CA1102204A - Bar soap and process of manufacture - Google Patents
Bar soap and process of manufactureInfo
- Publication number
- CA1102204A CA1102204A CA307,323A CA307323A CA1102204A CA 1102204 A CA1102204 A CA 1102204A CA 307323 A CA307323 A CA 307323A CA 1102204 A CA1102204 A CA 1102204A
- Authority
- CA
- Canada
- Prior art keywords
- soap
- fatty acids
- poly
- ethylene oxide
- blend
- 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.)
- Expired
Links
- 239000000344 soap Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 title claims description 3
- -1 poly(ethylene oxide) Polymers 0.000 claims abstract description 32
- 239000000194 fatty acid Substances 0.000 claims abstract description 25
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 24
- 229930195729 fatty acid Natural products 0.000 claims abstract description 24
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 24
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims description 44
- 239000002253 acid Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 150000007513 acids Chemical class 0.000 claims description 14
- 239000011734 sodium Substances 0.000 claims description 12
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 11
- 229910052708 sodium Inorganic materials 0.000 claims description 11
- 125000004432 carbon atom Chemical group C* 0.000 claims description 10
- 239000003599 detergent Substances 0.000 claims description 5
- 239000003760 tallow Substances 0.000 claims description 5
- 235000019864 coconut oil Nutrition 0.000 claims description 4
- 239000003240 coconut oil Substances 0.000 claims description 4
- 239000000155 melt Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000007493 shaping process Methods 0.000 claims description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 7
- 235000021355 Stearic acid Nutrition 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000003801 milling Methods 0.000 description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000008117 stearic acid Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000004166 Lanolin Substances 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000007792 addition Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 235000011187 glycerol Nutrition 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 229940039717 lanolin Drugs 0.000 description 3
- 235000019388 lanolin Nutrition 0.000 description 3
- 239000002304 perfume Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 239000003925 fat Substances 0.000 description 2
- 235000019197 fats Nutrition 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- IWDCLRJOBJJRNH-UHFFFAOYSA-N p-cresol Chemical compound CC1=CC=C(O)C=C1 IWDCLRJOBJJRNH-UHFFFAOYSA-N 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000271 synthetic detergent Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 102000011632 Caseins Human genes 0.000 description 1
- 108010076119 Caseins Proteins 0.000 description 1
- 241000905957 Channa melasoma Species 0.000 description 1
- 241000518994 Conta Species 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229910008046 SnC14 Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000005267 amalgamation Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002844 continuous effect Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 235000021588 free fatty acids Nutrition 0.000 description 1
- 230000002070 germicidal effect Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 239000003605 opacifier Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 229940080237 sodium caseinate Drugs 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0084—Antioxidants; Free-radical scavengers
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D9/00—Compositions of detergents based essentially on soap
- C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
- C11D9/22—Organic compounds, e.g. vitamins
- C11D9/225—Polymers
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D9/00—Compositions of detergents based essentially on soap
- C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
- C11D9/22—Organic compounds, e.g. vitamins
- C11D9/26—Organic compounds, e.g. vitamins containing oxygen
- C11D9/267—Organic compounds, e.g. vitamins containing oxygen containing free fatty acids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D9/00—Compositions of detergents based essentially on soap
- C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
- C11D9/48—Superfatting agents
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Detergent Compositions (AREA)
Abstract
ABSTRACT
Toilet soap bars superfatted with higher fatty acids and containing high molecular weight poly(ethylene oxide), and method of preparing same.
Toilet soap bars superfatted with higher fatty acids and containing high molecular weight poly(ethylene oxide), and method of preparing same.
Description
Superfatted toilet soap bars (such as those sold as cosmetic or complexion bars) are well known in the art and are described, for instance, in the United states patent to Megson et al 3,576,749. AS pointed out in the Megson patent, such bars are unlike bars made of synthetic deteryents which, according to that patent, give a very soft, slimy, messy type of smear . . . which is unacceptable in soap bars. According to the Megson patent free fatty acids in the bar improve the volume and quality of the lather, causing it to be more stable with small air bubbles which gives the user a lather which is characterized as "richer" and creamier, and the fa~ty acids also tend to soften the skin. The Megson patent teaches -that with such superfatted bars relatively large amounts of sodium chloride and relatively high milling te~peratures are required in order to attain firmness of the bar and smear resistance.
The superfatted toilet soap bars of the present inven-tion are substantially and preferably entirely devoid of synthetic detergents, form a rich creamy lather and give an e~tremely pleasant feel both in use and after use. When com-pared to commercial superfatted toilet soap bars which arebelieved to be made according to the teachings of Megson it is found that the novel bars of this invention are greatly pre-ferred ~y users, with respect to the nature of the lather and other characteristics~ The bars are firm and have high resist-ance to sloughing ox smear without the need for incorporation of added sodium chloride and without the need for using high milling temperatures.
In accordance with the present invention, there is provided a toilet soap bar consisting essentiall~ of sodium soap of higher fatty acids having about 8 to 20 carbon atoms as B
. .
substantially the sole detergent, about 6 to 12% of superfat~ing higher fatty acids having about 8 to 20 carbon atoms, about 1 to 4% poly~ethylene oxide) having a molecular weight in the range of about 100,000 to 5~000,000 and about 5 to 18% water.
In another aspect, the invention provides a process for preparing a toilet bar soap consisting essentially of sodium soap of higher fatty acids having about 8 to 20 carbon atoms as substantially the sole detergent, about 6 to 12% of super~atting higher fat~y acids having about 8 to 20 carbon atoms~
about 1 to 4% poly(ethylene oxide) having a molecular weight in the range of about 100,000 to 5,000,000,(~and about 5 to 18% water which process comprises mixing neat soap containing said sodium soap and about 30% moisture with a blend of said poly~ethylene oxide) in a melt of said superfatting higher fatty acids, subjecting the resulting mixture to drying conditions, and thereafter shaping the mixture into a bar.
~ la -.
, . . .
According to one a5pect of thls invention~ the super-fatted soap bars contaln an amount of free higher fatty acid in thP range of about 6 to 12~, such as about 8 to 10~, ~ogether with a high molecular weight poly(ethylene oxid~) in an amount of at least abou~ 0,5~ typically about 1 to 4~
preferably about 1~ to 2 ~ or 3~ has also been ~ound that poly(ethylene oxide)-containing super~atted bars which have particularly good slough - or smear - resistant properties -comprise a sod~um soap of about equal proportions of coco ~atty acids and tallow fatty acids super~atted with about equal amounts o~ coco ~atty acids and s~earic acidg as can be seen, for instance~ in the data tabulated ln Example 1 below.
Soap is conventionally manufactured py the ~aponi~i-cation o~ ~atty acids or esters (e,g. fats and oils) by either a "kettle" process or a continuous ~aponification technique~
- as di~cussed in Encyclopedia o~ Chemical Tech~ology (2nd edition) Vol. 18 pages 415-425, which states that "the end product of both the kettle and continuous saponification procedures is a neat soap containing approx~mately 30% water The 30~ w~ter content o~ neat soap must be reduced to 10-15 before shaping lnto bars..~"
Soap bars have b~en made commercially by adding powdered poly(ethylene oxide) to soap chips in a soap amalga-mator; such addition requires speclal precautions in order to a~oid ~ormation of specks in the final bar. ~ne use o~ high molecular weight poly(ethylene oxide) ("Polyox*resin") in synthetic detergent bars, which may contain some ~oap, ha8 been de~cr~bed and it h~ been suggeste~ that 1~the re~n may *Trade Mark
The superfatted toilet soap bars of the present inven-tion are substantially and preferably entirely devoid of synthetic detergents, form a rich creamy lather and give an e~tremely pleasant feel both in use and after use. When com-pared to commercial superfatted toilet soap bars which arebelieved to be made according to the teachings of Megson it is found that the novel bars of this invention are greatly pre-ferred ~y users, with respect to the nature of the lather and other characteristics~ The bars are firm and have high resist-ance to sloughing ox smear without the need for incorporation of added sodium chloride and without the need for using high milling temperatures.
In accordance with the present invention, there is provided a toilet soap bar consisting essentiall~ of sodium soap of higher fatty acids having about 8 to 20 carbon atoms as B
. .
substantially the sole detergent, about 6 to 12% of superfat~ing higher fatty acids having about 8 to 20 carbon atoms, about 1 to 4% poly~ethylene oxide) having a molecular weight in the range of about 100,000 to 5~000,000 and about 5 to 18% water.
In another aspect, the invention provides a process for preparing a toilet bar soap consisting essentially of sodium soap of higher fatty acids having about 8 to 20 carbon atoms as substantially the sole detergent, about 6 to 12% of super~atting higher fat~y acids having about 8 to 20 carbon atoms~
about 1 to 4% poly(ethylene oxide) having a molecular weight in the range of about 100,000 to 5,000,000,(~and about 5 to 18% water which process comprises mixing neat soap containing said sodium soap and about 30% moisture with a blend of said poly~ethylene oxide) in a melt of said superfatting higher fatty acids, subjecting the resulting mixture to drying conditions, and thereafter shaping the mixture into a bar.
~ la -.
, . . .
According to one a5pect of thls invention~ the super-fatted soap bars contaln an amount of free higher fatty acid in thP range of about 6 to 12~, such as about 8 to 10~, ~ogether with a high molecular weight poly(ethylene oxid~) in an amount of at least abou~ 0,5~ typically about 1 to 4~
preferably about 1~ to 2 ~ or 3~ has also been ~ound that poly(ethylene oxide)-containing super~atted bars which have particularly good slough - or smear - resistant properties -comprise a sod~um soap of about equal proportions of coco ~atty acids and tallow fatty acids super~atted with about equal amounts o~ coco ~atty acids and s~earic acidg as can be seen, for instance~ in the data tabulated ln Example 1 below.
Soap is conventionally manufactured py the ~aponi~i-cation o~ ~atty acids or esters (e,g. fats and oils) by either a "kettle" process or a continuous ~aponification technique~
- as di~cussed in Encyclopedia o~ Chemical Tech~ology (2nd edition) Vol. 18 pages 415-425, which states that "the end product of both the kettle and continuous saponification procedures is a neat soap containing approx~mately 30% water The 30~ w~ter content o~ neat soap must be reduced to 10-15 before shaping lnto bars..~"
Soap bars have b~en made commercially by adding powdered poly(ethylene oxide) to soap chips in a soap amalga-mator; such addition requires speclal precautions in order to a~oid ~ormation of specks in the final bar. ~ne use o~ high molecular weight poly(ethylene oxide) ("Polyox*resin") in synthetic detergent bars, which may contain some ~oap, ha8 been de~cr~bed and it h~ been suggeste~ that 1~the re~n may *Trade Mark
-2-Z~
be melted in combination with soap, detergent base, or other ingredients and then other material incorporated into the melt" (Davidson and Sittig "Water Soluble Resins" pub. 1962, pages 197-8). When it was attempted to incorporate about 2% powdered poly(ethylenezoxide)into a neat soap con~alning about 30% water ("kettle soap"), a mixture was obtained which was lumpy and poorly dispersed and not pumpable.
According to another aspect o$ this invention, it has been found that a superior blend is obtained by incorporat-ing the poly~ethylene oxide), desirably in powder form, into a melt of all, or a portion of, the higher fatty acids which are to be used for super~atting the soap. Best results are obtained when this blend also contains a minor amount of water. As will be seen in Example 3 below, the presence of the water has a marked effect on the nature of the blend of atty acid and high molecular weight poly(ethylene oxide~, significantly decreasing its viscosity; the presence of the water also tends to opacify the blend which may indicate that a water-in-oil type of dis-persion is formed. The water-containing blend can be pumped 2Q readily; its viscosity is well below the upper viscosity limit (which is about 7,0QO or 8,QOO centipoises~ of materials that can be handled readily by ordinary reciprocating pumps. It can thus be easily pumped into admixture with the kettle soap.
The poly~ethylene oxide)~containing soap bars made by this procedure have outstanding properties; they lather well, have an especially pleasant feel during and after use, have good slough resistance and resistance to wet-cracking.
. - , The use o~ thi~ invention make~ ik possible to produce toilet ~oap bars which give a rich and creamy9 but only moderately slippery, lather and which are fi~m and resis~;ant to sloughing and cracking in use.
The following Exampl~s ar~ given to illustrate this invention ~urther. In this application all amounts and proportions are by weight unles~ otherwise s~pecified.
EXA~IE 1 ___ (a) 4.5 parts o~ stearic a~d 4.5 parts coco ~atty acid~ ~re melted together at a temperature o~ 80C 1 n a ve~sel equipped wi~h a stirrer. 1.8 parts o~ hlgh molecular weigh~ poly(ethylene oxide) ("Polyox WRS N~750" sold by Union Carbideg haYing a molecular weight of about 3003000 a viscosity /~hen mea~ured on a 5~ 801ution in water7 o~
about 550 to 900 rps at 25C~ and a melting point in the neighborhood of 65C) are added thereto with stirring while maint~ining the blend at about 80C9 This blend is th~n mixed with a kettle soap (at 70C) in such proport~ons that the resulting mixture contains about 75 parts of the ~odium soap (expressed as anhydrous soap), 4.5 parts o~ the added stearic acid, 4?5 parts o~ the added coco fatty acids and 1.8 parts of the poly(ethylene oxide). The k~ttle soap is made by ~aponi~ying a.50~50 mixture of coconut oil and tallow w~th sodium hydrox~d~ solution, extraction o~ resultant glycerine~
~Iwash~ngi~ w~th electrolyte solution ~nd removal o~ high e}ectrolyt.e nigre 50ap layer all as i~ conventlonal in the manu~acture Or kettle ~oaps; it contain~ about 27~32~ (e~g.
. 30%) wate.r, up to about 1% (e.g. 0.5~) glycerol, up to about .
~z~
0.3% (e.g. 0.1%) NaOH, up to about 1% (e.g. 0.7%) ~aCl. The ingredients are stirred together for a few minutes and the mixture is then formed into dried soap chips containing about 10% moistureJ as by pumping the hot soap mixture onto a chilled roll, forming a thin film on the roll, slicing the film into chips or ribbons and then drying the chips or ribbons.
The chips are then blended with color and perfume (e.g. 0.7%
TiO2 and 1.5% perfume~ in conventional manner in a soap amalgamator at about room temperature, then milled to homo-genize them (e.g. at a temperature of about 15 to 35C), then extruded into a bar form hy means of a con~entional soap plodder (e.g. at a temperature of a~out 20-50C, e.g. ~0C), then cut into cakes; the surfaces of the cakes are cooled and the cakes are pressed into the desired shapes (e.g.
in a pin-die press~.
(hl Part (a) is repeated except that instead of using 4.5 parts stearic ac-,d and 4.5 parts coco fatty aci~ds there is employed 9 parts stearic acid.
(c~ Part (a~ is repeated except that instead of using 4.5 parts stearic acid and ~.5 parts coco fatty acids there is employed 9 parts coco fatty acids.
On testing the soap ~ars ~after aging at least 3 days~ the following results are obtained;
. ~ :
-Sponge Sloue~h 9~ Eroslon Lather (17 hY~ Hydration Cracklng NoO o~ S~ loss (2 hr. ) Index ~troke~ S~ galn ..... ...
(a) 60 1.5 2.6 16.1 12.5 18 (b) 80 3~5 2~2 18,8 11,6 15 (C) 68 5~2 18.7 19.6 10.~ 0 In the sponge lather tesk, which mea6ure8 the quickne86 o~
lather ~ormation~ ~he bar's ~lat sur~ace is alternatel9 rubbed against a sponge and dipped in a pan o~ water (with a hardne~ level o~ 125 ppm and a t~m3p~rature of` 95C3F~)o The up and-down motion of the lather machine produces the number o~ strokes it requires to ~o~m a continuou~ rlng of foam in the pan. me le6s the number of strokes, the quic~er 15 the lather. In the slough t~t, the bar~ are pl~ced ~lat with one side immer~ed in a Petri di~h for sevellksen hours,.
a~ter which time the so~t, muæh~ so~ i~ removed by finger~.
The percent weight 108t aæ slough ls reported. In the er*sion test the bar is inmer~ed in water ~or 260 trokes 20 (about 10 minutes~ of ~he la~h~r machine, a~d the a~nount o~
soap 108~ iS meaæured~, In the h~rdration test the bar~ are con~pletely immers~d in t~p wat~r ~or ~wo hour~ and the in-creas~ in welght is dekerr~inedl, The cracking index i~ an evaluation based on number ana ~everi~y o~ cracks ln a test 25 in which the bars are shaved on one side ts~ hal~ their orlginal ~ize~ then placed under tap water (about 100 ppm hardness) for one h~r, taken out and hung to dry in air until no sign o~ ~ree water remain~ or~ their sur~aces (usually overnight) .
2~4 The bar of part (a) shows unexpectedly high lather quic~ness3 unexpeckedly low slough loss and erosion loæs and quite acceptable cracklng behavior"
EXA~LE 2 _ Bars are made as in Example l(a) except that they alRo contain 0.5% lanolin with and without 0~5% sodium ca~einate solids3 ~hese ingredlents being incorporated with the hot ~atty acid-poly(e~hylene oxide) blend bePore mixing it with the kettle soap.
ExaD~le l(a) is repeated exc~pt that the ~ollowing procedure is employed in making the blend mixed with the kettle soap~ 5 parts o~ commercial stearic acid (m.pO 54C. ) and 5 parts of coco ~atty acids (m.p. 25C, iodine valu~ 6 are mel~ed tog~ther at a temperatur~ o:~ about 102C. One part o~ powder~d hiKh molecular weight poly(ethylerle oxid~
~"Polyox WSR N~750" m.p. about 65~C) i~ added thereto with stirring. The viscosity of the mixture at ~ 02C ls about 750 cps, at 88C it is about 4,000 cps and at 54C it ls about 5,000 cpæ~ (as determined with a Brook~i~ld vi~cosimet~r3 .
One more part of the ~ame Polyox ls then added with stirring. The viscosity of the mlxture 1~ about 18,000 cps at 94e" about 19 ,000 cps at 88C, about 33,500 cps at 66C and about 42,500 cps at 54C~
Then 0.5 part o~ lanolin i~ added with ætirring. ~na resulting blend n~w has a viscosity o~ about 15,000 Cp8 at 94C. and a similar viscc~sity at 70~C.
~7~
z~
Next 1 part o~ water i~ add~d. As a result~ th~ ~orm~r~
ly clear blend becomes cloudy or opaque. Its vl~co~lty i~
about 59000 cps at 77C, about 4,000 cps at 71~C and about 39250 cps Q~ 50 to 63co Ther~aft~r an additional 1 part o~ water is added with stirring~ The re~ulting blend ha~ a vi~co~ity of ~bout 2g250 eps a~ 84C~ 1,500 cp~ at 8~C, 930 cpæ at 71C~ 470 cp~ at 57C, 234 cpS at ~O~C and 114 cps ak 52C, ~ext 2.5 part~ of a solution of ~odium ca~einate (containing 20~ ca~ein) i~ added. The resulting blend is white. Its vi~cos~ty i~ about 23900 Cp8 at 81C9 2,520 cpæ
at 71C, 1,700 cps at 66C and 1,800 cp~ at 60C.
It will be seen that the addltion o~ the water give8 a blend who~e viscosity at, ~a~, 70C is gre~tly decrea~d (e.g. to well below hal~ lt~ valu~ be~ore the additlon of the water)0 Also the blend~ conta~ning water sho~ a r~-markable decrease in visc081ty with decr~ase in temperature (e.g. when temperature ~s reduced~ :erom 7o cr 80 ~, by 10C the viscosity drops by well ov~r 10%). Th~ above re-~ulting blend i~ pu~ed at a temp~ature o~ about 60 85~C
into a mixlng vessel containine kettle 80ap (at 70C) $n such proportions that the resulting m~xture ~ontalrl~ about 75 par*s o~ the ~odiwn soap (e~re~d a~ anhydrous soap), 4.5 part~ o~ the added ætearlc acld, 4.5 ps,rt~ o~ the add~d coco :~atty acids and 1~8 part~ o~ the poly(ethyl0ne oxide)~
~L~5 4 Exan~ple l(a) i~ repeated excep~ that in making ~a~d re~ult~ng blend, 10 par~s o~ ~tearlc ac~d are melt~d and 2 parks of the po.ly(o~hyl~n~ oxld~ of` ~ 1 are added 5 thereto3 followed by 1.5 par~s of wat~r3 while the mixture i8 stirred and maintained at abc>ut 70-90C.
EXAMP,IE 5 Eicample 4 ia r&p~a~ed excep~ that coco ~a~ty acid~
are u~ed in plac~ o~ ~tearic acid~
In the water-contairaine blerad o~ poly(e~hylen~ o~
and h~g~er ~atty ac~as ther~ ~Lre pre~erably abou~ 2 to 20 (more preferably about 4 to 8) part~ of~ the ~a~y acid~ p~r part of poly(ethyIene oxide~ and about 0,,5 lto 5 ~ore pre~
~srably about 1 to 2) part~ of water p~r part o~ poly~ethyl~ne oxide ) .
Xt i~ preferred thæt the amo~t o~ ~aol8tur~ in the in6redi2nt~ adde~ ~o ~he ~attle ~oap be stach that ~h~
mo~sture: 80ap rati o be mainta~ned belo~ about 33~ 67 ~ ~uch a~
about 27:73 to 32:68) to minimize ~o~ation of les~ deæ~r~bl~
ge~ 80~lp pha~e,.
It is desir~ble9 partlcularly in the formulation~
containing relatitrely large amount~ o~ coco ~atty acid~ t ~uch as la) to dry to a mo~sture content below about 18%9 pre-ferably to from a~out 5% to 12%, in order to reduce the tendarlcy for s~ickines~ during la~er blanding (e.g. in the amaIg~mator~ or proc~ingc To the ~ame end it ~ de~irable to use relat:Lvely low pludding te~ratures, pre-cool and pre-dry the outer ~ur~ac~ o~ ~he bar~ be~ox~ pr~s~lng in kh~
die~g and lubrlc~te the die~ (e.eO with ~ aqueous 801utlon conts.inlrlg 16% NaCl ~d 25% ~lycerolj wh~ch i8 then alr-blown off the 8urface~ of' the preæsed b~rs).
. .
~g~ ~
The high molecular weight poly(ethylene oxide) has an average molecular weight of at least about 100,000~
amples OI such compounds are tho~e sold by Union Carbide CompAny under the trademark "Polyox"O These polymer~ are 5 nonionic materials soluble in water, and their molecular w~ights range ~rom about 100~000 to about 5,000~000 or more.
It i8 preferred to employ polymers ~aYing average molecular welghts below 1,000~000, more pref`erably not above about 600,000 such as about 300,000 to 400,,000. For the material having an average molecular weight of about 300,000 a proportion in the neighborhood o~ 2% has glven excelleAt result~. Thiæ
300,000 molecular weight material (sold as Polyo~ WSR ~-750) ha~ a viscos:Lty at 25Co, for a 2~ aqueous solution, o~ about 40 centipoises (Brookfield Splndle No. 1 at 10 rpm): ~or a 5% solution thiæ viscosity is abou~ 600 - 1000 centlpoi~e~
Use of say 2~ o~ extremel~ high molecular weight poly(ethylene oxid~)3 e.g. o~ 4,000,000 average molecular weight~ cause~ the lather to be pituitou~ which is les8 de~irable. According to the man~facturer the Polyox materials typicall~ have a pH o~
about 10 (e.g. in 5% solution). Soap typically has a pH in 1%~aqueous solution of about 10 (eJg. 1002) 3 while the super-fatted soap~ of thiæ lnvention generally have lower pHæ such as about 9.5.
The poly(ethylene o~de) is genera~ly suppliea as a powder and t~pically has the following particle si~e di~tr~bu-tion when a ~ample thereof is screened through a~ serie~ o~
~ siev~s, expres~ed a~ weight percent retained on the lndicated : Sieve No. ~creen (U.S. Sieve Szries): No. 20-5.2%; No. 40-31.2%;
No. 60r20.7%; NoO 100;1607~ and through No. 100-balance. It i8 o~ten preferable to u3e a ~in~r partl~le ~ize poly(ethyl~ne o~id~) havlng the following distribution a~ mea~ured above:
NoO 20-0.5~; No. 40-13%; No. 60-13%; NoO 100-13.9~ and through No. 100-balance.
, Best results have thus far been obtained hy using a soap made by saponifying a blend of about equal parts of tallow and coconut oil. Generally it is preferred to use a tallow-coco ratio within the range of about 2:1 to 1:2 such as 3:2 or 2:3.
Before mixing it with the various ingredients, the kettle soap is preferably stabilized, as by incorporating into it about 0.06% SnC14 and O.Q24% tetrasodium salt of ethylenediaminetetraacetic acid~ these being added as aque-ous solutions.
~ith respect to the superfatting acid~ best results have thus far been obtained when this comprises about equal proportions of stearic and coco fatty acid. Generally it is preferred to use these acids in a ratio within the range of about 2 1 to 1:2 such as 3:2 or 2:3. The total amount of superfatting acids in the bar is generally less than about 15%.
It will be understood that cation-exchange of Na and ~ -H may occur during processing of the soap-fatty acid mixture and that it is most convenient to express the distri;bution of chain lengths in the mixture in terms which lump together the saponified and unsaponified fatty acids. Typical distributions, so expressed, in bars of this invention are tabulated below:
~ ~ .
..
' ' J~
. . ~ ~ ' ' ' ' ' ~ ' , ~zz~
Number o~ carbon atoms in ~atty acid (fatty acld Per~ent i~ saturat~d unless other-wise noted~ a ,,. ~
8 3.1 2~8 2.9 2,6 12 21~5 14 11~0 10.5 14 monounsaturated . 0~ 0.5 0.2 ~3 15 monoun8aturated 16 1~.0 18~6 16 monounsaturated 1~0 1.7 17 o.6 o.
17 monounsaturated 0.3 ---18 1304 1~.6 18 monounsaturated 21.6 25~9 18 diunsaturated 2.1 2~1 18 triunsaturated 0.3 0.3 ~
up to C12 30.3 26~9 C16 - C14 31.4 31O~
C18 - C17 38.3 41.3 ~z~
With r~spect to the moi~ture content below about 12%
during processing, lt should be noked that in U5~ or storag~, a~ter processing the moisture contenk may increase (see~ for instance~ the hydratlon data in Example l); preliminary r~-sults indicate, however, that the bars have a significantlylower tendency ~o hydrate than commerclal super~atted bars.
Conventional kettle s`oap contains up to about 1~
(e.g. 0.7%~ sodium chloride. The products of this invention ha~e good ~mear resistance wi~hout the need ~or addltion of sodium chlorlde, although it will be und~rstood that ~uch additions (as in the Megson et al patent) are not excluded from the broader scope of the invention~ The bars of this invention have good hardness, comparable to or gre~ter than that o~ ordinary toilet 80~p at gooF~ when khe milling i8 carried out at con~entional relatively low temperature~ (that is, their Dietert hardne~s at 90F is above about 85, e~g~
90 to 92); there is no need to use the higher milling tempera-tures set forth ln the Mcgson et al patent although it will b~
understood that ~he u~e of such milllng temperatures is not 20 excluded ~rom the broad~r scope o~ th~ invention.
The fatty acids in the soap and super~at, and the relative proportions of the various acids, may be as described ln the Uegson patent 3,576,7490 Thus~ these ~atty acids m~y contain about 8-20 carbon atom~. me superfattlng acid may ~ 25 c~ntain ~atty acid~ having an odd number o~ carbons; thus one may employ a fatty acid mixture containing equal proportions (one third each) o~ Cll, C12 and C13 ~aturated ~atty acids (Monsanto CR-1157). .`
.
be melted in combination with soap, detergent base, or other ingredients and then other material incorporated into the melt" (Davidson and Sittig "Water Soluble Resins" pub. 1962, pages 197-8). When it was attempted to incorporate about 2% powdered poly(ethylenezoxide)into a neat soap con~alning about 30% water ("kettle soap"), a mixture was obtained which was lumpy and poorly dispersed and not pumpable.
According to another aspect o$ this invention, it has been found that a superior blend is obtained by incorporat-ing the poly~ethylene oxide), desirably in powder form, into a melt of all, or a portion of, the higher fatty acids which are to be used for super~atting the soap. Best results are obtained when this blend also contains a minor amount of water. As will be seen in Example 3 below, the presence of the water has a marked effect on the nature of the blend of atty acid and high molecular weight poly(ethylene oxide~, significantly decreasing its viscosity; the presence of the water also tends to opacify the blend which may indicate that a water-in-oil type of dis-persion is formed. The water-containing blend can be pumped 2Q readily; its viscosity is well below the upper viscosity limit (which is about 7,0QO or 8,QOO centipoises~ of materials that can be handled readily by ordinary reciprocating pumps. It can thus be easily pumped into admixture with the kettle soap.
The poly~ethylene oxide)~containing soap bars made by this procedure have outstanding properties; they lather well, have an especially pleasant feel during and after use, have good slough resistance and resistance to wet-cracking.
. - , The use o~ thi~ invention make~ ik possible to produce toilet ~oap bars which give a rich and creamy9 but only moderately slippery, lather and which are fi~m and resis~;ant to sloughing and cracking in use.
The following Exampl~s ar~ given to illustrate this invention ~urther. In this application all amounts and proportions are by weight unles~ otherwise s~pecified.
EXA~IE 1 ___ (a) 4.5 parts o~ stearic a~d 4.5 parts coco ~atty acid~ ~re melted together at a temperature o~ 80C 1 n a ve~sel equipped wi~h a stirrer. 1.8 parts o~ hlgh molecular weigh~ poly(ethylene oxide) ("Polyox WRS N~750" sold by Union Carbideg haYing a molecular weight of about 3003000 a viscosity /~hen mea~ured on a 5~ 801ution in water7 o~
about 550 to 900 rps at 25C~ and a melting point in the neighborhood of 65C) are added thereto with stirring while maint~ining the blend at about 80C9 This blend is th~n mixed with a kettle soap (at 70C) in such proport~ons that the resulting mixture contains about 75 parts of the ~odium soap (expressed as anhydrous soap), 4.5 parts o~ the added stearic acid, 4?5 parts o~ the added coco fatty acids and 1.8 parts of the poly(ethylene oxide). The k~ttle soap is made by ~aponi~ying a.50~50 mixture of coconut oil and tallow w~th sodium hydrox~d~ solution, extraction o~ resultant glycerine~
~Iwash~ngi~ w~th electrolyte solution ~nd removal o~ high e}ectrolyt.e nigre 50ap layer all as i~ conventlonal in the manu~acture Or kettle ~oaps; it contain~ about 27~32~ (e~g.
. 30%) wate.r, up to about 1% (e.g. 0.5~) glycerol, up to about .
~z~
0.3% (e.g. 0.1%) NaOH, up to about 1% (e.g. 0.7%) ~aCl. The ingredients are stirred together for a few minutes and the mixture is then formed into dried soap chips containing about 10% moistureJ as by pumping the hot soap mixture onto a chilled roll, forming a thin film on the roll, slicing the film into chips or ribbons and then drying the chips or ribbons.
The chips are then blended with color and perfume (e.g. 0.7%
TiO2 and 1.5% perfume~ in conventional manner in a soap amalgamator at about room temperature, then milled to homo-genize them (e.g. at a temperature of about 15 to 35C), then extruded into a bar form hy means of a con~entional soap plodder (e.g. at a temperature of a~out 20-50C, e.g. ~0C), then cut into cakes; the surfaces of the cakes are cooled and the cakes are pressed into the desired shapes (e.g.
in a pin-die press~.
(hl Part (a) is repeated except that instead of using 4.5 parts stearic ac-,d and 4.5 parts coco fatty aci~ds there is employed 9 parts stearic acid.
(c~ Part (a~ is repeated except that instead of using 4.5 parts stearic acid and ~.5 parts coco fatty acids there is employed 9 parts coco fatty acids.
On testing the soap ~ars ~after aging at least 3 days~ the following results are obtained;
. ~ :
-Sponge Sloue~h 9~ Eroslon Lather (17 hY~ Hydration Cracklng NoO o~ S~ loss (2 hr. ) Index ~troke~ S~ galn ..... ...
(a) 60 1.5 2.6 16.1 12.5 18 (b) 80 3~5 2~2 18,8 11,6 15 (C) 68 5~2 18.7 19.6 10.~ 0 In the sponge lather tesk, which mea6ure8 the quickne86 o~
lather ~ormation~ ~he bar's ~lat sur~ace is alternatel9 rubbed against a sponge and dipped in a pan o~ water (with a hardne~ level o~ 125 ppm and a t~m3p~rature of` 95C3F~)o The up and-down motion of the lather machine produces the number o~ strokes it requires to ~o~m a continuou~ rlng of foam in the pan. me le6s the number of strokes, the quic~er 15 the lather. In the slough t~t, the bar~ are pl~ced ~lat with one side immer~ed in a Petri di~h for sevellksen hours,.
a~ter which time the so~t, muæh~ so~ i~ removed by finger~.
The percent weight 108t aæ slough ls reported. In the er*sion test the bar is inmer~ed in water ~or 260 trokes 20 (about 10 minutes~ of ~he la~h~r machine, a~d the a~nount o~
soap 108~ iS meaæured~, In the h~rdration test the bar~ are con~pletely immers~d in t~p wat~r ~or ~wo hour~ and the in-creas~ in welght is dekerr~inedl, The cracking index i~ an evaluation based on number ana ~everi~y o~ cracks ln a test 25 in which the bars are shaved on one side ts~ hal~ their orlginal ~ize~ then placed under tap water (about 100 ppm hardness) for one h~r, taken out and hung to dry in air until no sign o~ ~ree water remain~ or~ their sur~aces (usually overnight) .
2~4 The bar of part (a) shows unexpectedly high lather quic~ness3 unexpeckedly low slough loss and erosion loæs and quite acceptable cracklng behavior"
EXA~LE 2 _ Bars are made as in Example l(a) except that they alRo contain 0.5% lanolin with and without 0~5% sodium ca~einate solids3 ~hese ingredlents being incorporated with the hot ~atty acid-poly(e~hylene oxide) blend bePore mixing it with the kettle soap.
ExaD~le l(a) is repeated exc~pt that the ~ollowing procedure is employed in making the blend mixed with the kettle soap~ 5 parts o~ commercial stearic acid (m.pO 54C. ) and 5 parts of coco ~atty acids (m.p. 25C, iodine valu~ 6 are mel~ed tog~ther at a temperatur~ o:~ about 102C. One part o~ powder~d hiKh molecular weight poly(ethylerle oxid~
~"Polyox WSR N~750" m.p. about 65~C) i~ added thereto with stirring. The viscosity of the mixture at ~ 02C ls about 750 cps, at 88C it is about 4,000 cps and at 54C it ls about 5,000 cpæ~ (as determined with a Brook~i~ld vi~cosimet~r3 .
One more part of the ~ame Polyox ls then added with stirring. The viscosity of the mlxture 1~ about 18,000 cps at 94e" about 19 ,000 cps at 88C, about 33,500 cps at 66C and about 42,500 cps at 54C~
Then 0.5 part o~ lanolin i~ added with ætirring. ~na resulting blend n~w has a viscosity o~ about 15,000 Cp8 at 94C. and a similar viscc~sity at 70~C.
~7~
z~
Next 1 part o~ water i~ add~d. As a result~ th~ ~orm~r~
ly clear blend becomes cloudy or opaque. Its vl~co~lty i~
about 59000 cps at 77C, about 4,000 cps at 71~C and about 39250 cps Q~ 50 to 63co Ther~aft~r an additional 1 part o~ water is added with stirring~ The re~ulting blend ha~ a vi~co~ity of ~bout 2g250 eps a~ 84C~ 1,500 cp~ at 8~C, 930 cpæ at 71C~ 470 cp~ at 57C, 234 cpS at ~O~C and 114 cps ak 52C, ~ext 2.5 part~ of a solution of ~odium ca~einate (containing 20~ ca~ein) i~ added. The resulting blend is white. Its vi~cos~ty i~ about 23900 Cp8 at 81C9 2,520 cpæ
at 71C, 1,700 cps at 66C and 1,800 cp~ at 60C.
It will be seen that the addltion o~ the water give8 a blend who~e viscosity at, ~a~, 70C is gre~tly decrea~d (e.g. to well below hal~ lt~ valu~ be~ore the additlon of the water)0 Also the blend~ conta~ning water sho~ a r~-markable decrease in visc081ty with decr~ase in temperature (e.g. when temperature ~s reduced~ :erom 7o cr 80 ~, by 10C the viscosity drops by well ov~r 10%). Th~ above re-~ulting blend i~ pu~ed at a temp~ature o~ about 60 85~C
into a mixlng vessel containine kettle 80ap (at 70C) $n such proportions that the resulting m~xture ~ontalrl~ about 75 par*s o~ the ~odiwn soap (e~re~d a~ anhydrous soap), 4.5 part~ o~ the added ætearlc acld, 4.5 ps,rt~ o~ the add~d coco :~atty acids and 1~8 part~ o~ the poly(ethyl0ne oxide)~
~L~5 4 Exan~ple l(a) i~ repeated excep~ that in making ~a~d re~ult~ng blend, 10 par~s o~ ~tearlc ac~d are melt~d and 2 parks of the po.ly(o~hyl~n~ oxld~ of` ~ 1 are added 5 thereto3 followed by 1.5 par~s of wat~r3 while the mixture i8 stirred and maintained at abc>ut 70-90C.
EXAMP,IE 5 Eicample 4 ia r&p~a~ed excep~ that coco ~a~ty acid~
are u~ed in plac~ o~ ~tearic acid~
In the water-contairaine blerad o~ poly(e~hylen~ o~
and h~g~er ~atty ac~as ther~ ~Lre pre~erably abou~ 2 to 20 (more preferably about 4 to 8) part~ of~ the ~a~y acid~ p~r part of poly(ethyIene oxide~ and about 0,,5 lto 5 ~ore pre~
~srably about 1 to 2) part~ of water p~r part o~ poly~ethyl~ne oxide ) .
Xt i~ preferred thæt the amo~t o~ ~aol8tur~ in the in6redi2nt~ adde~ ~o ~he ~attle ~oap be stach that ~h~
mo~sture: 80ap rati o be mainta~ned belo~ about 33~ 67 ~ ~uch a~
about 27:73 to 32:68) to minimize ~o~ation of les~ deæ~r~bl~
ge~ 80~lp pha~e,.
It is desir~ble9 partlcularly in the formulation~
containing relatitrely large amount~ o~ coco ~atty acid~ t ~uch as la) to dry to a mo~sture content below about 18%9 pre-ferably to from a~out 5% to 12%, in order to reduce the tendarlcy for s~ickines~ during la~er blanding (e.g. in the amaIg~mator~ or proc~ingc To the ~ame end it ~ de~irable to use relat:Lvely low pludding te~ratures, pre-cool and pre-dry the outer ~ur~ac~ o~ ~he bar~ be~ox~ pr~s~lng in kh~
die~g and lubrlc~te the die~ (e.eO with ~ aqueous 801utlon conts.inlrlg 16% NaCl ~d 25% ~lycerolj wh~ch i8 then alr-blown off the 8urface~ of' the preæsed b~rs).
. .
~g~ ~
The high molecular weight poly(ethylene oxide) has an average molecular weight of at least about 100,000~
amples OI such compounds are tho~e sold by Union Carbide CompAny under the trademark "Polyox"O These polymer~ are 5 nonionic materials soluble in water, and their molecular w~ights range ~rom about 100~000 to about 5,000~000 or more.
It i8 preferred to employ polymers ~aYing average molecular welghts below 1,000~000, more pref`erably not above about 600,000 such as about 300,000 to 400,,000. For the material having an average molecular weight of about 300,000 a proportion in the neighborhood o~ 2% has glven excelleAt result~. Thiæ
300,000 molecular weight material (sold as Polyo~ WSR ~-750) ha~ a viscos:Lty at 25Co, for a 2~ aqueous solution, o~ about 40 centipoises (Brookfield Splndle No. 1 at 10 rpm): ~or a 5% solution thiæ viscosity is abou~ 600 - 1000 centlpoi~e~
Use of say 2~ o~ extremel~ high molecular weight poly(ethylene oxid~)3 e.g. o~ 4,000,000 average molecular weight~ cause~ the lather to be pituitou~ which is les8 de~irable. According to the man~facturer the Polyox materials typicall~ have a pH o~
about 10 (e.g. in 5% solution). Soap typically has a pH in 1%~aqueous solution of about 10 (eJg. 1002) 3 while the super-fatted soap~ of thiæ lnvention generally have lower pHæ such as about 9.5.
The poly(ethylene o~de) is genera~ly suppliea as a powder and t~pically has the following particle si~e di~tr~bu-tion when a ~ample thereof is screened through a~ serie~ o~
~ siev~s, expres~ed a~ weight percent retained on the lndicated : Sieve No. ~creen (U.S. Sieve Szries): No. 20-5.2%; No. 40-31.2%;
No. 60r20.7%; NoO 100;1607~ and through No. 100-balance. It i8 o~ten preferable to u3e a ~in~r partl~le ~ize poly(ethyl~ne o~id~) havlng the following distribution a~ mea~ured above:
NoO 20-0.5~; No. 40-13%; No. 60-13%; NoO 100-13.9~ and through No. 100-balance.
, Best results have thus far been obtained hy using a soap made by saponifying a blend of about equal parts of tallow and coconut oil. Generally it is preferred to use a tallow-coco ratio within the range of about 2:1 to 1:2 such as 3:2 or 2:3.
Before mixing it with the various ingredients, the kettle soap is preferably stabilized, as by incorporating into it about 0.06% SnC14 and O.Q24% tetrasodium salt of ethylenediaminetetraacetic acid~ these being added as aque-ous solutions.
~ith respect to the superfatting acid~ best results have thus far been obtained when this comprises about equal proportions of stearic and coco fatty acid. Generally it is preferred to use these acids in a ratio within the range of about 2 1 to 1:2 such as 3:2 or 2:3. The total amount of superfatting acids in the bar is generally less than about 15%.
It will be understood that cation-exchange of Na and ~ -H may occur during processing of the soap-fatty acid mixture and that it is most convenient to express the distri;bution of chain lengths in the mixture in terms which lump together the saponified and unsaponified fatty acids. Typical distributions, so expressed, in bars of this invention are tabulated below:
~ ~ .
..
' ' J~
. . ~ ~ ' ' ' ' ' ~ ' , ~zz~
Number o~ carbon atoms in ~atty acid (fatty acld Per~ent i~ saturat~d unless other-wise noted~ a ,,. ~
8 3.1 2~8 2.9 2,6 12 21~5 14 11~0 10.5 14 monounsaturated . 0~ 0.5 0.2 ~3 15 monoun8aturated 16 1~.0 18~6 16 monounsaturated 1~0 1.7 17 o.6 o.
17 monounsaturated 0.3 ---18 1304 1~.6 18 monounsaturated 21.6 25~9 18 diunsaturated 2.1 2~1 18 triunsaturated 0.3 0.3 ~
up to C12 30.3 26~9 C16 - C14 31.4 31O~
C18 - C17 38.3 41.3 ~z~
With r~spect to the moi~ture content below about 12%
during processing, lt should be noked that in U5~ or storag~, a~ter processing the moisture contenk may increase (see~ for instance~ the hydratlon data in Example l); preliminary r~-sults indicate, however, that the bars have a significantlylower tendency ~o hydrate than commerclal super~atted bars.
Conventional kettle s`oap contains up to about 1~
(e.g. 0.7%~ sodium chloride. The products of this invention ha~e good ~mear resistance wi~hout the need ~or addltion of sodium chlorlde, although it will be und~rstood that ~uch additions (as in the Megson et al patent) are not excluded from the broader scope of the invention~ The bars of this invention have good hardness, comparable to or gre~ter than that o~ ordinary toilet 80~p at gooF~ when khe milling i8 carried out at con~entional relatively low temperature~ (that is, their Dietert hardne~s at 90F is above about 85, e~g~
90 to 92); there is no need to use the higher milling tempera-tures set forth ln the Mcgson et al patent although it will b~
understood that ~he u~e of such milllng temperatures is not 20 excluded ~rom the broad~r scope o~ th~ invention.
The fatty acids in the soap and super~at, and the relative proportions of the various acids, may be as described ln the Uegson patent 3,576,7490 Thus~ these ~atty acids m~y contain about 8-20 carbon atom~. me superfattlng acid may ~ 25 c~ntain ~atty acid~ having an odd number o~ carbons; thus one may employ a fatty acid mixture containing equal proportions (one third each) o~ Cll, C12 and C13 ~aturated ~atty acids (Monsanto CR-1157). .`
.
3~ ;2f~L
The soap bars of this invention may contain conventional ingredlents such as opacifiers (e.g. 0.4% titanium dioxide added in the amalgamator), lanolin ~e.g. 1/2% added to ~he neat soap, preferably in admixture with the superfat), glycerine (e.g. 1% added in the amalgamator or to the neat soap), soap perfume (e.g. 1-3% such as 1.5-2% added in the amalgamator~, antioxidants (e.g. 0.02% di-~-bu~yl p-cresol or s~ added to the neat soap), protein (e.g.
0.5% sodium caseinate, added to the neat soap or, as an aqueous solution, in the amalgamator). Antibacterials or germicides such as those mentioned in Megson 3,576,749 and Kaniecki 3,598,746 may be included. It is within the broader scope of the invention to aerzte the bars, in a manner well known in the art, to give lower density ~floating) soaps, such as those having a spec-ific gravity of about 0.8.
Toilet soap bars range in size from the relatively small hotel size (weighing about 20-30 grams) to the regular si~e (about lO0 grams) to the bath siæe ~about 150g) to the extra large size (about 200g). The bars of this invention may be of such sizes, particularly in the range of about 100 to 200 grams.
As mentioned above, the poly(ethylene oxide) may be incorporated in two stages, one portion (such as about half or two thirds of the total polymer) being incorporated into the neat soap and the other portion being added to the soap chips in the amalgamator. In order to reduce the tendency to form specks when the latter addition i~ made in the amalgamator it is desirable to add the pol~mer there in the form of very finely ground material (such as material of which 98% passes through a no. 100 screen (U.S. Sieve series) ànd to thoroughly .
~z~
distribute the powdered polymer on the surPace& o~ the chips in t~e amalgamator prlor to adding the other ingredlents such as pigment~ When a significant portion of the total pol~mer is incorporated into the neat ~oap, the soap is le~
sticky during the incorpora~ion o~ the balance o~ the pol~mer in ~he amalgamator and the amalgamation process may be accomplished more easlly and with less power.
It is understood thàt the ~oregoing detailed descrip-tion is given merely by way o~ illustration and variatlons may be made ~herein wi~hout departing ~rom the ~pi~lt of the invention.
The soap bars of this invention may contain conventional ingredlents such as opacifiers (e.g. 0.4% titanium dioxide added in the amalgamator), lanolin ~e.g. 1/2% added to ~he neat soap, preferably in admixture with the superfat), glycerine (e.g. 1% added in the amalgamator or to the neat soap), soap perfume (e.g. 1-3% such as 1.5-2% added in the amalgamator~, antioxidants (e.g. 0.02% di-~-bu~yl p-cresol or s~ added to the neat soap), protein (e.g.
0.5% sodium caseinate, added to the neat soap or, as an aqueous solution, in the amalgamator). Antibacterials or germicides such as those mentioned in Megson 3,576,749 and Kaniecki 3,598,746 may be included. It is within the broader scope of the invention to aerzte the bars, in a manner well known in the art, to give lower density ~floating) soaps, such as those having a spec-ific gravity of about 0.8.
Toilet soap bars range in size from the relatively small hotel size (weighing about 20-30 grams) to the regular si~e (about lO0 grams) to the bath siæe ~about 150g) to the extra large size (about 200g). The bars of this invention may be of such sizes, particularly in the range of about 100 to 200 grams.
As mentioned above, the poly(ethylene oxide) may be incorporated in two stages, one portion (such as about half or two thirds of the total polymer) being incorporated into the neat soap and the other portion being added to the soap chips in the amalgamator. In order to reduce the tendency to form specks when the latter addition i~ made in the amalgamator it is desirable to add the pol~mer there in the form of very finely ground material (such as material of which 98% passes through a no. 100 screen (U.S. Sieve series) ànd to thoroughly .
~z~
distribute the powdered polymer on the surPace& o~ the chips in t~e amalgamator prlor to adding the other ingredlents such as pigment~ When a significant portion of the total pol~mer is incorporated into the neat ~oap, the soap is le~
sticky during the incorpora~ion o~ the balance o~ the pol~mer in ~he amalgamator and the amalgamation process may be accomplished more easlly and with less power.
It is understood thàt the ~oregoing detailed descrip-tion is given merely by way o~ illustration and variatlons may be made ~herein wi~hout departing ~rom the ~pi~lt of the invention.
Claims (11)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A toilet soap bar consisting essentially of sodium soap of higher fatty acids having about 8 to 20 carbon atoms as substantially the sole detergent, about 6 to 12% of superfatting higher fatty acids having about 8 to 20 carbon atoms, about 1 to 4% poly(ethylene oxide) having a molecular weight in the range of about 100,000 to 5,000,000, and about 5 to 18% water.
2. A toilet soap bar as in claim 1 in which said mole-cular weight is about 300,000 to 600,000 and the proportion of poly(ethylene oxide) is about 1.5 to 3%.
3. A toilet soap bar as in claim 1 or 2 in which said sodium soap is a mixture of tallow and coconut oil soaps in a ratio of about 1:2 to 2:1.
4. A toilet soap bar as in claim 1 or 2 in which said sodium soap is a mixture of about equal parts of tallow and coconut oil soaps.
5. A toilet soap bar as in claim 1 or 2 in which said super-fatting acids comprise a mixture of stearic and coco fatty acids in a ratio of about 2:1 to 1:2.
6. A toilet soap bar as in claim 1 or in which said super-fatting acids comprise a mixture of about equal parts of stearic and coco fatty acids.
7. Process for preparing a toilet soap bar consisting essentially of sodium soap of higher fatty acids having about 8 to 20 carbon atoms as substantially the sole detergent, about 6 to 12% of superfatting higher fatty acids having about 8 to 20 carbon atoms, about 1 to 4% poly(ethylene oxide) having a molecular weight in the range of about 100,000 to 5,000,000, and about 5 to 18% water which process comprises mixing neat soap containing said sodium soap and about 30% moisture with a blend of said poly(ethylene oxide) in a melt of said superfatting higher fatty acids, subjecting the resulting mixture to drying conditions, and thereafter shaping the mixture into a bar.
8. Process as in claim 7 in which said blend contains about 2 to 20 parts of said superfatting fatty acids per part of said poly(ethylene oxide).
9. Process as in claim 7 or 8 in which said blend con-tains a minor proportion of dispersed water sufficient to decrease the viscosity of said blend.
10. Process as in claim 7 or 8 in which said blend contains 0.5 to 5 parts of water per part of said poly(ethylene oxide).
11. Process as in claim 7 or 8 in which said blend contains about 4 to 8 parts of said superfatting fatty acids and about 1 to 2 parts of water per part of said poly(ethylene oxide).
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US05/816,119 US4169066A (en) | 1977-07-15 | 1977-07-15 | Process of incorporating poly(ethylene oxide) into soap |
| US816,119 | 1977-07-15 | ||
| US816,123 | 1977-07-15 | ||
| US05/816,123 US4169067A (en) | 1977-07-15 | 1977-07-15 | Bar product |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1102204A true CA1102204A (en) | 1981-06-02 |
Family
ID=27124033
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA307,323A Expired CA1102204A (en) | 1977-07-15 | 1978-07-13 | Bar soap and process of manufacture |
Country Status (20)
| Country | Link |
|---|---|
| AT (1) | AT379612B (en) |
| AU (1) | AU522873B2 (en) |
| BR (1) | BR7804518A (en) |
| CA (1) | CA1102204A (en) |
| CH (1) | CH637158A5 (en) |
| DE (1) | DE2830827C2 (en) |
| DK (1) | DK314878A (en) |
| ES (1) | ES471681A1 (en) |
| FR (1) | FR2397454A1 (en) |
| GB (1) | GB2001098B (en) |
| GR (1) | GR71683B (en) |
| IE (1) | IE47125B1 (en) |
| IT (1) | IT1105529B (en) |
| MX (1) | MX151225A (en) |
| NL (1) | NL178428C (en) |
| NO (1) | NO149067C (en) |
| NZ (1) | NZ187793A (en) |
| PH (1) | PH18992A (en) |
| PT (1) | PT68288B (en) |
| SE (1) | SE439646B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PT83523B (en) * | 1985-10-29 | 1988-11-30 | Procter & Gamble | PROCESS FOR THE PREPARATION OF A COSMETIC COMPOSITION USING SAUCE OF FATTY ACIDS C8-24 |
| GB9313859D0 (en) * | 1993-07-05 | 1993-08-18 | Unilever Plc | Improvements relating to soap bars |
| GB9718235D0 (en) | 1997-08-28 | 1997-11-05 | Unilever Plc | Soap bars |
| EP3074498B1 (en) | 2013-11-25 | 2019-04-17 | Unilever Plc. | Soap bar formulations with improved skin softness comprising nonionic polymer structuring system |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2894912A (en) * | 1954-09-21 | 1959-07-14 | Lever Brothers Ltd | Isethionate detergent bar |
| DE1108362B (en) * | 1960-01-26 | 1961-06-08 | Schmidt Sche Heissdampf | Method and device for cooling fission gases |
| US3376229A (en) * | 1964-12-11 | 1968-04-02 | Lever Brothers Ltd | Synthetic detergent bar |
| US3598746A (en) * | 1969-05-09 | 1971-08-10 | Armour Dial Inc | Cosmetic soap bar |
| ZA772992B (en) * | 1976-06-04 | 1978-12-27 | Colgate Palmolive Co | Toilet bar soap |
| NZ184181A (en) * | 1976-06-04 | 1979-10-25 | Colgate Palmolive Co | Preparing toilet soap bars comprising poly-(ehtyene oxide) of high molecular weight |
-
1978
- 1978-07-05 SE SE7807559A patent/SE439646B/en not_active IP Right Cessation
- 1978-07-07 GR GR56733A patent/GR71683B/el unknown
- 1978-07-07 AU AU37846/78A patent/AU522873B2/en not_active Expired
- 1978-07-07 NZ NZ187793A patent/NZ187793A/en unknown
- 1978-07-11 IT IT50247/78A patent/IT1105529B/en active
- 1978-07-13 DE DE2830827A patent/DE2830827C2/en not_active Expired
- 1978-07-13 PT PT6828878A patent/PT68288B/en unknown
- 1978-07-13 CA CA307,323A patent/CA1102204A/en not_active Expired
- 1978-07-13 GB GB7829798A patent/GB2001098B/en not_active Expired
- 1978-07-13 FR FR7820983A patent/FR2397454A1/en active Granted
- 1978-07-13 BR BR7804518A patent/BR7804518A/en unknown
- 1978-07-13 DK DK783148A patent/DK314878A/en not_active Application Discontinuation
- 1978-07-13 ES ES471681A patent/ES471681A1/en not_active Expired
- 1978-07-14 NO NO782445A patent/NO149067C/en unknown
- 1978-07-14 CH CH766878A patent/CH637158A5/en not_active IP Right Cessation
- 1978-07-14 MX MX174200A patent/MX151225A/en unknown
- 1978-07-14 NL NLAANVRAGE7807605,A patent/NL178428C/en active Search and Examination
- 1978-07-14 IE IE1424/78A patent/IE47125B1/en unknown
- 1978-07-14 PH PH21380A patent/PH18992A/en unknown
- 1978-07-17 AT AT0515278A patent/AT379612B/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| DK314878A (en) | 1979-01-16 |
| AU522873B2 (en) | 1982-07-01 |
| NL7807605A (en) | 1979-01-17 |
| NL178428C (en) | 1986-03-17 |
| CH637158A5 (en) | 1983-07-15 |
| GB2001098B (en) | 1982-01-27 |
| IT7850247A0 (en) | 1978-07-11 |
| NZ187793A (en) | 1981-04-24 |
| PT68288A (en) | 1978-08-01 |
| PH18992A (en) | 1985-11-29 |
| DE2830827C2 (en) | 1986-05-28 |
| IE781424L (en) | 1979-01-15 |
| DE2830827A1 (en) | 1979-01-25 |
| FR2397454B1 (en) | 1983-01-07 |
| AU3784678A (en) | 1980-01-10 |
| ES471681A1 (en) | 1979-02-01 |
| NO149067B (en) | 1983-10-31 |
| MX151225A (en) | 1984-10-15 |
| NO782445L (en) | 1979-01-16 |
| ATA515278A (en) | 1985-06-15 |
| IT1105529B (en) | 1985-11-04 |
| SE439646B (en) | 1985-06-24 |
| GR71683B (en) | 1983-06-21 |
| FR2397454A1 (en) | 1979-02-09 |
| SE7807559L (en) | 1979-01-16 |
| BR7804518A (en) | 1979-03-20 |
| NO149067C (en) | 1984-02-15 |
| GB2001098A (en) | 1979-01-24 |
| IE47125B1 (en) | 1983-12-28 |
| PT68288B (en) | 1994-01-18 |
| AT379612B (en) | 1986-02-10 |
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| MKEX | Expiry |