants,
e.g., alkyl glyceryl ether sulfonate and/or cocoyl isethionate in
personal cleansing bar compositions. The synthetic surfactant
diluents prc ~e a surprisingly acceptable improvement in bar
processabilitJ, while not significantly impairing bar mildness or
the desirable physical characteristics of the bars.
The C16-Clg alkyl sulfates are derived from corresponding
saturated straight chain alcohols. The C16-Clg alkyl sulfates, as
defined herein, comprise said C16-Clg alkyl chains at a level of
at least about 90%, preferably about 93%, and more preferably
about 97%. In general, the ratio of C16 to Clg can range from
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WO 92/16~09 '~ 1 0 ~i 0 9 0 PCI/US92/00689
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about 4:1 to about 1:4 by weight. A commercially available
C16-C1g alkyl sulfate is SIPON~ EC-111 (formerly SIPEX0 EC-111),
sodium cetearyl sulfate, which is approximately 60% C16 and 36%
C1g. SIPON~ EC-111 is sold by Alcolac Company, Baltimore, MD
21226. Another source is Henkel Corp., Ambler, PA 19002.
Henkel's sodium cetearyl sulfate, lANETTE E, is an estimated
50-50X C16-C1g alkyl sulfate sold as an emulsifier.
The percentages, ratios, and parts herein are on a total
composition or surfactant weight basis, unless otherwise speci-
fied. All formulae, levels and ranges herein are approximations
unless otherwise specified. Some preferred percentages and ratios
are described below.
The lathering synthetic surfactant comprises from 20% to 50%
by weight of the bars of this invention. A preferred bar com-
prises: about 25% to 45% lathering mild synthetic surfactant;
about 15% to 20% of non-soil-load synthetic surfactant diluent,
e.g., cetearyl sulfate; about 10% to 50X magnesium soap; and about
170 to 10%, preferably 2% to 9%, free fatty acid; about 0% to 8%,
preferably 0.2% to 2%, polymeric skin feel aid; and 2% to 15%,
preferably 4% to 10YO, water.
The bars of the present invention comprise a soil load
diluent (FFA, wax, etc.) to lathering mild synthetic surfactant
ratio of from 0.1:1 to 1:1, preferably from 0.2:1 to 0.9:1.
The bars of the present invention comprise a soil load
diluent to a non-soil-load diluent (including Mg soap) ratio of
from 0.1:1 to 1:1, preferably from 0.2:1 to 0.9:1, and without Mg
soap the ratio is 0.4:1 to 30:1.
The bars of the present invention comprise a lathering
synthetic surfactant to a non-soil-load diluent (with Mg soap)
ratio of from 0.2:1 to 3:1, preferably from 0.3:1 to 2:1, and
without Mg soap the ratio is 0.5:1 to 35:1.
The bars of the present invention comprise a magnesium soap
to lathering synthetic surfactant ratio of from 1:10 to 1:0.4.
preferably from 1:5 to 1:0.5, more preferably from 1:4 to 1:0.6.
The bars of the present invention comprise a magnesium soap
to total synthetic surfactant(s) (lathering + diluent) ratio of
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wo 92/16609 210 ~ o 9 o Pcr/US92t00689
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from 0.1:1 to 3:1, preferably ~rom 0.2:1 to 2:1, and more prefer-
ably from 0.3:1 to 1.5:1.
The bars of the present invention comprise a magnesium soap
to free fatty acid ratio of from 50:1 to 0.5:1, preferably from
30:1 to 1:1, more preferably from 15:1 to 2:1.
The bars of the present invention comprise a magnesium soap
to a soil load diluent (FFA, wax, etc.) ratio o~ from 0.3:1 to
5:1, preferably from 0.4:1 to 4:1.
For improved smears, it should be noted that when the mag-
nesium soap level is low, e.g., 10/O or less, and when the level of
the total synthetic surfactant(s) to magnesium soap is more than
5:1, the water level of the bar should be from about 2% to about
7%, preferably from about 2.5% to about 6% for improved smear.
More than one lathering synthetic surfactant can be used.
E.g., from about 2% to about 25%, preferably from about 3% to
about 20%, more preferably from about 4% to about 16%, of very
high lather enhancing surfactant, e.g., sodium lauroyl sarcosinate
can be used with AGS, as shown in the Examples herein.
Other bar ingredients are selected from: non-lathering
diluent surfactants, magnesium soap, soil load diluents, polymeric
skin feel aids, moisturizers, fillers, etc.
The mild personal cleansing bars can also have about 0-8%,
; preferably about 0.2-2%, polymeric skin feel aid if present.
A preferred bar of this invention can comprise about 0.1% to
5%, more preferably 0.2% to 2%, of a suitably fast hydrating
cationic polymer. The polymers have molecular weights of from
about 1000 to about 3,000,000. A preferred one is selected from
cationic guar gums having a molecular weight range of 2,500-
350,000. ?
The cationic polymer (skin conditioning agent) is selected
from the group consisting of:
(I) cationic polysaccharides;
(II) cationic copolymers of saccharides and synthetic
cationic monomers, and
35 (III) synthetic polymers selected from the group consisting
of:
(A) cationic polyalkylene imines
WO 9t/166~9 2 1 0 ~ 0 9 0 PCI/US~2/00689
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(B1 cationic ethoxy polyalkylene imines, and
(C) cationic poly[N-[-3-(dimethylam~onio)propyl]-N'-[3-
(ethyleneoxyethylene dimethylammonio)propyl]urea
dichloride].
Specific examples of members of the cationic polysaccharide
class include the cationic hydroxyethyl cellulose JR 400 made by
Union Carbide Corporation; the cationic starches Stalok~ 100, 200,
300 and 400 made by Staley, Inc.; the cationic galactomannans
based on guar gum of the Galactasol 800 series by Henkel, Inc. and
the Jaguar Series by Celanese Corporation.
Examples of members of the class of copolymers of saccharides
and synthetic cationic monomers include those composed of cel-
lulose derivatives (e.g., hydroxyethyl cellulose) and N,N-di-
allyl,N-N-dialkyl ammonium chloride available from National Starch
Corporation under the trade name Celquat.
The cationic synthetic polymers useful in the present in-
vention are cationic polyalkylene imines, ethoxypolyalklene
imines, and poly[N-[-3-(dimethylammonio~propyl]-N'-[3-(ethylene-
oxyethylene dimethylammonio)propyl]urea dichloride] the latter of
which is available from Miranol Chemical Company, Inc. under the
trademark of Miranol A-15, CAS Reg. No. 68555-3~-2.
Preferred cationic polymeric skin conditioning agents of the
present invention are those cationic polysaccharides of the
cationic guar gum class with molecular weights of 1,000 to
3,00~,000. More preferred molecular weights are from 2,500 to
350,000. These polymers have a polysaccharide backbone comprised
of galactomannan units and a degree of cationic substitution
ranging from about 0.04 per anhydroglucose unit to about 0.80 per
anhydroglucose unit with the substituent cationic group being the
adduct of 2,3-epoxypropyltrimethyl ammonium chloride to the
na~ural polysaccharide backbone. Examples are JAGUAR C-14-S, C-15
and C-17 sold by Celanese Corporation. In order to achieve the
; benefits described in this invention, the polymer must have
characteristics, either structural or physical which allow it ~o
be suitably and fully hydrated and subsequently well incorporate~
into the soap matrix.
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WO 92/16609 2 1 ~ ~ ~ 3 0 PCr/US9~/00689
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Other ingredients of the-present invention are selected for
the various applications. E.g., perfumes can be used in formu-
lating the skin cleansing products, generally at a level of from
about 0.1% to about 1.5% of the composition. Alcohols, hydro-
tropes, colorants, and fillers such as talc and clay, can also beused. Preservatives, e.g., sodium ethylenediaminetetraacetate
(EDTA), generally at a level of less than 1% of the composition,
can be incorporated in the cleansing products to prevent micro-
biological growth. Antibacterials can also be incorporated,
usually at levels up to 1.5%.
A preferred bar of the present invention can contain from
about 0.5% to about 4%, preferably from about 2% to about 3.5%,
trisodium phosphate.
The following patents disclose or refer to such ingredients
and formulations which can be used in the mild personal cleansing
bars of this invention, and are incorporated herein by reference:
Pat. No.Issue Date Inventor(s~
4,234,454 11/1980 Morshauser
4,061,602 12/1977 Oberstar et al.
4,472,297 9/1984 Bolich et al.
4,491,539 1/1985 Hoskins et a1.
4,540,507 9/1985 Grollier
4,673,525 6/1987 Small et al.
4,704,224 11/1987 Saud
4,812,253 3/1989 Small et al.
4,820,447 4/1989 Medcalf et al.
The magnesium soaps can be added as is, or made in situ~
e.g., via adding a base, e.g., Mg(OH)2, to convert free fatty
acids in the composition mix.
In another preferred (suitable) method of preparing bars of
the present invention, the synthetic detergent, neutralized with a
solution of an alkali metal hydroxide or carbonate, to which the
salting-out electrolyte has been added (if insufficient electro-
lyte will be formed in situ during the neutralization step and inother steps of the process), is introduced into a suitable mixer.
such as a soap crutcher. Some water can then be added to improve
, .- . .... . . . . ..... .
W O 92/16hO9 2 1 0 5 0 9 PCT/US92tOO689
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fluidity, and a sodium soap, preferably as soap containing about
30YO water, is added. These ingredients are mixed and then an
appropriate amount of water-soluble alkaline earth metal salt,
such as magnesium sulfate or chloride, or calcium chloride, is
added to convert a portion of the water-soluble soap to water-
insoluble soap, sodium salting-out electrolyte being formed as
by-product. In a preferred method, the magnesium soap is made
before the synthetic surfactant is added to the mix. Mixing is
then continued to insure the equilibrium in the formation of the
magnesium soap is attained. Desirable adjustments in water-
soluble soap content may, of course, be made after the magnesium
soap has been formed.
Two Preferred Processes for Makinq a
Preferred Mild Personal Cleanslng Bar
I. Crutchinq - Neutralization
1. Add predetermined quantity of AGS paste at 65'C (150'F)
to the crutcher.
2. Outside the crutcher, add the predetermined quantity of
NaCl and Na2SO4 to enough hot water at 75-C (167-F) to
get the final crutcher moisture up to 50%, accounting
for all other raw material moisture content. After
dissolution of the electrolytes in the hot water, add
the mixture to the crutcher.
3. Turn the agitator and recirculation pump (optional) on
and maintain a crutcher temperature of 75-85-C
(167-185'F) by adjusting steam and water valves.
4. Add predetermined amount of TiO2 powder to the crutcher.
5. Add predetermined amount of Mg(OH)2 powder at ambient
temperature to the crutcher. A slurry of this material
may also be used. Mix until powder is visibly dis-
tributed fully.
6. Add predetermined amount of fatty acid to the crutcher
to produce magnesium soap. Ideally, the acid should be
added in a molten form at 75-85'C (167-185F). If added
as a powder, continue mixing until powder is visibl~
melted.
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WO 92/16609 . ` 2 1 0 ~; O ~ O PCI/US92/00689
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7. Add predetermined quantity of sarcosinate solution at
ambient temperature to the crutcher. Allow crutcher to
return to target temperature.
8. Add predetermined quantity of molten paraffin at 75-85'C
(167-185-F) to the crutcher. lf flakes of paraffin are
added, allow paraffin to melt completely.
9. Allow contents of crutcher to completely mix and react
until the pH of the crutcher reaches a target of
7.3-8.0, while maintaining the crutcher t~mperature at
75-85-C (167-185'F). This typically takes 20-40
minutes.
10. Add predetermined ~uantity of excess fatty acid, at a
temperature consistent with the previous fatty acid
addition. Allow the crutcher to mix for an additional
10 minutes.
II. Crutchinq - Ion Exchanqe
1. In the crutcher, put the required amounts of soap, fatty
acids and triglyceride at 82-88'C (180-190'F) and mix
until homogeneous, approximately 10 minutes.
2. Solubilize the MgCl2 in water and add to the crutcher.
Continue to mix at 82-88'C (180-lgO'F) until reaction is
complete, approximately 10 minutes.
3. Add the liquid sodium lauroyl sarcosinate, the sodium
cocoyl glyceryl ether sulfonate, and the amine oxide to
the crutcher, maintaining the temperature at 82-88C
(180-l90'F). Mix until homogeneous, approximately 10
minutes.
4. Add the desired amount of Polyoxyethylene WSR-35 and mix
for 5 minutes.
Drvina for Both I. and II.
The crutcher mix is dried and cooled using a combination
flash chamber and chill roll or chill belt. The crutcher mix is
first heated to approximately 132-C (270-F) by a heat exchanger
and then flash dried in a chamber above the chill roll or chill
belt. From the flash chamber the hot, dried mix is extruded onto
the chill roll or chill belt. The chill belt or chill roll
provides a uniform, thin, cool (29-35C, 85-95F) product in flake
or chip form. Typical moisture for the flake is 2-12%, preferablv
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WO 92/16609 ~ .1 U 5 0 !) O PCI/US92/OlK89
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6-8%. The ways to regulate the moisture, in the order of prefer-
ence, are (1) increasing or decreasing steam pressure on the heat
exchanger; (2) increasing or decreasing crutcher mix rate to the
heat exchanger; and (3) increasing or decreasing crutcher mix
temperature to the heat exchanger.
Amalqamatinq
The flakes are weighed and mixed in a batch amalgamator to
obtain uniform flake size. Preweighed perfume is added to the
flakes and mixed in the amalgamator to obtain the desired finished
product perfume level. The perfumed flakes are transferred to the
mill hopper or directly to the plodder.
Millinq (ODtional)
The 3-roll soap mills are set up with the first roll at 38C
(100F) and the other two mills at about 21-C (70-F). The soap is
passed through the mills several times to provide a homogeneous
mixture of perfume and dried flakes.
P oddinq and Stampinq
The plodder is set up with the barrel temperature at about
21'C (70-F) and the nose temperature at 38-49'C (100-120'F). The
ideal plodder is a dual stage plodder that allows use of a vacuum
of about 15-25 inches of Hg. The plugs should be cut in 5"
sections and stamped with a cold die block using die liquor such
as alcohol, if appropriate.
EXAMPLES
The following examples and methods are illustrative and are
not intended to limit the scope of th4 invention(s~. The detailed
methods of making and purifying generic alkyl glyceryl ether
sulfonate per se are disclosed in U.S. Pat. No. 2,988,511, sucra.
incorporated herein by reference. The percentages, ratios, and
parts herein are on a total composition or surfactant weight
basis, as indicated, unless otherwise specified. All levels and
ranges, te~peratures, results etc., are approximations unless
otherwise specified.
The mild personal cleansing bars of Examples 1-7 are mabe
using the above preferred crutching neutralization process.
Example 8 is made by adding magnesium chloride to Na soap to for~
the Mg soap by ion exchange before mixing with the synthet~-
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WO 92/16609 2 1 0 ~ ~ 9 0 P~T/US92tO0689
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surfactants. Comparative Example A is made similar to the bars of
Examples 1-7, except that sodium hydroxide is used instead of
Mg(OH)2 and is used as a standard for the mildness and smears.
Comparative Example B is the "B" bar and is used as a second
standard for the mildness and smears. Comparative Example C is a
leading commercial all soap bar and is used as a standard for
typical all soap bars. Example 3 is the preferred overall bar for
mildness, lather, and smears.
Two bar smear tests are disclosed below, the "Mush Smear 1"
and the "Bar Character Smear 2."
Mush Smear "I" Test Procedure
EauiDment:
1. #2-202C Fisher Brand Hexagonal Polystyrene weighing dishes
(4" x 3").
2. ~14-366A Fisher Brand Spatula.
3. Balance capable of weighing to two decimal points.
4. 120-F Temperature Room.
5. Timer.
Test Method
1. Label and weigh the number of weighing dishes needed (two
weighing dishes per sample, one labeled M for mush dish, one
labeled S for soak dish).
2. Weigh the original bar and record the weight. Place bar in
preweighed dish labeled S.
3. Add 30 mls room temperature city water to the dish containing
the bar prototype (pour water down side of weighing dish).
Add 30 mls room temperature city water to the dish containing
the control`bar. When placing the bars in the dish make sure
the bars are not touching the sides of the dishes. -'
4. Allow bars to soak in weighing dishes at room temperature for
2 hours undisturbed.
5. After 2 hours of soaking, pick bar up carefully and allow ~o
drain into the same dish for 15 seconds.
6. After 15 seconds, invert bar and place in preweighed dlsn
labeled M. -
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7. Weigh soaked bar and record.
8. Scrape the wet surface or mush from the bar, with a spatula,
into the same preweighed dish labeled M, weigh and record.
Best results for scraping are seen when the spatula is held
loose in hand being careful not to gouge the bar or to scrape
too deeply. When the surface of the bar no longer appears to
look wet or shiny, scraping is completed. To e1iminate
variability of scraping from person to person7 results from
each test will be reported relative to the control placed in ?
that test.
9. Weigh and record the scraped bar.
10. Place the soak dish, the mush dish, and the scraped bar in
the 120'F Temperature Room for water evaporation for 48
hours.
11. After 48 hours, weigh and record the dry weight of the soak
disht the mush dish and the scraped bar.
12. Calculate the surface area of the scraped portion of the bar
by measuring (in inches) length times width.
13. Add the number of dry grams of mush (smear) to the number of
dry grams of soak. This is the overall result in grams.
All series of testing should include control, and all samples
should be run in duplicates. A maximum of 7 products (6 plus a
control) can be tested at one time, and an interval of 10 minutes
between every 4 samples should be allotted for the addition of
water as tu not a110w any products a lag time for soaking longer
than 2 hours.
Bar Character Smear "2" Test
5 ml Smear Test
E~uioment
"Alathon" soap dishes
Small measuring cylinder
Method
1. Wet soap bar to be tested by dipping surface to be soaked in
distilled water and shaking off excess water. This procedu~e
leads to more uniform bar smear.
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WO 9Z/16609 2 1 0 ~i O !3 0 PCI/U592/l)O689
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2. Place bar centrally on '`-Alathon" dish containing 5 ml of
distilled water. Rock dish to break water tension. The
Alathon dish was selected as being a standard, readily
available (in U.S.) dish with low ridges.
3. Store overnight (approximately 18 hours) in standard con-
ditions of temperature and humidity (27'C/80-F/80% RH were
used). As this test measures the bar's ability to recover as
well as absorb water, standard conditions avoid seasonal
variations which may occur in uncontrolled laboratory over-
night conditions.
4. Next morning, remove bar with a careful vertical lift andinvert for judging.
Judqinq
Bar Smear - Each judge grades soap bar smear by fingering the
15 bar and taking into account both types of smear and amount of
smear.
Grade Smear DescriDtion
Excellent
9 Very good smear
20 8 Good smear (Target)
7 Siightly poorer than desired
6 Marginal but still acceptable
Minimum acceptable smear
4 Poor and unacceptable
25 3 Very poor smear
2 Poorest normally seen
1 Extremely poor smear
Clinical Assessment of the Toilet Bars
The clinical test procedure used to evaluate several toilet
bar formulations for skin mildness is given below.
Mildness Forearm Wash Test Procedure
The washings are performed by a technician. Each panelist is
assigned a set of 8 products for washings, 4 per arm. The test
35 procedure for each arm is:
.
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WO 92/16609 P~/US92J00689
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Protocol
l. Place 3M Micropore surgical tape with 4 precut 3.2 cm
diameter holes on the volar forearm. Center tape on the
lower inner forcarm trying to keep the lower treatment
area away from the wrist area.
2. ~et the forearm with warm (35-40-C) water.
3. Wet a nonwoven paper towel (Masslinn Towel, Chicopee
Mills, New Brunswick, New Jersey) with w~rm water. Rub
the towel on the appropriate test product using a
circular motion for 6 seconds.
4. Rotate the towel at each test site for 10 seconds.
5. Allow lather from the test products to remain on the
test site for 90 seconds.
6. Rinse each site with warm water (35-40'C) for 15
seconds.
7. Pat area dry with soft, disposable (BOUNTY~) paper
towel.
8. Wait 2 minutes and repeat above procedure for a second
time.
9. This procedure is to be followed 2 times daily, for 4
consecutive days, and 1 time the final day of the study,
for a total of 17 washings. Each of the daily visits
will be approximately 3 hours apart. A visual inspec-
tion of each test site is to be made just prior to the
second wash procedure of the third day and 3 hours after
the final wash of the fifth day. Observable dryness and
erythema will be scored at each examination period.
lO. The following grading scales are used:
Clinical Test Skin Grading Scales
The forearm skin grading scales reported herein are set out
below.
Forearm Gradinq Scale - Skin Drvness
O Perfect skin.
l.O Patches of checking and/or slight powderiness
and occasional patches of small scales may be
seen. Distribution generalized.
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2.0 Generalized slight powderiness. Early cracking
or occasional small lifting scales may be present.
3.0 ~eneralized moderate powderiness and/or
moderate cracking and lifting scales.
4.0 ~eneralized heavy powderiness and/or heavy
cracking and lifting scales.
5.0 Generalized high cracking and lifting scales.
Eczematous change may be present. Powderiness
may be present but not prominent. May sPe
bleeding crack.
6.0 Generalized severe cracking. Eczematous change
may be present. Bleeding cracks may be present.
Scales large, may be beginning to disappear.
Forearm Grading Scales - Skin Ery~hema
0 No redness
1.0 Barely detectable redness
2.0 Sl;ght redness
3.0 Moderate redness
4.0 Heavy or substantial redness
5.0 Severe redness
6.0 Extreme redness
The term "generalized" as used herein means that more than
50% of the surface area of the forearm exhibits the attribute.
Whole unit skin grades reflect generalized condition. Half units
are used to represent intermediate conditions. -
Flex Test Wash
Protocol
1. Wet one sponge under warm, about 37-C (95-lOO'F) water
until completely wet.
2. Squeeze the sponge 3-4 times to remove excess water.
3. Lather the moistened sponge, in a circular motion.
directly on the test bar for 10 seconds.
4. Wash the appropriate test areas of the inner volar
forearm for 60 seconds (i.e., washing motions of 2-3
circular revolutions per second).
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W~ 92/16~09 2 1 0 5 V .~ ~ PCI/U~;92/00689 '.
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S. Thoroughly rinse the wash area and pat dry with a paper
towel ~15-second rinse recommended).
6. This procedure is to be followed 3 times daily for 5
consecutive days for a total of 15 washings. Each of
S the daily wash procedures will be approximately 2 hours
apart. A visual inspection of each test site is to be
made just prior to the next wash procedure. Observable
erythema will be scored at each examination period. The
final examination is to be made about 2 hours following
the last wash procedure.
7. The following erythema scoring scale is to be used:
O = no evidence of erythema
1 = slight erythema (spotty and/or minimally
perceptible)
2 = moderate erythema (more uniform, pink-red)
3 = marked erythema (uniform, relatively brighter
or deeper red)
Intermediate 0.5, 1.5, 2.5, and 3.5 increments may also
be scored with necessary.
8. Arms are no longer subjected to the washing procedure if
a rating of "2" or greater is attained. The score of
"2" is assigned for the remainder of the study.
9. Products are statistically compared by examining the
number of Grade 2 or higher ratings. The fewer the
number of these ratings, the milder the product is
judged to be.
In the following Examples, which include magnesium soap, some
or all of the magnesium soap can be replaced with other alkaline
earth metal soap such as calcium, zinc, aluminum, and other soaps,
which are substantially insoluble on the order of magnesium soap
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TABLE 1
Ex. 1 Ex. 2 Ex. 3 Ex.
Inqredient Wt.% Wt.% Wt.% Wt.%
Magnesium Soap
(Cocoate) - 33.0 - -
(Laurate) 29.7 - 22.5
(Stearate~) - - 38.0
(75 Tallow/25 Palm
Kernelate)
o Sodium Soap
(50 Tallow/SO Palm
Kernelate) 1.4
Sodium Cetearyl Sulfate 11.8
Sodium Cocoyl Glyceryl
Ether Sulfonate 15.7 25.0 21.0 40.9
Sodium Lauroyl
Sarcosinate 6.9 7.0 12.0 7.5
C12-13 Alkyldimethyl
Amine Oxide
Lauric Acid 2.9 - 3.0 3.2
Coconut Acid - 3.0 - -
Sodium Chloride 1.0 1.0 1.5 1.5
Sodium Sulfate 1.5 1.5 1.85 1.5
Paraffin (M.P. 55-C)14.7 17.0 10.0 10.7
Triglyceride I-8
Hardstock
Polyoxyethylene WSR-35
Titanium Dioxide 0.2 0.2 0.2 0.2
Fragrance 1.0 1.0 1.0 1.0
Water 10.1 8.7 9.3 6.8
Miscellaneous 3.1 2.6 1.7 4.2
Totals100.0 100.0 100.0 100.0
*Emersol 132 (Emery Industries) is really a mixture of
stearate and laurate having a titer of about 55 and a
maximum I.Y. of 0.5.
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Ex. 1 Ex. 2 Ex. 3 Ex. 4
Smear 1 (Mush Smear "1" Test described belowJ
Wet (grams)* 0.66 1.44 1.51 1.93
Dry (grams) O.S8 0.52 1-11 0.86
5Average 0.62 0.98 1.31 1.40
Smear 2 (Method described below)
5 ml.** 7.5 7.5 6.5 7.5
pH 8.02 7.45 7.55 7.41
Soap/FFA ratio 10:1 11:1 12.2:1 7:1
*Lower numbers the better.
**Higher numbers the better.
The totals for: lathering mild synthetic surfactant; mag-
nesium soap; non-soil-load, non-lathering surfactant; and soil
load diluent for Examples 1-4 are as follows:
Totals Ex. 1 E_. 2 Ex. 3 Ex. 4
Mild Lathering
Synthetic
Surfactant 21.5 ~0.25 31.53 45.54
Magnesium Soap 29.7 33.0 38.0 22.5
Non-Soil, Non-
Lathering Diluent
(including Mg Soap) 42.6 34.75 39.47 25.36
Soil Load Diluent
(FFA, Wax, Tri-
glyceride) 17.68 20.0 13.0 13.9
Mg Soap/Total
Synthetic 0.9:1 1:1 1.15:1 0.5:1
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W o 92/J6609 2 1 ~ ~ 9 PCT/US9~/~0689
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TAB~E 1 (Continued)
Ex. 5 Ex. 6 Ex. 7 Ex 8
Ingredient Wt.% wt.% wt.% Wt.%
Magnesium Soap
(Cocoate)
(Laurate) 12.8 24.0
(Stearate*) - - 10.0
(75 Tallow/25 Palm
Kernelate) - - - 27.6
Sodium Soap
(50 Tallow/50 Palm
Kernelate)
Sodium Cetearyl Sulfate 32.1 - 14.0 -
Sodium Cocoyl Glyceryl
Ether Sulfonate 17.1 35.0 32.0 13.6
Sodium Lauroyl ::
Sarcosinate 7.4 7.0 10.0 15.9
C12 13 Alkyldimethyl
Amine Oxide - - - 2.3
Lauric Acid 3.2 3.0 5.0
Coconut Acid - - - 7.9
Sodium Chloride 1.5 1.5 1.5 3.7
Sodium Sulfate 1.5 1.5 1.85 0.6
Paraffin (M.P. 55'C) 12.6 13.0 13.0
Triglyceride I-8
Hardstock - - - 16.1
Polyoxyethylene WSR-35 - - - 0.4
Titanium Dioxide 0.2 0.2 0.2 0.25
Fragrance 1.0 1.0 1.0 1.0
Water 7.4 10.2 7.5 9.0
Miscellaneous 3.2 3.6 3.9 1.6
Totals 100.0 100.0 100.0 100.0
*Emersol 132 (Emery Industries)
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~ Ex. 6 Ex. 7
Smear I
Wet (grams)* 2.35 2.38 4.26 N/A
Dry (grams) 1.37 1.64 2.00 N/A
Average 1.86 2.01 3.10 N/A
Smear 2
5 ml.** 7.5 7.0 6.5 8.0
pH 7.97 7.57 7.59 8.00
Soap/FFA ratio 4:1 8:1 2:1 3.5:1
*Lower numbers the better.
**Higher numbers the better.
N/A = Not available.
The total level of synthetic surfactants in Example 7 is 56%,
and the water level is 7.5%; the ratio of Mg soap to total
synthetic is 0.18:1. The smears could be improved in Example 7 by
lowering the water level to below about 7%. Note that Example 5
which has a total synthetic of 56.6% and a Mg soap to total
synthetic ratio of 0.22:1 but has a higher Mg soap level, 12.8%
vs. 10%, has a better smear, notwithstanding equal water levels
for Examples 5 and 7.
For improved smears, it should be noted that when the mag-
nesium soap level is low, e.g., 10% or less, and when the level of
the total synthetic surfactant(s) to magnesium soap is more than
5:1, the water level of the bar should be from about 2% to about
7%, preferably from about 2.5% to about 6% for improved smear.
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TABlE 2
COMPARATIVE EXAMPlES A-C
~x. A Ex. B Ex. C
Inqredient Wt % Wt.% Wt.%
_.
Sodium Cl2/cl4/cl6/cl8 ~
58/21/10/g/.. (AGS) 48.2
Sodium Lauroyl Sarcosinate 12.5
Sodium Cocoyl Isethionate - 49.1
Sodium Linear
Alkylbenzene Sulfonate - 2.0
Lauric Acid 6.5 - -
Stearic Acid 9.8 25.0
Sodium Chloride 5.3 O.S 0.81
Sodium Sulfate 1.3
Sodium Isethionate - 6.0
Sodium Soap
(60 Stearate/40 Laurate) 7.2 12.0
(85 Tallow/15 Cocoate)
(75 Tallow/25 Cocoate) - - 75.25
Titanium Dioxide 0.25 0.4
Fragrance 1.0 1.0 0.16
Water 3.5 4.0 23.5
Miscellaneous 4.4 - 0.28
Totals 100.0 100.0 100.0
Comparative Example A is an ultra mild bar having fairly good
smear, about the same as the 'IB'' bar, a mild, commercially avail-
able, soap/synthetic bar. Comparable mild bars of this invention,
e.g., Examples 1-6 and 8 have improved smears over Example A, as
well as the Standard Comparative Example B, which is the "B" bar.
Comparative Example C is a leading pure soap bar to show ~he
superior mildness of the bars of this invention over it.
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Ex. A Ex. B Ex C
Smear 1
Wet (grams)* 3.20 3.66 -
Dry (grams) 1-50 1.43 .
Average 2.35 2.55 -
Smear 2
5 ml.** 7 5 7.0 7 0
pH 7.3 7.3 9.5
Soap/FFA ratio 0.4:1 0.5:1 1:0
*Lower numbers the better.
**Higher numbers the better.
Summarv of AGS Surfactant Chain lenqths Used in ExamDles
lS % Chain Lenqth Distribution % Cl6-cl8
Example _12 _14 _16 _18Chain Length
1-8 68 25 7 - 7
A* 58 21 10 9 19
*Comparative Example A.
The average smears for Examples 1-6 are better than Compara-
tive Example A, notwithstanding the higher AGS alkyl chain distri-
bution, more C16 and 9~O C18 on an AGS weight basis.
Mildness Test Results
Flex Test*
Ervthema
Ex. C 2.42
Ex. 4 1.18
Ex. 3 o.go
Ex. 7 0.68
Ex. B 0.65-1.29
Ex. 8 1.59 Previous Test
Ex. A 1.09 Previous Test
In the above Flex Test Erythema Results, the lower the
erythema, the milder the personal cleanser. Comparative bar
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Example C, a leading all soap bar, has the highest erythema grade
of 2.42. Examples 4, 3, and 7 have erythema grades comparable to
the "B" bar which show grades of from about 0.65 to about 1.29,
the low and the high of four "B" bar grades. The erythema grades
for 4, 3, and 7 are, respectively, 1.18; 0.90; and 0.68. The
erythema grades for Example 8 and Comparative Example A are better
than the all soap bar, Example C, and are close to the "B" bar.
The "B" bar results 0.65-1.29 are the low and high of four
side-by-side Flex Tests for Examples C, 4, 3, and 7. The Flex
Test results for Examples 8 and A, while not part of the Example
C, 4, 3, and 7 test series, are shown to suggest that Example 8 is
not as good as "B," but milder than the all soap bar, Comparative
Example C. It is noted that Example 8 has less preferred fatty
matter, specifically a lower titer (37) and a higher Iodine Value
(38) than Examples 4, 3, and 7. The tîters and I.Y.'s for
Examples 4, 3, 7, and 8 are:
ExamDle Titer Iodine Value
4 41-44 Maximum 1.0
3 54.5-55.5 Maximum 0.5
7 54.5-55.5 Maximum 0.5
8 37 38
Referring to Table 1, Example 8, however, has an excellent Smear 2
25 of 8.
Forearm Clinical*
Redness DrYness
Ex. 8 1.18 1.68
Ex. A 1.19 1.66
Ex. A 1.16 1.70
Ex. B 1.70 S 2.22 S
Ex. 2 1.37 1.44
Ex. B 1.69 S 1.63 S
*Lower numbers the better.
S = Significance at 90-95% confidence.
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Forearm Clinical results suggest that Examples 8, 9, and 2
are all better than "B" for both Redness and Dryness. Examples 8
and A are about equal, and A is significantly better than B.
Example 2 is also significantly better than "B."
Example 2 also has superior smears over "B" as shown in
Tables 1 and 2; Average Smears 1 are 0.98 for Example 2 vs. 2.55
for "B," which shows a significant advantage for Example 2.
Smears 2 are 7.5 for Example 2 vs. 7.0 for "B," which is a slight
advantage for Example 2.
A panel of experts compared some sensory characteristics of
Example 2 with those of the "B" bar. The results are: Example 2
has sensory characteristics, tightness, smoothness, and softness,
comparable to the "B" bar. The tightness result is surprising in
view of the presence of 33% magnesium soap in Example 2.
WHAT IS CLAIMED IS:
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