CN1240474A - Pourable cast melt bar compositions comprising low levels of water and minium ratios of polyol to water - Google Patents
Pourable cast melt bar compositions comprising low levels of water and minium ratios of polyol to water Download PDFInfo
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- CN1240474A CN1240474A CN 97180669 CN97180669A CN1240474A CN 1240474 A CN1240474 A CN 1240474A CN 97180669 CN97180669 CN 97180669 CN 97180669 A CN97180669 A CN 97180669A CN 1240474 A CN1240474 A CN 1240474A
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Abstract
The present invention relates to cast melt bar compositions comprising surfactant, fatty acid, generally lower MW polyalkylene glycol and small amounts of water wherein the ratio of total polyol to water is at least 3:1. By using less water and greater variants of polyol, the bars allow larger amounts of generally insoluble materials to be used and also allow retention of bar integrity using limited amounts of soap (important for mildness).
Description
Technical field of the present invention
The present invention relates to cast melt bar compositions, but because of its founding, therefore can process, and if desired, can also carry a large amount of beneficial agents (as, in extruding bar, when using a small amount of beneficial agent, usually be difficult to carry, and when its consumption was enough to deposit, this bar was often processed because of soft being difficult to again).Also have because water-content is low and ratio polyvalent alcohol and water reach minimum, but this bar founding also can be carried and is very difficult to the water soluble ingredient carried usually.
Background technology
The personal cleansing bar just constantly trends towards the mild formulation with the oily softener, to improve the nursing to skin.Traditional bar extrude technology (as, wherein each composition is merged, high temperature mixes, chilling is to form fragment, then the fragment mold pressing is extruded), be difficult to produce low melting point lubricant and gentle water soluble surfactant active (as, the liquid ingredient) product that content is high especially.But by use so-called casting technology (as, liquid ingredient can form the finished product bar by cooling in mould), can easilier prepare the high bar of liquid ingredient content.More particularly, though do not think bound by theory, it is believed that this is because the network structure of the crystalline solid state component of bar (as, fatty acid soaps) can be held back high-load liquid, and expressing technique can destroy this network structure, causes liquid phase separation inevitably; But casting technology can make network structure not be damaged, and can be used for holding back liquid ingredient.
But in the melt cast compositions of prior art, need water-content that requirement will be dissolved the soap composition to reduce to minimum and make it to form the crystallization reticulated structure, keep low viscosity isotropy molten simultaneously.And when the consumption of water not enough (that is, subsistence level 10%), this prescription is (that is, viscosity is too high, can not cast) that can not process.Furtherly, as mentioned above, need be with the water of minimum quantity with the dissolving soap, and form the crystalline network structure.
For example, the United States Patent (USP) № 5262079 that authorizes people's such as Kacher United States Patent (USP) № 5227086 and authorize people such as Kacher provides frame system (promptly, founding) skin clean bar, wherein comprise 5-50% lipid acid (in United States Patent (USP) № 5262079, in and 20-65%; And in United States Patent (USP) № 5227086, all be free acid basically), the negatively charged ion of about 15-65% or the water of firm auxiliary agent of nonionic bar and 15-55%.
WO 95/26710 (belongs to Procter﹠amp; Gamble) claimed a kind of skin clean bar that foams wherein comprises the lipid actie skin moisturizer of (a) 5-40 part; (b) fatty acid soaps of 10-50 part; (c) synthetic surfactant that foams of 1-50 part; (d) water of 10-50 part.
Go up clear statement as the 20th page of reference WO 95/26710, be lower than 10% water-content and will have a strong impact on these bars, because this moment, said composition was (that is, viscosity is too high, can not cast) that can not process.On the contrary, though bar of the present invention also can make being lower than under 10% the water-content by the isotropic mixture of can casting.
In the United States Patent (USP) № 5520840 that authorizes people such as Massoro, the claimed a kind of bar of applicant (belong in principle extrude, but not cast melt bar thing), it is formed some and is similar to the present composition.
Composition in this reference paper comprises synthetic surfactant, water-soluble structure agent (high-molecular weight polyoxyalkylene or polyoxyalkylene mixture in being preferably), the water-insoluble structural agent (as, lipid acid) of 10-60% and the water of low levels.
But because these compositions belong to usually and extrude bar compositions, thus they with bar of the present invention between have some mainly difference.
At first, the polyol component of bar of the present invention (b) should have " liquid " more much higher than the bar content of Massaro (as, lower molecular weight) component, can guarantee like this, and this melt can be cast when casting with the preparation bar.Therefore, bar of the present invention needs the many alkoxide components of alkylidene group (as, C
2-C
4Aklylene glycol and/or glycerine), but also requirement, many alcohol of alkylidene group or the many alcohol of alkylidene group add that the ratio of beneficial agent and polyalkylene glycol is about 0.8: 1 or higher.
The second, the bar of Massaro has and preferably is no more than 10% soap, and bar of the present invention then has and is higher than 10% soap, the soap of preferred 10.5-20% weight.Though do not think to it is believed that in casting technology under the situation of bound by theory, the soap that needs minimum quantity with form can hold back liquid ingredient (as, water and low molecular weight polyols) network structure.And opposite, extrude bar and needn't require the soap amount minimum.
The 3rd, it is introduced, the bar of Massaro (as, extrude bar) use seldom or not use any beneficial agent (as, when using siloxanes, it is only as processing aid, even and if like this, its consumption is also below 0.5%).On the contrary, bar of the present invention comprises 0-30% weight, preferred 1-25% weight, the more preferably beneficial agent of 1.5-15% weight.
At last, reference paper about people such as Kacher, people such as Kacher not only do not introduce the importance of polyvalent alcohol kind, even if consider that egregious cases (promptly, WO 95/26710 introduces, the water of 10-50% and the polyvalent alcohol of 0.5-35%), the polyvalent alcohol that may reach is 35% to 10% with the ceiling rate of water, or 3.5: 1.But obviously, the total hope of Kacher has higher water-content (as, the 15-40% that the US reference paper is introduced) and lower polyvalent alcohol content.Therefore, Kacher does not introduce or hints the ratio 3: 1 of polyvalent alcohol of the present invention and water, preferably at least 3.5: 1, more preferably at least 4: 1.In order to be able to successfully the cast scope of founding, the present invention requires these ratios.
Rephrase the statement, the original idea of Kacher obviously is that higher water and polyvalent alcohol ratio (referring to embodiment) will be provided, and bar is necessary because this is processing.On the contrary, it is considered herein that,, also can successfully process even if under the ratio of high polyvalent alcohol and water.
General introduction of the present invention
Beyond thoughtly be, the applicant has been found that a kind of like this situation, wherein, by very carefully selecting various variablees, can when keeping gentle tensio-active agent and transferring out relative a large amount of beneficial agent (possibility that is higher than prior art), founding obtain bar.This bar can be than thought founding under the low situation of possible water-content in the past.
Specifically, the present invention includes the bar compositions that is used for founding, wherein comprise:
(a) the synthetic nonsoap detergent of 10-40% weight or the mixture of synthetic nonsoap detergent;
(b) polyvalent alcohol of 10-50% weight, this polyvalent alcohol comprises the mixture of following material
(i) the about 2000-20000 of molecular weight, the about 55-65 of fusing point ℃, and have the polyalkylene glycol of following general formula:
R wherein
1=hydrogen atom, C
1-C
4Alkyl;
R
2=hydrogen atom, CH
3And
N=is about 40200, preferred 40-100; With
(ii) its fusing point at room temperature is the C of liquid
2-C
4The many alcohol of alkylidene group (as, ethylene glycol, propylene glycol or glycerine);
Wherein the many alcohol of alkylidene group add component with the ratio or the many alcohol of alkylidene group of polyalkylene glycol
(e) ratio of beneficial agent and polyalkylene glycol is about 0.8: 1 or higher;
(c) the water-insoluble structural agent of 5-40% is selected from the saturated C of preferred straight chain
8-C
24Free fatty acids and C
8-C
20Preferred straight chain saturated alkoxides;
(d) greater than 8%, the soap of preferred 10-30%;
(e) 0-30%, preferred 1-25%, more preferably the beneficial agent of 1.5-15% (as, siloxanes or other soothing oil); With
(f) the following % of 2-10, the water of preferred 2-8%;
The ratio of wherein total polyvalent alcohol (b) and water is at least about 3: 1, more preferably at least about 4: 1.
In the preferred concrete example of the present invention, can be by adding 1-10%, the wax of preferred 2-5% as the lipid acid substitute with further raising use properties.
Detailed description of the present invention
The present invention relates to cast melt bar compositions, wherein comprise gentle surfactant system (as, synthetic, non-soap active substance).Because they are not soap structural system, therefore, carefully option table surface-active agent and its are dissolved or dispersed in solvent wherein, could guarantee that like this tensio-active agent is easy to dissolving or dispersion is uniform to form, preferred isotropic melt.In addition, this melt should have enough low viscosity to be inhaled to carry out pump, and cooling back solid should have the structural integrity of personal cleansing bar.
Prior art cast melt bar thing (as, people's such as above-mentioned Kacher bar) but need relatively large water could produce pumping viscosity, though bound by theory not it is believed that the present invention can be by a large amount of low molecular weight solvent of use, and avoids using a large amount of water like this.
Relate to prior art reference paper that extrudes bar (as, people's such as above-mentioned Kacher bar) even the importance of also not recognizing solvent system, but because extrude bar and do not require the pumping low viscosity mixtures.
Beyond thoughtly be, the applicant has been found that a low-down water-content scope, wherein, and by considering solvent system (and ratio of polyvalent alcohol and water), can obtain synthetic non-soap surfactant low viscosity (as, under 90 ℃, be lower than about 10000 centipoises) but the pumping mixture.And as a kind of cast melt bar thing, it can use than extruding bar (in extruding bar, beneficial agent just has loss man-hour adding) consumption and want big softener/beneficial agent.
In fact, the applicant has identified the low melt cast compositions of a kind of water-content, and it can guarantee the more substantial softener of delivery ratio prior art.
The various components of this system below will be described in further detail.
(a) synthetic non-soap surfactant
Bar of the present invention comprises the 10-50% that accounts for total bar compositions, preferred 20-50%, the more preferably synthetic non-soap surfactant of 25-50%.
More particularly, this surfactant system generally comprises at least a anion surfactant, amphoterics, or the mixture of preferred anionic tensio-active agent or anion surfactant and zwitterionics.
Operable anion surfactant is an aliphatic sulfonate, as uncle's alkane (as, C
8-C
22) sulfonate, uncle's alkane is (as, C
8-C
22) stilbene-4,4'-bis-(1-azo-3, 4-dihydroxy-benzene)-2,2'-disulfonate, C
8-C
22Alkene sulfonate, C
8-C
22Hydroxyl alkane sulfonate or alkyl glycerol ether sulfonate (AGS); Or aromatic sulphonate, as alkylbenzene sulfonate.
Anion surfactant also can be that alkyl-sulphate is (as, C
12-C
18Alkyl-sulphate) or sulfated alkyl ether (comprising alkyl glycerol base ether sulfate).Alkylether sulfonate has following structural formula:
RO(CH
2CH
2O)
nSO
3M
Wherein R is for having 8-18 carbon atom, the alkyl or the alkenyl of preferred 12-18 carbon atom, and the mean value of n is preferably greater than 3 greater than 1.0; And M is the solubilising positively charged ion, as sodium, potassium, ammonium or replacement ammonium.Zetesol AP and Zetesol NL are preferred.
Anion surfactant can also be that alkyl sulfo succinate (comprises list and dialkyl group, as C
6-C
22Sulfosuccinate); Alkyl and acyl taurine salt, alkyl and acyl sarcosinate, sulfosalicylic acetate, C
8-C
22Alkylphosphonic and phosphoric acid salt, alkyl phosphate and alkoxyalkyl phosphoric acid ester, acyl-lactate, C
8-C
22Monoalkyl succinate and maleate, sulfosalicylic acetate, alkyl glycoside and acyl-hydroxyethyl sulfonate.
Sulfosuccinate can be the monoalkyl sulfosuccinate with following structural formula:
R
1O
2CCH
2CH (SO
3M) CO
2M; With
Acid amides-MEA sulfosuccinate with following structural formula:
R
1CONHCH
2CH
2O
2CCH
2CH(SO
3M)CO
2M
R wherein
1Be C
8-C
22Alkyl, and M is the solubilising positively charged ion.
Sarcosinate generally can be by formula R CON (CH
3) CH
2CO
2M represents that wherein R is C
8-C
22Alkyl, and M is the solubilising positively charged ion.
Taurate generally can be represented by following structural formula,
R
2CONR
3CH
2CH
2SO
3M
R wherein
2Be C
8-C
22Alkyl, R
3Be C
1-C
4Alkyl, and M is the solubilising positively charged ion.
Particularly preferably be C
8-C
18Acyl-hydroxyethyl sulfonate.These esters can by the basic metal isethionate with have 6-18 carbon atom and iodine number mixing-in fat acid-respons and obtain less than 20.The mixed fatty acid of at least 75% weight has 12-18 carbon atom, and the mixed fatty acid of maximum 25% weight has 6-10 carbon atom.
As long as exist, acyl-hydroxyethyl sulfonate is generally about 10-40% of total bar compositions weight.This component is preferably about 15-35% weight.
Acyl-hydroxyethyl sulfonate can be the alkoxylate isethionate, and is described as people's such as Ilardi United States Patent (USP) 5393446, incorporates it into the present invention as a reference at this.This compound has following general formula
Wherein R is the alkyl with 8-18 carbon atom, and m is the integer of 1-4, and X and Y are hydrogen atom or the alkyl with 1-4 carbon atom, and M
+Be monovalent cation, as sodium, potassium or ammonium.
In general, anionic group accounts for about 10-40% weight of bar compositions, preferred 15-35% weight.
Can be used for ampholytic detergent of the present invention and comprise at least one acidic group, described acidic group can be carboxyl or sulfonic group.They comprise quaternary nitrogen atoms, are the season amic acid therefore.They generally should comprise alkyl or the alkenyl with 7-18 carbon atom.They have following formula usually:
R wherein
1Alkyl or alkenyl for 7-18 carbon atom;
R
2And R
3Respectively independently for having alkyl, hydroxyalkyl or the carboxylic of 1-3 carbon atom
Alkyl;
N is 2-4;
M is 0-1;
X is the alkylidene group of 1-3 carbon atom being replaced by hydroxyl arbitrarily, and
Y is-CO
2-or-SO
3-.The suitable ampholytic detergent of above-mentioned general formula comprises the simple trimethyl-glycine of following structural formula:
Acyl ammonia trimethyl-glycine with following structural formula:
Wherein m is 2 or 3.
In last two formulas, R
1Alkyl or alkenyl for 7-18 carbon atom; And R
2And R
3Be alkyl, hydroxyalkyl or the carboxyalkyl of 1-3 carbon atom independently respectively.R
1Specifically can be C derived from coconut
12Alkyl and C
14The mixed form of alkyl, so at least half, preferred 3/4 R
1Group has 10-14 carbon atom.R
2And R
3Preferable methyl.
Ampholytic detergent can also be the sultaine of following structural formula:
Or
Wherein m is 2 or 3, perhaps can be wherein-(CH
2)
3SO
3-by following formula alternate variant,
In these structural formulas, R
1, R
2And R
3Definition is as described in the acyl ammonia trimethyl-glycine.
Ampholytic detergent generally accounts for the 1-10% of bar compositions weight.
Also can use other tensio-active agent (as, non-ionic, cationic), although they generally account for below the 0.01-10% of bar compositions weight.
Nonionogenic tenside especially comprises the compound with hydrophobic group and active hydrogen atom, reaction product as fatty alcohol, acid, acid amides or alkylphenol and oxyalkylene, especially separately and oxyethane, or with the reaction product of the mixture of oxyethane and propylene oxide.Specific nonionic detergent compounds is alkyl (C
6-C
22) phenol-ethylene oxide condensate, aliphatic series (C
8-C
18) straight or branched uncle or the condensation product of secondary alcohol and oxyethane and the product of making by the condensation reaction of oxyethane and propylene oxide-reacting ethylenediamine product.Other so-called nonionic detergent compounds comprises long chain tertiary amine oxide compound, long chain tertiary phosphine oxide and dialkyl sulphoxide.
Nonionic detergent compounds can also be sugared acid amides, as polysaccharide amide.Specifically, this tensio-active agent can be that United States Patent (USP) № 5389279 (authorizes people such as Au, incorporate it into the present invention as a reference at this) described a kind of lactose amide, and as the described polyhydroxy amides of United States Patent (USP) № 5312954 (authorize people such as Letton, incorporate it into the present invention as a reference) at this.
The example of cationic detergent is a quaternary ammonium compound, as the alkyl dimethyl ammonium halide.
Operable other tensio-active agent is at the United States Patent (USP) № 3723325 that authorizes Parran Jr and Schwartz, Perry﹠amp; " tensio-active agent and washing composition " (I﹠amp of Berch; The II volume) in description is arranged, incorporate it into the present invention as a reference at this.
Preferred compositions comprises the acyl-hydroxyethyl sulfonate of 10-40% weight and the trimethyl-glycine of 1-10% weight.More than 20% weight of this surfactant comprise bar compositions, preferred 25-40% weight.
(b) polyol component
The of the present invention second required component is the mixture of polyvalent alcohol, described polyvalent alcohol comprises polyalkylene glycol component and the many alkoxide components of alkylidene group, wherein the many alcohol of many alcohol of alkylidene group (AP) or alkylidene group are about 0.8: 1 or higher with the mixture of beneficial agent and the weight ratio of polyalkylene glycol, be preferably greater than 1.5: 1, more preferably greater than 2: 1.This upper limit is preferably less than about 20: 1.
Polyalkylene glycol should be middle high molecular or low-molecular-weight material, and its molecular weight ranges is about 2000-20000, preferred 4000-10000, and its fusing point is 55-65 ℃.
The many alcohol of alkylidene group have following formula:
R
1-O(CH
2-CHO)
nH
R wherein
1Be hydrogen atom (H), C
1-C
4Alkyl;
R
2Be H or CH
3And
The about 40-200 of n=.
The preferred C of the many alcohol of alkylidene group
2-C
4How pure alkylidene group is, and its fusing point should make it at room temperature for liquid.Its example comprises ethylene glycol, propylene glycol and glycerine.
Owing in these cast melt bar things, used the water (but this helps to guarantee good pumping) of low levels, therefore importantly, as mentioned above, the many alcohol of many alcohol of alkylidene group or alkylidene group will be above the content of polyalkylene glycol with the content of the mixture of beneficial agent.
(c) water-insoluble structural agent/lipid acid
The of the present invention the 3rd required component is used about 5-40% weight, and the water-insoluble structural agent of preferred 10-25% weight is as lipid acid.Specially suitable material is a lipid acid, and especially its carbochain is the lipid acid of 12-24 carbon atom.Its example be lauric acid, tetradecanoic acid, palmitinic acid, stearic acid, arachidonic acid and docosoic acid, and composition thereof.These lipid acid can be from coconut, topping coconut, palm, palm nuclear, Ba Basu and tallow fatty acid and partially or completely sclerosing fatty acid or distilled fatty acid.Other suitable water-insoluble structural agent comprises alkanol, the especially hexadecanol of 8-20 carbon atom.The water solubility of these materials under 20 ℃ generally is lower than 5 grams per liters.
The use wear rate of the relative proportion may command bar of water-soluble structure agent (b) and water-insoluble structural agent (d).Therefore the solvency action that the water-insoluble structural agent can delay bar when using in water can delay wear rate.
The total amount of component (d) is preferably the 5-40% of composition weight, more preferably 10-25%.
(d) soap
The of the present invention the 4th required component is a soap, promptly contains about-30% weight more than 8, preferred-Yue 20% soap more than 10.
Soap is meant the salt of the mono fatty acid with 8-22 carbon atom chain length, for reaching optimum structure and gentle degree, preferred C
16-C
22
Though do not think bound by theory,, it is believed that it is its important difference part that soap content is reduced to minimum for the bar that extrudes that not necessarily requires high soap content like this.
(e) beneficial agent
Owing to be founding, therefore a key element of the present invention is, can add 0-30% weight in bar compositions, the ability of the beneficial agent of preferred 1-25% weight.
Beneficial agent of the present invention " composition " can be single beneficial agent component, maybe can be the beneficial agent compound that adds by carrier.And the wherein a kind of or whole compounds of the mixture that this beneficial agent composition can be two or more compounds are useful.In addition, when people wished to add other component in this bar compositions, this beneficial agent itself can play a part these component carriers.
Beneficial agent can be " soothing oil ", promptly a kind ofly comes softening skin (stratum corneum) and reduces and keep the material of dermalaxia by delaying water-content by increasing water-content.
Preferred softener comprises:
(a) silicone oil, natural gum and modified form thereof are as straight chain and X 2-1401; Amino, alkyl, alkaryl and aryl silicone oil;
(b) fat and oils are comprising natural fat and oils, as simmondsia oil, soya-bean oil, Rice pollard oil, Lipoval A, Prunus amygdalus oil, sweet oil, sesame oil, persic oil, Viscotrol C, Oleum Cocois, ermine oil; Theobroma oil; Butter, lard; The winterized stearin that obtains by the aforementioned oils of hydrogenation; And synthetic glycerine list, two and three acid esters, as tetradecanoic acid glyceryl ester and 2 ethyl hexanoic acid glyceryl ester;
(c) wax class is as carnauba wax, spermaceti, beeswax, lanolin and derivative thereof;
(d) hydrophobic plant milk extract;
(e) hydro carbons is as whiteruss, Vaseline, Microcrystalline Wax, ceresine, squalene, pristane and mineral oil;
(f) higher fatty acid is as lauric acid, tetradecanoic acid, palmitinic acid, stearic acid, docosoic acid, oleic acid, linolic acid, linolenic acid, lanoceric acid, Unimac 5680 and polyunsaturated fatty acid (PUFA);
(g) higher alcohols is as lauryl alcohol, hexadecanol, stearyl alcohol, oleyl alcohol, behenyl alcohol, cholesterol and 2-hexadecanol;
(h) ester class is as Octanoic acid, hexadecyl ester, lactic acid meat myristyl ester, lactic acid cetyl, Isopropyl myristate, Tetradecyl tetradecanoate, Wickenol 111, hexanodioic acid isopropyl ester, butyl stearate, decyl oleate, Unimac 5680 cholesteryl ester, glyceryl monostearate, distearin, Tristearoylglycerol, lactic acid alkyl ester, citric acid alkyl ester and tartrate alkyl ester;
(i) perfume oil is as peppermint, jasmine, camphor, cdear, bitter orange peer, ryu, rosin, Chinese cassia tree, Citrus bergamia, lemon, Calamus, pine tree, lavandula angustifolia, bay, cloves, day Thujopsis dolabrata, eucalyptus, lemon, May star, Thymus vulgaris, peppermint, rose, red sage, menthol, Terpane, eugetinic acid, citral, lemongrass, borneol, coriandrol, Geraniol, Flower of Beltleaf Primrose, camphor, thymol, spirantol, penene, limonene and terpenoid;
(j) lipoidis is as cholesterol, ceramide, sucrose fat and European patent specification 556957 described plan ceramides;
(k) VITAMIN, as vitamin A and E, and the VITAMIN alkyl ester, comprising the vitamins C alkyl ester;
(l) sunscreen products is as octyl methoxycinnamate (Parsol MCX) and the stupid formyl radical methane of butyl methoxyl group (Parsol 1789);
(m) phosphatide; With
(n) mixture of any aforementioned component.
Particularly preferred beneficial agent is a siloxanes, and preferably its viscosity is greater than the siloxanes of about 10000 centipoises.Siloxanes can be gummy and/or it can be a mixture of siloxanes.An one example is the polydimethylsiloxane of about 30000 centipoises of viscosity.
(f) water
At last, as mentioned above, another crucial part of the present invention is to use the water of low levels, i.e. 2-10% weight, preferably 2-8% weight, more preferably 3-7% weight.The purpose that keeps low water content is in order to guarantee that but a kind of the cooling forms hard solid isotropy pumping melt.Excessive water can cause occurring in the melt being separated, and obtains obsolete soft solid when cooling.
Because water-content is so low, therefore importantly, the content of many alcohol and water is preferably greater than 3.5: 1, more preferably greater than 4: 1 than at least about 3: 1.That is, the low-molecular-weight polyol that is in the great majority by use (many alcohol of alkylidene group or the many alcohol of the alkylidene group content that adds beneficial agent and PAG than at least about 0.8: 1) as previously mentioned, but be enough to guarantee the said composition pumping.
The present invention comprises that also use wax is as the lipid acid surrogate.Wax preferably accounts for the 1-10% of bar compositions weight, more preferably 2-5%.
The example of operable wax comprises paraffin (fusing point is 45-70 ℃).
Unless refer else, above-mentioned all percentage ratios all by weight.
Following examples only are used to illustrate the present invention, in any case therefore can not be in order to limit claim.
Embodiment
Raw material
Coconut acyl group sodium isethionate is supplied by Lever Hammond.Polyoxyethylene glycol is supplied by UnionCarbide.AMPHORAM C30 and Tego Care (stearin) are supplied by Goldschmidt.Palmitinic acid/stearic acid is supplied by Emery.Polydimethylsiloxane is supplied by General Electric.Propylene glycol is supplied by Fisher.Paraffin is by Moore﹠amp; MungerMarketing Inc. supply.
Preparation steps (founding)
Bar prepares by fusion casting.At first, under 80-120 ℃, in 500 ml beakers, each component is mixed, then water-content is adjusted to about 10-15% weight.Cover batching, in case moisture loss mixed about 15 minutes then.Remove lid, allow the mixture drying.In drying process, in different time, take a sample, use the turbine titration apparatus then, by Karl Fisher titration measuring water-content.When reaching final water-content (～5%), pour the mixture in the beaker (free-pouring liquid form) into soap dye, the room temperature cooling is 4 hours then.By solidifying, can in soap dye, this mixture be molded as bar.
Method
The zein test
In 8 ounces of jars, prepare 30 milliliters of the aqueous dispersions of bar prescription 2.0%.This dispersion liquid is placed in 45 ℃ of baths up to dissolving fully.Balance adds 1.50 gram zeins in every kind of solution during to room temperature, stirs 1 hour fast simultaneously.Solution is transferred in the centrifuge tube, then under the speed of about 3000rpm, centrifugal treating 30 minutes.Isolate not molten zein, rinsing is dried to constant weight then in 60 ℃ vacuum oven.By gravimetric determination zein dissolved percentage ratio, this value is directly proportional with pungency.
The test of gelatinization value
Bar is placed in the vinyl disc, adds 25 ml waters, measure bar gelatinization value then.Cover dish, keep not touching reaching 24 hours.Scrape gently with scraper then and stick with paste layer, weigh, then with commercially available Dove
(R)Bar compares.
The wear rate test
The pottle container is placed under 105 the mobile tap water.Hand and test bar were immersed in the water 3 seconds.Take out, then bar is rotated in hand 10 times.Repeat this step, finally once bar is immersed in the water, be stored in then in the flat soap box that contains 7.5 ml waters.This washing procedure carried out 4 times in first day, second day 4 times.This bar dried overnight calculates the average gram number (two bars) of each washing loss then, notes.
Measure by the siloxanes that FTIR carries out
In the Nicolet 5SXB FTIR spectrograph of being furnished with horizontal decay specular reflectance included (ATR) annex, collect infrared spectra.The ATR element is the 60ZnSe crystal on 7 centimetres of sampling surfaces of 1 cm x.Along plane of crystal, smear the bar sample.Then at 8cm
-1Under the resolving power, collect spectrum; Scan 32 times, be averaged.At 800cm
-1Compare siloxanes average peak amplitude down, estimate the relative different on the PDMS concentration.
The external deposition scraping pigskin of siloxanes stays dermatome, is cut into 25 square centimeters thin slice then before processing.With the front and back mode of motion, with rub this skin 10 times of bar sample, to handle this skin sample.The liquid that produces foamed 30 seconds, then with the water rinse 10 seconds that is adjusted to 90-95.The skin sample of handling is put into the borosilicate scintillation vial that contains 10 milliliters of dimethylbenzene.Sample is placed in the platform electromagnetic shaker 1 hour to extract siloxanes.After leaching process, from pipe, take out skin, analyze extracting solution to determine content of siloxane by graphite furnace atomic absorption spectrometry then.At 10ppm siloxanes standard, specimen solution.
Embodiment 1
Prepare bar with following prescription.
| Table 1: melt-cast formulation | |||
| Component | ??????1 | ??????2 | |
| ????1 | Coconut acyl group sodium isethionate | ????28.5 | ????28.5 |
| ????2 | AMPHORAM C30 | ????5.0 | ????5.0 |
| ????3 | Sodium stearate | ????20.0 | ????15.0 |
| ????4 | Polyoxyethylene glycol 8000 | ????5.0 | ????10.0 |
| ????5 | Palmitinic acid/stearic acid | ????13.1 | ????13.1 |
| ????6 | Paraffinic waxes | ????3.0 | ????3.0 |
| Foreign material (as salt) | ????1.4 | ????1.4 | |
| ????7 | Propylene glycol | ????18.3 | ????18.3 |
| ????8 | Water | ????5.7 | ????5.7 |
Prepare this bar according to following steps:
(1) adds component 4-7, be heated to 90 ℃ under stirring then;
(2) add component 3 and dissolving, add component 2 and 8 then;
(3) in case form isotropic mixture, adding component 1 and dissolving;
(4) in a single day form isotropy hot melt material, just prepare, pour in the mould then.
Should be noted that order is not crucial, other multiple possibility is arranged.
Acceptable paste value of embodiment 2-and wear rate
Under about 90 ℃, bar 1 and 2 all forms the relative low isotropy melt of viscosity.These hot solution were at 20 seconds
-1Under about 1000 centipoises of viscosity.When discovery prepared in the combined packet installation, they were easy to be pumped in the mould.The gained bar foams functional, and after dipping was also swiped in 24 hours gently in water, has the Dove of ratio
(R)(about 12.0) will be low the paste value, that is, about 6.6 grams stick with paste (bar 1) and 4.4 grams are stuck with paste (bar 2).This bar has about 2.8 grams (bar 1) of each washing and 2.4 and restrains (bar 2) and (equal Dove in addition
(R)) than low consumption speed.Consider the liquid component (that is, water and polyvalent alcohol) that contains higher percentages in these bars, these numerical value are wonderful.Therefore as can be seen, by founding, can when adding the high amount of liquid composition, prepare the second best in quality bar.
Embodiment 3-low irritant
At first test and estimate the stimulation performance of filling a prescription to found that about 20% zein dissolves by zein.Dissolve zein than commercially available Dove
(R)The dissolving of bar will lack about 100%.This shows that pungency is reduced.
Embodiment 4-adds siloxanes in base composition
The applicant tries to find out, soothing oil (being specially the 60000cst polydimethylsiloxane) from selected melt-cast formulation, deposit on the skin degree how.It should be noted that owing to following 2 reasons, and use casting technology in washing process, to carry these oil:
1. substitute its liquid portion by part, soothing oil is easy to add in the cast melt bar thing.
2. compare with extrusion process, these oily discrete liquids are bigger, are easier to remain in the bar matrix.
About first point, when with excessive 1%, particularly excessive 3-4% directly adds soothing oil, and during as siloxanes or mineral oil, conventional synthetic detergent bar is often rapidly softening, makes to be difficult to maybe can not carry out extrusion process.
According to the prescription in the table 12, the PDMS with 5%, 7.5% and 10% partly substitutes propylene glycol (being respectively prescription 3,4 and 5, following table 2).
| Table 2: the prescription that comprises polydimethylsiloxane | |||
| ??????3 | ?????4 | ?????4 | |
| Coconut acyl group sodium isethionate | ????28.5 | ????28.5 | ????28.5 |
| The coconut amido betaines | ????5.0 | ????5.0 | ????5.0 |
| Sodium stearate | ????10.0 | ????10.0 | ????10.0 |
| Polyoxyethylene glycol 8000 | ????10.00 | ????10.0 | ????10.0 |
| Palmitinic acid/stearic acid | ????14.5 | ????14.5 | ????14.5 |
| Paraffinic waxes | ????3.0 | ????3.0 | ????3.0 |
| Stearin (Tego Care) | ????5.0 | ????5.0 | ????5.0 |
| Propylene glycol | ????13.3 | ????10.8 | ????8.3 |
| Water | ????5.7 | ????5.7 | ????5.7 |
| Polydimethylsiloxane | ????5.0 | ????7.5 | ????10.0 |
PDMS it seems by stirring and is evenly dispersed in the melt.
In case pour into and cool off, need to measure the extent of migration of PDMS in bar matrix.Used time of cooling step can sufficiently long, so that the siloxanes cohesion floats on the bar surface then.In order to test, use the scalper cutting to comprise the bar of 7.5%PDMS.Take out sample from the upper and lower, left and right and the center of bar.On the Ze-Se of Nicolet FTIR crystal, smear then.Note the absorption spectrum (800cm of Si-O band
-1), the result shows that siloxanes is evenly distributed in the bar.Specifically, the consistence of peak height represents that siloxanes is not obviously migration in cooling step, distributes but evenly remain in the bar.
Embodiment 5-deposition
The deposition of PDMS on skin
Carry out external deposition on pigskin, determine PDMS and deposit to degree on the pigskin by prescription 3 (5%PDMS), 4 (7.5%PDMS) and 5 (10%PDMS), contrast with routine washing bar, the result provides in following table.
| The deposition of polydimethylsiloxane on pigskin | ||||
| ?Dove (R)* | Lux (R)* | Embodiment 3 (5%PDMS) ω | Embodiment 4 (7.5%PDMS) ω | Embodiment 5 (10%PDMS) ω |
| ??0.25 | ??0.25 | ????1.6 | ??????2.1 | ??????8.5 |
Microgram/square centimeter.
*Use common process (non-founding), 5%PDMS is dispersed in the conventional bar.
ωPDMS is used for cast melt bar thing technology.
The sedimentation of melt-cast formulation of the present invention is apparently higher than the conventional bar (Dove that wherein simply disperses 5%PDMS
(R)And Lux
(R)).
Claims (11)
1. cast melt bar compositions wherein comprises:
(a) the synthetic nonsoap detergent of 10-40% weight or the mixture of synthetic nonsoap detergent;
(b) polyhydric alcohol composition of 10-50% weight, this polyhydric alcohol composition comprises the mixture of following material:
(i) about 2000-20000 of molecular weight and the about 55-65 of fusing point ℃ polyalkylene glycol; With
(ii) under the room temperature C of liquid
2-C
4How pure alkylidene group is; Wherein the many alcohol of this alkylidene group add that with the ratio or the many alcohol of this alkylidene group of polyalkylene glycol the weight ratio of following component (e) beneficial agent and polyalkylene glycol is about 0.8: 1 or higher;
(c) the water-soluble structure agent of 5-40% is selected from C
8-C
24Lipid acid and C
8-C
20Alkanol;
(d) about soap of-20% weight more than 8;
(e) beneficial agent of 0-30% weight; With
(f) water of 2-less than 10% weight;
The weight ratio of wherein total polyvalent alcohol (b) and water is at least about 3.1.
2. according to the composition of claim 1, wherein the molecular weight of polyalkylene glycol is about 4000-10000.
3. according to the composition of claim 1, wherein said polyalkylene glycol has following structure:
R wherein
1=hydrogen atom, C
1-C
4Alkyl;
R
2=hydrogen atom, CH
3And
The about 40-200 of n=.
4. according to the composition of claim 1, wherein said alkyl polyols is selected from C
2-C
4Aklylene glycol and glycerine.
5. according to the composition of claim 1, wherein said lipid acid accounts for the 10-25% of composition weight.
6. according to the composition of claim 1, wherein said lipid acid is the saturated C of straight chain
12-C
14Lipid acid.
7. according to the composition of claim 1, wherein said alkanol is a hexadecanol.
8. according to the composition of claim 1, it also comprises the soap of 10-20% weight at least.
9. according to the composition of claim 1, wherein the weight ratio of polyvalent alcohol (b) and water (f) was at least about 3.5: 1.
10. according to the composition of claim 9, wherein polyvalent alcohol (b) was at least about 4: 1 with the weight ratio of water (f).
11. according to the composition of claim 1, it also comprises the wax of 1-10% weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97180669 CN1240474A (en) | 1996-10-16 | 1997-10-01 | Pourable cast melt bar compositions comprising low levels of water and minium ratios of polyol to water |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US08/733,036 | 1996-10-16 | ||
| CN 97180669 CN1240474A (en) | 1996-10-16 | 1997-10-01 | Pourable cast melt bar compositions comprising low levels of water and minium ratios of polyol to water |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1240474A true CN1240474A (en) | 2000-01-05 |
Family
ID=5177801
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 97180669 Pending CN1240474A (en) | 1996-10-16 | 1997-10-01 | Pourable cast melt bar compositions comprising low levels of water and minium ratios of polyol to water |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1240474A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106459334A (en) * | 2015-05-08 | 2017-02-22 | 三悠瑞克株式会社 | Polyol composition for producing polyurethane resin composition |
| CN111164194A (en) * | 2017-10-05 | 2020-05-15 | 路博润先进材料公司 | Structured unit dose cleaning products |
-
1997
- 1997-10-01 CN CN 97180669 patent/CN1240474A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106459334A (en) * | 2015-05-08 | 2017-02-22 | 三悠瑞克株式会社 | Polyol composition for producing polyurethane resin composition |
| CN106459334B (en) * | 2015-05-08 | 2018-06-12 | 三悠瑞克株式会社 | Polyurethane resin composition manufacture glycol composition |
| CN111164194A (en) * | 2017-10-05 | 2020-05-15 | 路博润先进材料公司 | Structured unit dose cleaning products |
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