Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
:
WO 92/07931 PCI/VS91/07774
209~039
SYNDET 8AR WITH LONG CHAIN ALKYL SULFATES FOR IMPROVED
PROCESSABILITY AND BAR CHARACTERISTICS
\
TECHMICAL FI~D
Tilis inven~ion rela~es to cleansing bars based on synthetic
surfac~an~s and to processes of making them.
BAC'<GROUND OF THE IN'/ENTION
Syn~hetic surfactant-based personal cleansing bars 'nave
attract2d much interest rec~ntly becaus2 they tend to be milder to
the s.~in than soap-based products. This mildness, however, comes
with negatives to both the manufacturer and the consumer. The
manufacturer experiences difficult processability due to the
sticky nature cf such products, as well as high raw material
costs. The consumer experiences the negative performance prop-
erties of smear, bar softn~ss and consequently high wear rates.
There is a strong need to develop a mild bar product that is
easily processable on conventional equipment while having accept-
able in-use characteristics.
OBJECTS OF THE INYENTION
This invention relates to skin cleansing syndet bar compo-
sitions which provide improved processability and still maintain
consumer acceptable bar quality. Therefore, one obJect of this
-- invention is to provide a composition which exhibits improved
processability.
SUMMARY OF THE INVENTION
This invention is an improved mild personal cleansing syndet
- bar comprising: at least about 18% by weight long chain alkyl
sulfate having essentially saturated Cl5-c22~ pre~erably C16-C18~
alkyl chains, preferably cetearyl sulfate, combined with a
~5 selected plasticizer preferably selected from paraffin, fatty
acids, and polyethylene glycols, and mixtures thereof.
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W o 92/07931 PCT/US~1/07774
2~ 2 -
DETAILED DESCRIPTIO~ OF THE INVENTION
To de~/olop a mild syn~hetic surfactant-bas~d bar ~ithout the
processability and perfo~nance n~gat;ves outl;n~d aboYe, it is
advantageous to think of ~he bar as C',10 separate components: the
matrix and the ~ctiv~s. The matrix pro~;d2s the physical charac-
teristics (proc~ssability and bar mPssin2ss) ~hile the actives
provid~ lathoring and mild prop~rties. ThQ matriV7 if not chosen
correc-cly, can ;mp~de lacnor gPnenation, cause poor bar fPel,
enhance ~ear ra`~e oeyond an asseatable lsYel, and/or reduce
product mildn~sà. LikaYiae, ';il.? lCti`/.'S illUst be chosen 50 as co
provide acc~ptaDIa 'i~Yeis or iathering ni',;ilollr negaci~aiy impac~-
ing milciness, a co~on trade~i- in ;;ornu'1ations.
It will be appr~cia'ced thac che de~1elopment or an appropriate
matriV is a delicatq ~alancing 3ct, bet~ Qn plastir.i~,y and brittle-
ness whil2 not compru~ A,3 lather pelAf~~^manc . Typical matrixmaterials such as triglycerides, fatty alcohols, monoglycerides,
etc., tend to form a sufficiently plastic matrix but also tend to
depress lather potential. Other commonly used matrix materials
~ such as salts, sugars, polysaccharides, etc., tend to make an
; 20 overly brittle and water-soluble matrix that induces poor bar
messiness performance.
' Disclosed is a syndet bar comprising: (1) from about 18% to
about ~5%, preferably from about 20% to about 4SX, of C15-C22~
preferably C1~-C1g, essent,ally saturated lung alkyl (chain)
sulfates; (2) from about 10% to about 50%, preferably from about
15% to about 40YO plasticizer; (3) from about 10% to about 45%,
preferably From about 15Yo to about ~0~0, hign lathering, mild
surfactants; (4) 'From 0~0 to about 20%, pre~erably ~rom 5% to about
' 15%, sodium soap;`and (5) from about 2% to about 107o, preferably
; 30 from about 3X to about 8%, water.
The long chain alkyl sul~ates, as defined herein, comprise
said long chain alkyl chains at a level of at least about 90%,
preferably about 93YO~ and more preFerably about 97%. The long
chain alkyl sulfates are deriv2d from corresponding saturated
straight chain alcohols. The preTerred alkyl sulfate has a ratio
of C16-C1g in the range of from about lOOYo C15 to about 100% C18
by weight. A commerciallY avallaole C16-C1g alkyl sulfate is
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w o 92/07931
PCT/~S91/07774
- 3 - 2 ~ 9 ~ 0 3 9
SIPON~ EC-1I1 (formerly SIPEX4 EC-1II), sodiumicetearyl sulfate,
which is approximat31y ~0~0 C10 ~nd 36~, C1g. SIPONa EC-I11 is sold
by Alcolac Company, ~ltimore, MD 21226. Another source is Henkel
Corp., Ambler, ~A 19002. Henkel's sodium cetearyl sulfate,
LANETTE E, is an estimated ~0-5GYo C16-C1g al~yl sulfate sold as an
emulsi T i er.
The terms "s;~nth3tic bar," also "syndet bar," as used herein
mean chat tha bar has mor~ syntn~cic iur;actant than soap unless
other~ise specil1ed. T,le tarm "'S syndet bar" mrans a syndet bar
IO containing ~lkyl sul; te ,sl.li';i3C,a,lt~ Tild ~a'~^m "long chainl' maans
C1s and G2~, and mi;ctures cnereo,.
Th2 percancases, ratios, and ~arti hersin are on a total
composition weight basis, unless ocher~ise speci~ied. All levels
and ran~es herein arr approvi~atisns unless othe~ise specified.
IL jS not3d th~ sur,actant mildness can be measured by a
skin barrier destruction test which is used to assess the irri-
tancy potential of surfactants. In ~his test the milder the
surfactantj the lesser the skin barrier is destroyed. Skin
barrier destruction is measured by the relative amount of radio-
labeled water (3H-H20) which passes from the test solution through
the skin epidermis into the physiological buffer contained in the
diffusate chamber. This test is described by T.J. Franz in the
J. Invest. DermatQl., 1975, 6~, pp. I90-195; and in U.S. Pat. No.
4,673,i25, Small eL al., issued .,une lS, I987, incorporated her21n
by reference, and which disclose a mild alkyl glyceryl ether
sulfonate (AGS) surfactant based synbar comprising a "standard"
alkyl glyceryl ether sultonate mixture. Barrier destruction
testing surprisingly shows that the long chain alkyl sulfates are
milder than standard AGS.
Thq long chain alkyl sulfate comprises 18-55~ by weight of
the bars of this invention. Other syndet bar ingredients are
selected from: other surfactants, polymeric skin feel aids, moist-
urizers, plasticizers, fillers, etc. A preferred syndet bar
; comprises: about 20-~5% of cetearyl sulfate; 5-15% soap; and about
1-35%, preferably about 5-30%, moisturi~er; lO-50% plasticizers;
and 2-10%, prefQrably 3-8%, water. To insure mildness and bar
firmness, the synthetic detergent surfactant system in the bars
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WO 92/07931
P~r/US91/07?~4
3~ - 4 -
sh contain the long chain alkyl sulfate.
Other detergent surfactants can be uséd; particularly from
about lO~o to about 50%, preferably from about 15% to about 40%, of
lather enhancing detergent co-surfactant, e.g., mild ones, e.g.,
sodium lauroyl sarcosinate, alkylglycerylethsr sulfonate, and
sulfonated fatty acids. NumProus P~amples of othPr surractantr.
are disclosed in the patents incorporated herein by reference.
TheY include l;mited amounts of other al~yl sulFates, anionic acyl
sarcosinates, methyl acyl taurates, ~I-acyl glutamates, acyl
ise~hionates, alkyl sulfosuccinates, all~yl phosph~ta esters,
e~hoxylated alkyl phospha-Le esters, -~rideceth ..ulfa'ces, protei
condensat~s, mixtures of ethoxylated alkyl sulrates and ~ yl
amine oxides, betaines, sultaines, and mi~tures thereof. Included
in the surfactants are the alkyl ether sulfates ~ith 1 to 1~
- 15 ethoxy groups, especially ammonium and sodium lauryl ether sul-
fates. Alkyl chains for these other surfactants are Cg-C22,
preferably C1o-C18~ The acyl esters of isethionic acid salts,
with esters of C16-C1g acyl isethionates and no more than 25% or
lower C14 acyl groups are also useful. Preferred is stearoyl
isethioniate with C14 3%; C16 50%; and C1g 47%. Alkyl glycosides
and methyl glucose esters are preferred mild nonionics which may
be mixed with other mild anionic or amphoteric surfactants in the
I compositions of this invention. The bars of this invention can
have up to about 10% of shorter chain or traditional (cocsnut-)
alkyl sulfates and still maintain the mildness requirement of the
` bar.
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~; A second essential material of the present invention is a
plastic binder, also referred to herein as a plasticizer. The
syndet bar of this invention also comprises from about 10% to
about 50X., preferably from about 15X to about 40X., plasticizer.
The plasticizer can be chosen from a group, but not limited to,
paraffin, fatty acid, fatty alcohols, polyethylene glycols. The
- above-mentioned nonionic surfactants, e.g., tallow alcohol ethoxy-
lates (TAE), e.g., TAEgo, TAEg, etc., are also good plasticizers.
Other plasticizers (binders) are identified in the published
literature such as J. Amer. Oil Chem. Soc. 1982, 59, 442.
The preferred cation in the AS salt is sodium. HoweYer,
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WO 92/0793~ PCr/US91/07774
- 5 - 20 9 ~ 039
other cations such as triethanolammonium (TEA), ammonium, and K,
etc., are also usable. As used herein the term "cationic polymer"
includes naturally and synthetically derived cationic polymers.
The abbreviation "CN" means coconut and "T" means tallow herein,
unlPss otherwise specified. Al~-percentages and proportions are
by weight, unless otherwise specified.
A preferred synbar contains a mixture of free fatty acid (or
polyethylene glycol) and paraffin at a ratio of from 3:1 to 1:1.
A preferred AS synde~ bar also contains from about 10% to
about 3$~, moisturizer, preferably one selected from glycerin and
Fre2 Fat~ acid or mixtures thereof. In this case, the freD fatt~
ac1d s~rJes thD purposs as mois~urking and plastici~Dr
- ingredient.
The syndet bar of this invention may comprise 0% to aDou~ 5~/O
of a suitably fast hydrating cationic polymer. The polymers have
molecular weights of from about 1000 to about 3,000,000.
The cationic polymer (skin conditioning agent) is selected
from the group consisting of:
(I) cationic polysaccharides;
20 (II) cationic copolymers of saccharides and synthetic
cationic moncmers, and
(III) synthetic polymers selected from the group consisting
of:
-(A) cationic polyakylene i~ines
(B) cationic ethoxy polyalkylene imines, and
(C) cationic poly~N-[-3-(dimethylammonio)propyl]-N'-[3-
(ethyleneoxyethylene dimethylammonio)propyl]urea
~ dichloride3.
; Specific examples of members of the cationic polysaccaride
-~ 30 class include the cationic hydroxyethy1 cellulose JR 400 made by
~; Union Carbide Corporation; the cationic starches Stalok~ 100, 200,
300 and 400 mada 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-
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W O 92/07931 PCT/~S91/07774
2a9~~9 - 6 -
allyl,N-~i-dialk~l ammonium chloride a~ailable from Niational Starch
Corporation under the trade name Celquat.
The cationic -,yni.',le ic pol~i77ers u~fl1l in the present in-
vention ar~ c~tionic pol~al'~ylene iri?in^,s, e1choxypolyal'~le7ne
imin2s, l"~7 j~jol~?l-,-3~ i?~ ,i"ic,710)-ir~ [3~ h~lqn2-
oxyethylene dimechylalnrnonio)sropyl~uP~a dichloridei the latt~r of
~hich is ~ ?l?.~ F ~ fq~ nt~?i~ C!~m~n~7 Inc. ~Ind~r ~h~
trademar;~ oF,1iranol A-lX, O,'~S ~-e5. ,'o. ~ 555-3~-2.
?r~;ar,^?d ca~ionic o~l~mia~fic S~iil cr~nditi oning agents of tha
pr~sen~ ,n~/enirinll ar~ t/lmose catin7ic po!~s7cc!7arides of t'ne
J .~ 3~ r; ~ 7 01~7~ r ~
3, OOO, ~ o`~ '?, .?'`r''~ S 'r'? -; r~ln ~,5~O co
350, C(~ ';3 ,~31~",~,r~ ;l.,'J ` 1 i~o ~ C,~-077" ~mpY i ~qd
of c?-~lactoma7^,nall uni~s a,ld a d~gr~e o; calionic suostitution
ranging from about 0.0~ per anhydroglucosa unit to about 0.80 per
anhydroglucose unit with the substitu2nt cationic group being the
adduct of 2,3-epoxypropyltrimethyl ammonium chloride to the
natural 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 to
be suitably and fully hydrated and subsequently well incorporated
; into the soap matrix.
Other ingredients of the present inven~ion are selectPd for
the various applications. E.g., perfumes can be used in formu-
lating the s'~in cl~ansing products, g~nerally at a level of from
about 0.1% to about 1.5X of the comp~sition. Alcohols, hydro-
tropes, colorants, and fillers such as talc, clay, calcium carbo-
nate and dextrin can also be used. Cetearyl alcohol is a mixture
of cetyl and stParyl alc^hols. Preservatives, e.g., sodium
ethylenediaminetetraacetatP (EDTA), generally at a level of less
- than lYo Of the composition, can be incorporated in the cleansing
products to prevent color and odor d2gradation. Antibacterials
can also be incorporated, usually at ls~els up to 1.5%. The
following pac~ncs disclose or r~rer to SUCIl ingredients and
formulations whicn can be used in the soap/synbars of this inven-
tion, and are incorporated herein by rsfPrence:
w o ~2/07931
pCT/US9I/07774
- 7 2~ 9 ~ 039
Pat. No.Issue Oate Inventor(s)
~,234,4~4 ll/19~0 ~orshauser
4,061,602 12/1977 Oberstar et al.
~, 472, 297g/i984 Bolich et al.
~,~91,53g 1/1985 Hoskins et al.
~', 540, 507'~l 198~ Grollier
4,673,5~5 o/1987 Small et al.
"7o4~L2 411/1~87 Saud
4,312,253 3!1989 ~mall et al.
~,32c,il.a73/19~ ,edcalf et al.
356l,2823/13~9 2ys et al.
The syndet bars of this inv2n~lon have a p'~ of from ~ to 9 in
a 1% aqu40lls solution. The pr~forr2d pH is i to 8, mor~ prefer-
; 15 ably about 7.
LaboratorY Assessment Qf Bar
; The following test procodures are used to evaluate thecritical bar performance attributes of mildness and bar processa-
bility.
Rollinq Cvlinder Adhesion Test (RCAT) Methodoloqy
The rolling cylinder adhesion test (RCAT) is designed to
simulate the adhesion of the processed synbar formulation to the
surfaces of the proc ssing equipment (dryingjflaking/plodding/-
milling/stamping). It has ~een sho~Jn to corre~late with s~ickiness
of products during processing. This stickiness is inversely
related to overall bar processability. The synbar of this inven-
tion has a Relative RCAT (Rolling Cylinder Adhesion Test) Value of
less than 1, preferably less than O.g, and more preferably less
than 0.8. A Relative RCAT Yalue of 1 is assigned to a comparable
;~ ~ 30 bar made without the proc~ssing aid.
The equipment used for this test is the following. An
incl-ined plane (15) with raised edges is used as the base for the
rolling cylinder. The cylindar itself is mad from plexiglass
tubing of 4" outer diameter and 11-7/8" overall length; it weighs
735.2 grams.
All evaluations are conducted in a constant temperature/-
humidity environment at 80F (26C) and 15% relative humidity.
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WO 92/07931 PCr/US91/07774
~o9~039 - 8 -
The synbar product to be tested is grated into small pieces (about
2 mm in length). About 20 srams of the grated product are spread
evenly over the surface of the inclined plane (which is covered
wi~h Kraft freezer paper). The preweighed cylinder is then placed
at the head of the inclined plane and allowed to roll freely over
the material until it reaches the end of the run. Tha cylinder is
re~eighed, the difference being the weight of material adhering to
it. The high2r the amount of material adhering to the cylinder,
the stickier the product and the more d;ffic~lt to process. T'ne
data is ~xprassed as a percentage of material stuc~ to the c~l-
ind2r (RCAT ~-~,) relative to the amount or material available (20
grams).
1~ Table 1 below, syndet bar Examples 1-45 (described in more
detail belo~ in the Examples s~ction of Table 5) are tested for
stic~iness using RCAT. Comparative Example 1 is a state-of-the-
art syndet bar similar to the exemplified bars of Small et al.,
supra.
TABLE 1
Rollin~ Cvlinder Adhesion (Stickiness) Test (RCAT~ Values
ExamD]e RCAT (%! Rel. RCAT*
1 56.5 l.0 **
2 32.8 0.58***
3 18.5 0.33
4 ~ 17.5+ 0.31
6 23.8 0.42
7 25.7 0.45
8 18.9 0.33
9 17.2+ 0.30
18.2+ 0.32
11 19.2 0.34
12 28.1 0.50
18.1 0.32
16 25.3 0.47
17 24.7 0.44
18 30.7 0.54
19 24.4 0.43
21 39.9 0.71
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w o 92tO7s31 PCTtUS9ltO7774
- 9 - 2~ 3~
TABLE 1 (Continued)
Rollinq CYlinder Adhesion (Stickiness) Test (RCAT) Values
Exam~le RCAT (%) Rel. RCAT*
23 34.0 0.60
26 39.3 0.70
; 27 28.0 0.~0
29 31.3 0.5
~0.0 0.71
- 31 29.8 0.53
32 16.0+ 0.28
33 23.~ 0.~2
3~ 20.0 0.35
4~ 26.0 0.~6
4~ 12.0+ 0.21
19.5 0.35
46 g.5+ 0.17
*RCAT/56.5.
**State-of-the-art syndet bar.
***VEL~ syndet bar.
+ Best bars of less stickiness.
The RCAT data is a measure of processability in that it
; correlates very well with stickiness during processing. Compa-
- rative Example 1 is difficult to process because the material
adheres to cooling, plodding and stamping equipment during manu-
facture. All formulas which have a relative RCAT value of less
than 1.0, therefore, are easier to process. Of Examples 3-46, for
which data are available, all have lower RCAT values and improved
processability.
The improved processability of these formulas is a direct
result of the decreased hygroscopicity of these formulas.
H~qroscooicitv Test lProcessability~
Hygroscopicity is the tendency for a product to take up water
under equilibrium conditions. It is a causative factor in the
stickiness of materials. ~he higher the hygroscopicity, the
stickier and more difficult to process a material tends to be.
Hygroscopicity is measured by shaving approximately one gram
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WO 92tO7931 PCI/US91/07774
209;5039 ~o
of a bar product and knowing the initial weight and moisture
accurately . The shavQd product i s plac~d in a constant tempera-
ture (80'F), constant humidity (80% R.H.) environment. The total
weight of the sampl2 is taken 'nourly until no further weight is
gained. T'ne diFferenc2 between ~ne initial and f;nal weights is
the inc, 23S3 in molsturo C3nCcilt of t,la ,ample; this value, ~hen
combined l,~ith the initial moisture, is the hygroscopicity.
In Table 2, ;;he E~3mples corres~pond to chose sho~:1n in Tabl,-~ 1
and are described in d~cail in Table 5 hereinbelow. The
experimental synde~ bar Evam~i?s i1l have impro~Jed hygroscopicity
over 'he standard b-r -x-mnl~
31.~ 7
Hv~rosc~lpic~ Yaluas
Exain~ Jaroscol~ i c i t~ 0) K~ /2 ~1~/9roscooi ci tv*
1 26.83 1.0
16 9.24 0.34
23 9.29 0.35
24 - 7.59 0.28
9.54 . 0.32
` 20 26 6.69 0.25
27 7.73 0.29
28 7.73 ~.29
29 8.12 0.30
8.42 0.31
31 9.28 0.35
32 7.40 0.28
33 8.~9 0.32
34 9.70 0.3
~Hygroscopicity/26.83 = Standard
In Vitro Skin Barrier Penetration Test (Mildness)
Th;s test was performed according to the procedure described
in U.S. Pat. No. 4,812,253, Small et al., issued Mar. 14, 1989,
said patent incorporated herein by reference.
Frequently, materials which tend to improve processability
also tend to have other negatives, particularly in terms of
product mildness. Referring to Table 3, using the barrier
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WO 92/07931 PCI/US91/07774
- 11 2~039
destruction method to assess product mildness, ;ndividual raw
materials sod1um c~tear~l sulfat~ is sho~iln to b2 surprisingly more
mild than the ultra mild sodium cocoglycerylether sulfonate, as
well as a silor-;;en chai-,led AS, sodium dod~cyl sulFate. The lower
5 the number in Table 3 t,le Inild~r the pnoduct.
_S 3
ma 3H~o TransDorted
'~,a ~n 0.137
Sod1llm Ce'3ar~/l Sul,ate 0.302
Sodinm r,^r.ogl~yreryl~r,h~r Su1,~nate 0.~58
Sùdl~l" ~
r~ 5
et!noa qr ;1a,l~i n~ Syndec 8ars
Cru-tchina
1. Add melted sodium cetearyl sulfat2 to the crutcher.
2. Add pr~determined quantity of Hamposyl L-30 solution to
the crucher mix.
3. Add the predetermined quantity of AGS paste to the water
in the crutcher. The AGS paste can be at ambient
temperature or preheated to 150-F (65-C).
4. Turn on the agitator and recirculation pump and maintain
temperature in crutcher at 130-150-F (54-6~-C) by
ad'usting steam and water valves.
5. Allow contents in crutcher mix to return to 130-I50~F
(54-65'C) prior to adding predetermined quantity of
staaric acid.
6. Add to heated crutcher mix pr2determined quantity of
soap or NaOH to form in-situ soap.
307. Allow the contcnts in the crutcher to mix and/or react
for about 15 minutes while maintaining the temperature
at 130-150-F (54-65'C).
8. ~dd to heat~d crutcher mix the predetermlned quantity of
acyl isethionat2. Allow contents in crutcher to mix for
h ~ 35about 20 minutes ~hile maintaining temperature at
- 130-150F (S~-65C).
9. Add sodium chloride plasticizer and titanium dioxide to
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W O 92/~7931 PCT/~S91/07774
~ 20~a39 -12 -
the heated crutsher mix.
10. Add lauric and/or coconut fatty acids to crutcher mix
and allow con~ents of crutcher to mix for abou-~ 1S
minutes while maintaining temperature at 130-150'F
(54-65C).
DrYinq
The crutcher mix is dried and cooled using a combination
flash chamber and chill roll or chill belt. Th2 crutc,ler mi~ is
first heated to approximately 300F (1~9C) by a heat e~han$~r
and then flash dried in a chamber abo~/e the chill roll Of c'1ill
belt. From th~ flash chamber ~h~ not, dried mix i, e~truded onto
the chill roll or chil1 bPlt. T'ne chill belt or chi11 roll
provides a uniform, thin, cool (~5-95'F, 29-35'C) product in flak2
or chip form. Typical moisture for the flake is 1-10%, preferably
about 2-4.5%. The ways to~ rPgulate the moisture, in thq order of
preference, 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 tne heat exchanger.
Amalgamating
The flakes are weighed and mixed in a batch amalgamator to
obtain uniform flake sizc. Preweighed perfume is added to the
flakes and mixed in the amalgamator to obtain the desired finished
product perfume level. The perfumed fl~kes are transferred to the
i 25 mix hopper or directly to the plodder.
Millinq ~Ontional)
The 3-roll soap mills are set up with the first roll at 120'F
(49C) and the other two mills at about ~4F (7-C). The material
is passed through the mills several times to provide a homogeneous
mixture of perfume and dried flakes.
Ploddinq and Stampinq
The plodder is set up with the barrel temperature at about
125F (52-C) and the nose temperature at 120F (49~C). 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.
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- 13 -2~9~039
EXAMPLES
The following examples are illustrative and ar2 not intended
to limit the scope of the invention(s). The deta;led methods of
making milled bars is well known. A11 levels and ranges, Lem-
peratur2s, results etc., used herein are approximations unl~ssother~ise speciried.
The formulations illustrated in Examples 1 and 2 ar~ compara-
tive examles included for illustration. 'xampl~ 1 is an A~S-
based, stata-of-the-art product, while E~ample Z is an ~stimated
formulation of Colgate-Palmoli~/e YEL~ syndet bar ~ jTh ~13.0~/~
sodium c~t?aryl sul,ata.
Examples 3-~9 contain rrom r~O ~, sodium cetearyl sul, -~e an(i
represent th~ broad range of tormulations accr~ptablrJ ~.li-thin rh~
; matrix of this invention. The sodium cetearyl sulfate contains
primary C16-C1g al~yl chains.
COMPARATIyE EXAMPLE_1
Comparative Example 1 is the control bar for assessing
processability of the bars of this invention. See Table 4. Using
this comparative example, it will be shown that bars described
below have improYed processability without sacrificing mildness or
other bar performance properties.
COMPARATIVE EXAMP~E 2
Comparative Example 2 is a standard syndet bar made by the
Colgate-P~lmolive Co. under the name Yel~. This product contains
an estimated 10% to lSYo sodium cetearyl sulfate, significantly
less than the levels required in the present invention. Addi-
tionally, the Vel bar has unacceptable bar use properties such as
smear and lather volume.
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W o 92/07931 PCT/US91/07774
2 ~ 3 9 - 14 -
TABLE_4
Com~arati~/e ~xam~les l_and 2
t.%)
Inqredient Ex 1 Ex. 2
Sodium Cocoglyceryletner
5uiron ~e ~3.7
. Sodium Lauroyl Sarcosinate 12.5
S~ Sv~p 7.2
Sodium Cocomonoglycor~l
Sul~tq - 40-~5
~o',ui~ C t ar~l 5ul,a~ - 10-15
~r~ c~,i,ol - 15.0
St_arlc Ac,d 9.8
Lauric Acid 6.5
Cncon~lt Oil
: Coconut Fatty Acid - 2.4
Sodium Chloride 4.0 10.9
Sodium Sulfate - 6.3
Polyquaternium-7 l.0
Polyquaternium-lO 0.5
Water 4.0 1.0
EXAMPLES 3-34
Examples 3-49 are all based on a matrix composed of sodium
cetearyl sulfate (26-46X) and stearic acid (0-20%). To this
matrix are added various la~hering surfactants such as sodium
lauroyl sarcosinate (0-20%~; sodium cocoglycerylether sul~onate
(0-3~%); sodium cocoyl ise~hionate (0-17%); and sodium soap
(0-15%). Lauric acid (0-20%) along with the stearic acid, are
added to ensure product pH less than or equal to 7.5. Processing
aids such as plasticizers (paraffin, cottonseed oil and PEG-8000),
and fillers, calcium carbonate and dextrins are added (0-15%) to
reduce stic!ciness and improve plodding.
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W~ 9~/07931 PCI-/US91/07774
~ 209~039
- 1 5 - : .;
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TABLE 5
~ E~. 4 Fx. 5 ~X. 6
: Inqredi~n~ t.%) (Wt.%) (Wt.%)(Wt.%)
Sodium Ce~earyl
: 5 Sul-fate 46.0 36.0 36.0 36.0
Sodium Lau,o~l
SarcosinatQ 15.0 15.0 15.0 15.0
d~,u~ g,~
eth2r Sul,o~.at. - - - 15.0
Sù~i Ui~ 3`/l
atniona.,..... 15.~ .O 17.3
Sodium o.~p - 10.0 7.~ 8.0
~: Scearic Acid 20.0 20.0 20.0 20.0
ater ~-0 4-0 ~-3 4.0
Total 100.0 100.0 100.0 100.0
.
. TABL_~ (Continuedj
::`
Ex. 7 Ex._8 Ex. 9Ex. 10
~; 20 In~redient (Wt.X)(Wt.%) (Wt.%)(Wt.%)
Sodium Cetearyl
Sulfate 38.0 38.0 36.2 36.0
. Sodium Lauroyl
Sarcosi~at2 12.5 15.0 12.1 11.9
25~ Sodium Cocoglyceryl-
ether Sulfonate 17.5 11.0 17.0 16.5
Sodium Soap 8.0 8.0 7.3 7.1
~ Stearic Acid 20.0 20.0 19.4 19.0
; : Sodium Chloride - 4.0 3.0 5.0~; 30 ~ Water ~ 4-0 4-0 5.0 5.0
` ; ~ Total 100.0 100.0 100.0 100.0
i ~ .
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WO 92tO7931 PCI/US91/07774
2 ~ 9 ~ 0 3 9 - 16 -
TABLE 5 (Continued)
Ex. ll Ex. I2 Ex. 13Ex. l4
In~redient (Wt.%) ('ilt.%) (',It.%)(',Jt.%)
Sodium Cetearyl
Sulfate 34.4 34.4 36.0 35.0
Sodium Lauroyl
Sarcosinate 11.5 11.5 15.0 15.0
Sodium Cocoglyc3ryl-
ether Sulfonate15.7 15.7 17.0 9.0
Sodium Cocoyl
Isethionat~ - - 3.0
Sodium Soap 6.9 6.9 ~.0 3 0
Stearic Acid 18.4 13.4 20.0 14.i3
Lauric Acid - - - 6.0
Sodium Chloride 8.0 8.0
Water 5.1 5.1 4.0 4.0
Total100.0 100.0 100.0100.0
TABLE 5 (Continued)
Ex. 15 Ex. 16 Ex. 17Ex. 18
Inaredient (Wt.%) (~t.7.) (Wt.%)(Wt.%)
Sodium Cetearyl
Sulfate 35.3 35,3 33.5 45.0
Sodium Lauroyl
Sarcosinate 15.0 lS.0 14.3 5.0
Sodium Cocoglyceryl-
ether Sulfonate 9.0 9.0 8.6 17.5
Sodium Cocoyl
Isethionate 9.0 9.0 8.6
Sodium Soap 7.5 7.5 7.1 7.5
Sodium Lauryl
Sulfate - - 5.0 5.0
Stearic Acid 14.0 14.0 13.3 16.0
Lauric Acid 6.0 6.0 5.7 4.0
Water 4.3 4-3 4.0 5.0
Total 100.0 100.0 100.0100.0
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W o 92/07931 2 ~ 9 ~ o 3 9 PCT/US91/07774
- 17 -
TABlE 5 (Continued)
Ex. 19 Ex. 20 Ex. 21 Ex. 22
~ Inaredient (Wt.%) (~,~t.%) (Wt.%) (~t.%)
: Sodium Cetearyl
Sulfate 40.0 40.0 45.0 4~.0
- Sodium Lauroyl
Sarcosinate 8.0 10.0 - -
Sodium Cocoglyc~ryl-
ether Sulfonate14.5 12.5 14.5 14.5
Sodium Soap 7.5 7.5 7-5 7 5
:~ Sodium Lauryl
Sulfate 5.0 5.0 3.0 8.0
~:~ St~aric Acid 13.0 13.0 18.0 1a.0
Lauric Acid 2.0 2.0 2.0 2.0
~; 15 Water 5.0 5.0 5.0 5-0
Total100.0 100.0 100.0 100.0
,
TABLE 5 (Continued)
Ex. 23 Ex. 24 Ex ~5 Ex. 26
Inqredient (Wt.%) -(Wt.%) (Wt.%) ~Wt.%)
, Sodium Cetearyl
Sulfate 26.3 32.0 32.0 26.3
. Sodium Lauroyl
Sarcosinate 15.0 13.8 13.8 15.0
. Sodium Cocoglyceryl-
~; ether Sulfonate 9.0 8.3 8.3 18.0
Sodium Cocoyl
Isethionate 9-.0 8.3 8.3
Sodium Soap 7.5 6.9 6.9 7.5
: : : Stearic Acid 14.0 12.9 12.9 14.0
Lauric Acid 4.0 5.5 5.5 4.0
Paraffin 10.0 - - 10.0
: Calcium Carbonate - 7.5 - -
Dextrin - - 7.5
Water 5.3 4.8 4.8 5.2
Total 100.0 100.0 100.0 100.0
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w o 92~07931 pcr/us91/o7774
~9~39 - 18 -
TABlE ~ (Continued~
EY 27 Ex. 28 Ex. Z9Ex. 30
Inaredient (~,~t.%) (Wt.%) (Wt.%)(Wt.%)
Sodium Cetearyl
Sul,at~ ~o.3 36.3 34.3 45.0
Sodiun1l~uroyl
Sarcosinate 15.0 lO.O 7.0 6.5
Sodium Cocoglyc~ryl-
P~her SulFonate 18.0 18.0 18.0 28.5
Sqdium Soap 7.5 7.5 . 7.5
Stearic ~cid 11.0 1~.0 1~.0
L~ur~ic ~C,tl :~.O ~.O ~ O
~ar3,r1n - i.O - 15.0
PEG-~OCu lO.O - lO.C
Wat~r 5.2 5.2 5.2 5.2
Total 100.0 100.0 100.0100.0
~e~L~_~ (Continued)
~ Ex. 3~ Ex. 33Ex. 34
~: Inaredient (Wt .~o) ~Wt .X~ (Wt.%)(Wt.%~
Sodium Cetearyl
Sulfate 45.0 40.0 30.5 37.5
Sod,um Lauroyl
Sarcosinate 10.0 12.5 12.0 10.0
Sodium Cocoglyceryl-
;~: ether Sulronate 28.5 27.5 16.0 25.0
Sodium Soap - - 7.5
` Stearic Acid - - 13.0
Lauric Acid - - 6.0
~` Paraffin 11.5
~.~ Calcium Carbonate - - - 7.5
- ~ ~ PEG-8000 - - 15.0 10.0 15.0
,: ~ Water 5.0 5.0 5.0 5.0
Total 100.0 100.0 109.0 100.0
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WO 92/07931 PCI'/US91/07774
1929~039
TABLE 5 (COnt;nUed)
~X. 35 EX. 36 EX. 37EX. 38
Inaredi2nt (Wt.%) (Wt.%) (W~.%)(Wt.%)
Sodium Cet aryl
SU1Tate 30.5 30.5 33.5 32.8
Sodium Lauroyl
Sarcosinate 12.0 12.0 6.0 7.5
Scdium Cocoglyce,yl-
ether Sul;onate16.0 16.0 19.0 18.3
Sodium Soa~ 7.55 7.5 7.5 7.5
Sbea,Aic ~cld ~.3 9.5 6.0 ~.0
~u~ 'ci~ 13.0 9.~ 13.0 13.0
Ot~û 10.~ 10.0 10.0 10.0
: I.J~tPr 5.0 5.0 5.0 5.0
TotallOO.O 100.0 100.0100.0
~: .
. TABlE 5 (Continued)
Ex. 39 Ex, 40 Ex. 41 Ex. 42
Inqredient (Wt.%) (Wt.%) (Wt.%) (Wt.%~ -
Sodium Cetearyl
Sulfate 32.0 30.5 20.0 30.0
Sod;um Lauroyl
Sarcosinate 9.0 12.0 12.0 7.2
25 , Sodium Cocoglyceryl-
' ether Sulfonate17.5 16.0 11.0 33.0
: Sodium Soap 7.5 : 7.5 12.0 4.3
Stsaric AC;d . 6.0 6.0 12.0 5.9
~ Lauric Acid 13.0 13.0 18.0 3.9
; 30 Paraffin - ~ 10.0 ~ - -
PEG-8000 10.0 - 10.0 10.0
: Water ~ 5.0 5-0 5-0 5-0
Total100.0 100.0 100.0 100.0
.~ .
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WO 92/07931 PCI-/US91/07774
- 20 -
2095039 ~ (Continued)
Ex. 43E~. 44 E~. 45 E~
Inaredient (1,~t.%)(!~t.~o)('iJt.%) (',~t.
Sodium Cetearyl
Sulfate 30.0 25~0 32.0 30.0
: ~ Sodium Lauroyl
Sarcosinate 14.0 14.0 14.0 14.0
Sodiu~ Cocoglycaryl-
ether Sulfonate 7.0 7.0 7.0 7.0
Sodium Soap 10.0 10.0 ln ~ 10.0
Stearic Acid 20.0 ^C.3 20.0 5.0
Lauric Acid i.0 5.0 ~.0 2i.3.0
Calci~m Carbonate - 5.0 5.~ -
PEG-8000 10.0 10.0 lO.0 10.0
Water 5.0 5.0 5.0 5-0
Total 100.0100.0 100.0 100.0
,, .
: TABLE 5 (Continued)
Ex. 47 Ex. 48 Ex. 49
Inqredient (Wt-%) ` (Wt.%3 (Wt.
Sodium Cetearyl
Sulfate 25.0 28.1 29.5
` ~ Sodium Lauroyl
; Sarcosinate 13.0 11.1 la.0
:~ 25 Sodium Cocoglyceryl-
ether Sulfonate 16.0 1~.7 7.0
Sodium Soap 10.0 5.9 10.0
; Stearic Acid 20.0 12.0 20.0
:; Lauric Acid 5.0 5.5 5.0
^Calcium Carbonate - 7.5
~` PEG-8000 7.0 9.2 10.0
:~ JR-400 0.5
Water 5.0 5 0 5 0
.~
~' ~ Total 100.0 100.0 100.0
` E~amples 33, 43 and 49 are highly preferred syndet bars which
are easy to process while still ?erforming ~ell in terms of bar
properties.
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