CA2095039A1 - Syndet bar with long chain alkyl sulfates for improved processability and bar characteristics - Google Patents

Syndet bar with long chain alkyl sulfates for improved processability and bar characteristics

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Publication number
CA2095039A1
CA2095039A1 CA002095039A CA2095039A CA2095039A1 CA 2095039 A1 CA2095039 A1 CA 2095039A1 CA 002095039 A CA002095039 A CA 002095039A CA 2095039 A CA2095039 A CA 2095039A CA 2095039 A1 CA2095039 A1 CA 2095039A1
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CA
Canada
Prior art keywords
bar
syndet
sodium
long chain
syndet bar
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
CA002095039A
Other languages
French (fr)
Inventor
James R. Schwartz
Wayne E. Eccard
Theresa A. Bakken
Lawrence A. Gilbert
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Procter and Gamble Co
Original Assignee
Individual
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Filing date
Publication date
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Publication of CA2095039A1 publication Critical patent/CA2095039A1/en
Abandoned legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D10/00Compositions of detergents, not provided for by one single preceding group
    • C11D10/04Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap
    • C11D10/042Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap based on anionic surface-active compounds and soap
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047Detergents in the form of bars or tablets
    • C11D17/006Detergents in the form of bars or tablets containing mainly surfactants, but no builders, e.g. syndet bar
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/04Carboxylic acids or salts thereof
    • C11D1/10Amino carboxylic acids; Imino carboxylic acids; Fatty acid condensates thereof
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/126Acylisethionates
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/16Sulfonic acids or sulfuric acid esters; Salts thereof derived from divalent or polyvalent alcohols

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Detergent Compositions (AREA)
  • Cosmetics (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Steroid Compounds (AREA)
  • Bakery Products And Manufacturing Methods Therefor (AREA)
  • Moulds For Moulding Plastics Or The Like (AREA)

Abstract

This invention is an improved mild personal cleansing syndet bar comprising: long chain alkyl sulfate having essentially saturated C15-C22, preferably C16-C18, alkyl chains, more preferably cetearyl sulfate, combined with a selected plasticizer.

Description

:

209~039 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 .
.

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.
, .
~; 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.

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 ' 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 . , .
~ . .

- 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.
:

, `',, ~ ' ' ~: ;

W ~ 92/07931 PCT/US91/07714 - 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 3-49 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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~ 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 ;:
.

:
-~: , W o 92/07931 2 ~ 9 ~ o 3 9 PCT/US91/07774 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 ~' , .

, ~ -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 .~ .

~:
.

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.

. ' "

.

Claims (9)

Claims
1. A personal cleansing syndet bar comprising: from about 18% to about 55% of essentially saturated long chain C15-C22 alkyl sulfate;
from 0% to about 20% of soap; and from about 10% to about 50% of a plastic binder selected from the group consisting of: paraffin waxes, fatty acids, wherein said plastic binder has a melting point of from about 23°C to about 110°C; wherein said plastic binder is selectedfrom the group consisting of paraffin, nonionic surfactants, fatty acid, fatty alcohols, and polyethylene glycols, and mixtures thereof;
and wherein said syndet bar has a pH of from about 4.0 to about 8.5.
2. A personal cleansing syndet bar according to Claim 1 wherein said plastic binder is selected from the group consisting of: paraffin waxes and fatty acids.
3. The syndet bar of Claim 1 or 2 wherein the level of long chain alkyl sulfate is from about 20% to about 45% by weight of said bar and said soap is from about 5% to about 15% by weight of said bar; and wherein said plastic binder melting point is from about 30°C to about 100°C and wherein said long chain is C16-C18.
4. The personal cleansing syndet bar of Claim 1 or 2 wherein said bar primarily comprising: from about 15% to about 40% of said plastic binder; and wherein said long chain alkyl sulfate is present at a level of from about 20% to about 40% and is a saturated long chain alkyl sulfate surfactant saturated alkyl chains of from about 16 to about 18 carbon atoms; and from about 15% to about 40% of a mild cosurfactant.
5. The syndet bar of Claim 4 wherein said mild cosurfactant selected from the group consisting of higher lathering sodium lauroyl sarcosinate, alkyl glycerylether sulfonate, sodium cocoyl isethionate, stearoyl isethionate, and mixtures thereof, and from about 2.0% to about 10% water and wherein said syndet bar is a milled bar and has a pH of from about 5 to about 8.
6. The syndet bar of Claim 1 or 2 wherein said soap-synthetic bar contains other components selected from: moisturizers, colorants, solvents, fillers, other surfactants, polymeric skin feel and mildness aids, perfumes, and preservatives, and water at a level of from about 3% to about 8% wherein said bar contains said C16 and C18 alkyl chains having a ratio of from about 4:1 to about 1:4.
7. The syndet bar of Claim 3 wherein said long chain alkyl sulfate is at least 90% C15 and C18.
8. The personal cleansing syndet bar of Claim 4 wherein said mild cosurfactant is selected from the group consisting of sodium lauroyl sarcosinate, alkyl glycerylether sulfonate, sodium cocoyl isethionate, stearoyl isethionate, and mixtures thereof, and is from about 2.0% to about 10% water; and wherein said syndet bar is a milled bar and said pH is from about 5 to about 8; and wherein said bar contains said C16 and C18 alkyl chains having a ratio of from about 4:1 to about 1:4 and contains from about 15% to about 40% of a mixture of free fatty acids and paraffin at a ratio of from about 3:1 to about 1:1.
9. The syndet bar of Claim 3 wherein said plastic binder is a mixture of free fatty acid and polyethylene glycol at a ratio of from about 3:1 to about 1:1.
CA002095039A 1990-10-30 1991-10-21 Syndet bar with long chain alkyl sulfates for improved processability and bar characteristics Abandoned CA2095039A1 (en)

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US6326339B1 (en) * 1997-03-04 2001-12-04 Lever Brothers Company, Division Of Conopco, Inc. Cleansing system comprising synthetic detergent bar and pouf
BRPI0608628A2 (en) * 2005-03-18 2010-11-30 3M Innovative Properties Co solid cleaner for heated surfaces, method of cleaning a heated surface, and cleaning article
US20070066500A1 (en) * 2005-09-21 2007-03-22 Conopco, Inc., D/B/A Unilever Composition with enhanced squeaky feel
JP2022532073A (en) 2019-05-07 2022-07-13 ビーエーエスエフ ソシエタス・ヨーロピア Aqueous surfactant composition and bar soap
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EP0239165A3 (en) * 1986-03-27 1988-03-23 Cornelis Van Buuren Synthetic soap and method for the preparation thereof
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