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1. CA2064483 - COMPOSES D'AMMONIUM, METHODE DE PREPARATION CONNEXE ET UTILISATION DE CES DERNIERS COMME AGENTS DE NETTOYAGE, SUBSTANCES COSMETIQUES DE BASE ET AGENTS ADOUCISSANTS, ET PARTICULIEREMENT COMME ASSOUPLISSEURS DE TISSUS

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[ EN ]
Novel ammonium compounds preparation thereof and use thereof as cleaninq aqent, cosmetic raw material and softener, in particular as final-r:inse fabric softener
The present invention relates to novel ammonium compounds, processes for preparing them and the use thereof as cleaning agent, cosmetic raw material and softener, in particular as final-rinse fabric softener.
In the washing of textiles it is customary to employ in the last wash cycle fabric softeners in order that harshening of the fabrics by drying may be avoided and the fabric hand of the treated textiles may be positively influenced.
The final-rinse fabric softeners used are customarily cationic compounds, for example quaternary ammonium compounds which in addition to long-chain alkyl radicals may also contain ester or amide groups. It is also advantageous to use mixtures of different softening components which are added to the rinse bath in the form of aqueous dispersions.
These cationic compounds are effective softeners when used in the final-rinse bath, but they do have some disadvantages in use.
One of the disadvantages of such agents is that the softener components are not dispersible in cold water; another is that the textiles treated therewith possess unsatisfactory remoisture capability.
Remoisture capability for the purposes of the present invention is the ability of the fiber to reabsorb moisture. Inadequate remoi~ture capability i5 a disadvantage whenever major quantities of moisture are to be absorbed from the surface of the skin, for example in the case of hand and bath towels, underwear and bed linen.
It is an object of the present invention to overcome the abovementioned disadvantages of conventional final-rinse fabric softening formulations and to make available highly concentrated final-rinse fabric softeners which combine ready biodegradability and a soft fabric hand with significantly improved dispersibility or solubility even in cold water and improved remoisture capability.
It has been found, surprisingly, that final-rinse fabric softeners comprising mixtures of quaternary ammonium compounds with or without ester groups that are preparable by quaternization or by protonation with inorganic or organic acids not only meet these requirements but give clear solutions in cold water even in high concentrations of up to about 30% by weight.
The present invention accordingly provided ammonium compounds of the general formula (1)
R2~ CH2)~-~-(Rqst- C-R~-C-(R6)~-Y-(CHz)~-~-R7l .~~ B-
where
R1 = identically or differently H, -CH3, -C2H5, -(C3H50)ClH, -(C2H40)C2H
R2, R3, R7, R8 = identically or di:Eferently a straight chain or branched alkyl or alkylene radical of 1-18 carbon atoms
R , R = -(CH2-CHR9-0)~-(CH2-CHRl-O)b- where R9Rl0 =
H or -CH3, a, b = identically or differently 0-10
R5 = radical of the dimerized fatty acid x, y z 0 and/or NH
A-B- = identically or differently the anion of a water-soluble monobasic or polybasic inorganic or organic acid such as methylsulfuric acid, ethylsulfuric acid, a halohydric acid, phosphoric acid, formic acid, acetic acid, oxalic acid, glycolic acid, citric acid, tartaric acid, malic acid and in particular hydrochloric acid and lactic acid and the total number of negative charges in the molecule is equal to the total number of positive charges k, n - identically or differently 2-4
Cl, C2 = identically or differently 1-5 l, m = identically or differently 0 or 1 with l - 0 when x - NH and m = 0 when y = NH.
The present invention further provides aqueous final-rinse fabric softeners comprising
A) from 5 to 30% by weight of at least one of the compounds of the general formula 1
R2-l-(CH2)~-~-(R4)l- c-R3-c-(R6)m-~-(rH2)n-l-R~ - BR1 = identically or differently H, -CH3, -C2H5,
- ( C3H50 ) ClH, - ( C2H40 ) C2H
R2, R3, R7, R3 = identically or differently a straightchain or branched alkyl or alkylene radical of 1-18 carbon atoms
R, R = -(CH2-CHR9-O)A-(CH2-CHR1-O)b- where R9Rl0 =
H or -CH3, a, b = identically or differently 0-10
R5 = radical of the dimerized fatty acid x, y = 0 and/or NH
A-B- = identically or differently the anion of a water-soluble monobasic or polybasic inorganic or organic acid such as methylsulfuric acid, ethylsulfuric acid, a halohydric acid, phosphoric acid, formic acid, acetic acid, oxalic acid, glycolic acid, citric acid, tartaric acid, malic acid and in particular hydrochloric acid and lactic acid and the total number of negative charges in the molecule is equal to the total number of positive charges k, n = identically or differently 2-4
C1, Cz = identically or differently 1-5 1, m = identically or differently 0 or 1 with 1 = 0 when x = NH and m = 0 when y = NH and to 100% by weight
B) water, dyes, perfume, thickeners and customary auxiliary and additive substances.
According to the invention, preference is given to using compounds of the general formula 1 where
Rl is identically or differently H or -CH3, RZ1 3- 7- 8 iS the methyl radical,
R5 is the radical of the dimerized fatty acid having a dimer content of 2 80% by weight, k, n = 2 or 3, 1 and m = 0 and A- and B- are identically or differently the lactate radical or the methosulfate radical.
The compounds of the general formula 1 used according to the present invention are prepared in a conventional manner, in general by esterifying or amidating the prim./tert. amine or the alkanolamine in the presence of acid catalysts such as methanesulfonic acid or hypophosphorous acid under nitrogen at 140-200C and continuously distilling off the resulting condensate, if necessary under reduced pressure in the final stage.
Instead of the fatty acids it i8 also possible to use their esters.
The dimeric fatty acids used for preparing the compounds according to the present invention are the commercially available products which are prepared by polymerization of saturated or unsaturated natural or synthetic monobasic aliphatic fatty acids of 16-22 carbon atoms by known methods (cf. US Patent 2,482,761, US
Patent 3,256,304). Typical commercially available dimeric fatty acids have approximately the following composition: monomeric acids 0 - 15% by weight dimeric acids 60 - 95% by weight trimerized acids and higher polymers 1 - 35% by weight the content varying within these limits depending on the origin of the monomers, of the polymerization process and of the workup process.
The dimeric fatty acid used can also be present in hydrogenated form.
The dimeric acid content can be raised as far as 100% by weight by generally known distillation methods.
The dimeric acid content is determined by the known methods of gas liquid chromatography (GLC).
If distilled dimeric fatty acid is used, the products obtained have an improved color number. On the other hand, it is perfectly possible to use commercial technical-grade polymerized fatty acid for the preparation. If technical-grade dimeric fatty acid is used, it should be pointed out that relatively high trimeric fatty acid contents may result in products having a poorer color number and higher viscosities. This depends on the particular level of dimeric and monomeric fatty acid in the polymerized fatty acid, and the desired values can be determined in a few simple exploratory experiments of the kind which are within the compass of the everyday workmanlike routine of a person of average skill in the art. If desired, it is also possible according to the invention to use the distillation residues from the distillation of the dimerized fatty acids alone or mixed with commercially available dimeric fatty acids. These distillation residues generally have approximately the following composition: monomeric acids:0 - 1% by weight dimeric acids:15 - 25% by weight trimeric and higher polymeric acids:75 - 85% by weight
However, preference is given to distilled dimeric fatty acid having a dimeric fatty acid content of 80-96%.
The alkanolamines or amines with primary and tertiary amine groups in the molecule used according to the present invention are commercially available products of the general formulae 2a and 2b
R2, R3-N-(CH2)2-oH (2a)
R2, R3-N-(CH2)3-NH2 (2b) where R2 and R3 are each as defined above, but preferably have alkyl radicals of 1-4 carbon atoms and according to the invention are preferably methyl or ethyl radicals.
The compounds of the formula 2a can be alkoxylated, i.e. preferably - according to the invention - ethoxylated, in a conventional manner. In general this is done by reacting the amines in a pre6sure reactor at 120-160C, in the presence or absence of basic, in particular alkaline, catalysts, at 1-4 bar with an amount of alkylene oxide, preferably according to the present invention ethylene oxide and propylene oxide or mixtures thereof, corresponding to the desired degree of alkoxylation.
The products obtained are compounds of the general formula 2c
R2,R3-N-(CH2) 2-- ( CH2-CH2- ) ~- ( CH2CHR1- ) bH where a, b = 0-10 (2c) and a + b 2 1The compounds used according to the presentinvention can be protonated with organic or inorganic acids in a conventional manner. This i9 preferably done by adding the aqueous protonic acid with or without a solvent, for example a short-chain alcohol, to the reaction mixture with intensive stirring.
Examples of the organic acids used are formic acid, acetic acid, methylsulfuric acid, ethylsulfuric acid, in particular lactic acid, malic acid, tartaric acid, citric acid, oxalic acid, glycolic acid; inorganic acids such as halohydric acids, in particular hydochloric acid, sulfuric acid, phosphoric acid. Preference according to the present invention is given to lactic acid and hydrochloric acid.
Examples of the quaternizing agents used are short-chain dialkyl phosphates and sulfates such as, in particular, dimethyl sulfate, dimethyl carbonate, diethyl sulfate, dimethyl phosphate, diethyl phosphate, shortchain halohydrocarbons, in particular methyl chloride.
The quaternization is effected in a conventional manner. Preference according to the present invention is given to admixing the molten substance, in the presence or absence of a solvent, preferably a short-chain alcohol such as isopropanol, at 60-90C with equimolar amounts of the quaternizing agent with stirring, under atmospheric or superatmospheric pressure, and following the progress of the reaction by monitoring the total amine number (TOT).
By using the compounds according to the present invention it is possible to prepare final-rinse fabric softeners which give clear solutions even in cold water in concentrations of up to about 25-30% by weight, based on total mixture, and confer on textile materials, in particular those made of natural and regenerated cellulose and also wool and terry, not only a soft fabric hand but also excellent remoisture capability.
The final-rinse fabric softeners according to the present invention are therefore used not only on the usual textile materials but in particular wherever large amounts of wetness and moisture are to be removed from the body surface within a short time, such as on hand and bath towels. But the final-rinse fabric softeners according to the present invention are also successfully usable where moisture has to be absorbed directly from the skin within longer time spans, such as on underwear or bed linen.
The final-rinse fabric softener concentrates are prepared by dissolving the particular individual components in water. This can be done using the procedures for dispersions customary in this field, but there is no need for the otherwise necessary heating of the water or the active ingredient.
The customary procedure for doing this comprises adding with thorough stirring to the initially charged water at room temperature first the dye solution, then the antifoam emulsion which may be necessary and then the active ingredient according to the present invention. If necessary, the customary auxiliary and additive substances and perfume oils can likewise be added. They are in particular complexing agents, optical brighteners, dyes, scents, electrolytes and higher molecular weight ether compounds for viscosity regulation, small amounts of organic solvents and - provided they have no adverse effect on the remoisture capability - customary surfactants. If necessary the pH is adjusted to about 3-5 with the inorganic or organic acids customary in this field, in particular HCl, H3P04, H2S04, lactic acid or citric acid. ike the prior art fabric softeners, the fabric softeners according to the present invention are added to the final-rinse cycle immediately following the actual washing process. The concentration after dilution with water varies with the field of application within the range from 0.1 to 10 g of fabric softener per liter of treatment liquor.
The concentrates obtained with an active ingredient content of up to about 30% by weight, based on the total recipe, are clear solutions of low viscosity which, in addition to having the abovementioned advantages, are markedly easy to disperse in the rinse water of the washing machines.
To assess the fabric hand, the textile material, made of wool, cotton, 50:3 polyester/cotton and polyester, is treated for about 10 minutes with a liquor comprising tap water (about 9 German hardness and a temperature of 15-20C) and the novel dispersion. The concentration of the compounds according to the present invention in the liquor is 0.025% by weight, based on the total active ingredient. The dried textiles were checked by nine people with experience in the assessment of the softness of textiles in respect of their soft fabric hand and assessed against textiles which had either not been treated with fabric softeners or which had been treated with a commercially available fabric softener. The assessments are rated according to a graduated points system, the final reported result being the arithmetic averge. After drying, the textile material thus treated has an excellent soft fluffy fabric hand, and compared with commercially available agents, a much improved remoisture capability.
The remoisture capability is measured on the lines of German Standard Specification DIN 53 924, except that the strips of fabric (test pieces) are 1.5 cm in width.
Aside from their use in final-rinse fabric softeners the compounds according to the present invention can be used with success in hair and body care agents, in household and industrial cleaning agents and also in textile auxiliaries, in particular as softener/ hand finish with hydrophilizing properties and high substantivity for the final finish of textiles.
In the examples which follow, the abbreviations used have the following meaning:
AN = acid number
TOT = total amine number
TERT = tertiary amine number
Cat. S03 = cationic substance.
These analytical values are determined by the following methods generally customary in thiY field:
Acid number (AN)
The acid number is a measure of the free acid content of a fat or technical-grade fatty acid and indicates the milligrams of potassium hydroxide which are necessary for neutralizing 1 gram of substance.
The values are determined by DGF (German Society for Fat Chemistry) standard method C-V4.
Cationics content (Cat. S03)
This method is used for determining the level of cationic substances. were the cationic substances are long-chain compounds which contain quaternary ammonium groups. The content is reported in % of quaternary compound calculated as S03 equivalent with a molecular weight of 80 g/mol.
It is determined by a two-phase titration as described in ISO standards 2871-1 and 2871-2 (1988 E).
Dry matter content
It is determined by heating and drying at 105C to constant weight.
Total amine number (TOT), tertiar,v amine number (TERT)
The total amine number indicates the number of milligrams of potassium hydroxide which are equivalent to the total amine basicity of 1 g of the amine compound (mg of KOHtg). The tertiary amine number indicates the number of milligrams of potassium hydroxide which are equivalent to the tertiary amine basicity of 1 g of the amine compound.
The values are determined by American Oil
Chemists Society (A.O.C.S.) Official Method TF 2a - 64.
Preparation of compounds according to the invention
Example 1
To l,150 g (2.03 mol; MW 566 g/mol) of dimer fatty acid D 96 are added 450 g (5.06 mol) of dimethylethanolamine and after addition of 2.3 g (0.2%) of hypophosphorous acid and 1.15 g (0.1%) of methanesulfonic acid the batch is heated to 180C under N2. The water of reaction is gradually distilled off through a column.
After the reaction has ended (about 12 h), the excess dimethylethanolamine is distilled off in vacuo at 180C and 12 mbar.
Analytical data: acid number 2.8
TOT 148
TERT 147
Example 2 386 g (0.5 mol) of dimer fatty acid diester as per Example 1 are mixed with 150 g of isopropanol and quaternized with 147 g (1.17 mol) of dimethyl sulfate at 70C under N2 until the TOT is less than 4.
Analytical data: DS 80%
TOT 2.6
Cat. S03 acid 12.4
Example 3
A solution of 465 g (0.61 mol) of dimer fatty acid diester as per Example 1 in 50 g of isopropanol is neutralized by the gradual dropwise addition of 121 g (1.2 mol) of lactic acid 90% at 50C by thorough stirring under N2-
nalytical data: DS 82.8%TOT 108
ExamDle 4
A solution of 850 g (1.1 mol) of dimer fatty acid diester as per Example 1 in 110 g of isopropanol is quaternized at 60C under N2 with 138 g (1.1 mol) of dimethyl sulfate. Then the mixture is neutralized by the gradual dropwise addition of 114 g tl.l mol) of lactic acid 90% by thorough stirring under N2.
Analytical data: DS 87%
TOT 53
Cat. S03 acid 14.9
Example 5
To 1,530 g (2.64 mol; MW 580 g/mol) of dimer fatty acid D 96 are added 3 g (0.2%) of hypophosphorous acid, followed by 650 g (6.4 mol) of dimethylaminopropylamine, and the batch is heated to 180C under N2. The water of reaction is gradually distilled off through a column. After the reaction has ended (about 4 h), the excess amine is distilled off in vacuo at 180C and 12 mbar.
Analytical data: acid number 0.7
TOT 157
TERT 156
Example 6 500 g (0.66 mol; MM 748 g/mol) of dimer fatty acid diamide as per Example 5 are admixed with 165 g of 1,2-propylene glycol and then quaternized under N2 at 70C with 171 g (1.35 mol)ofdimethylsulfateuntiltheTOT ~ 3.
Analytical data: DS 82.2%
TOT 1.5
Cat. S03 acid 12.0
Example 7
A solution of 810 g (1.1 mol) of dimer fatty acid diamide as per Example 5 in 250 g of 1,2-propylene glycol is quaternized at 60C with 143 g (1.1 mol) of dimethyl sulfate under N2. The batch is then neutralized by the gradual dropwise addition of 113 g (1.1 mol) of lactic acid 90% by thorough stirring under N2.
Analytical data: DS 79%
TOT 47
Cat. S03 acid 13
Example 8
A solution of 530 g (0.75 mol; MM 714 g/mol) of dimer fatty acid diamide as per Example 5 in 170 g of 1,2-propylene glycol is neutralized with 150 g (1.5 mol) of lactic acid 90% at 50C under N2.
Analytical data: DS 71.2%
TOT 95
Example 9
To 540 g (0.75 mol; MW 725 g/mol) of dimer fatty acid diester as per Example 1 are gradually added dropwise at 180C under N276.5 g (0.75 mol) of dimethylaminopropylamine in the course of 2 h. After a further 4 h the liberated dimethylethanolamine i~ distilled off in vacuo at 12 mbar and 180C. nalytical data: AN 2.0
TOT 151
Example 10 740 g (1.0 mol; MW 740 g/mol) of dimer fatty acid ester-amide as per Example 9 is admixed with 170 g of isopropanol and then quaternized under N2 at 70C with 249 g tl.94 mol) of dimethyl sulfate.
Analytical data: DS 85%
TOT 1.8
Cat. S03 13.2
Example 11
A solution of 740 g (1 mol) of dimer fatty acid ester-amide as per Example 9 in 80 g of isopropanol is neutralized by the gradual dropwise addition of 200 g (2 mol) of lactic acid 90~ at 50C by thorough stirring under N2 Analytical data: DS 85.2%
TOT 112
Example 12
A solution of 740 g (1 mol) of dimer fatty acid ester-amide as per Example 9 in 160 g of isopropanol is quaternized at 60C with 126 g (1 mol) of dimethyl sulfate under N2. Then the mixture i8 neutralized by the gradual dropwise addition of 100 g (1 mol) of lactic acid 90% by thorough stirring under Nz.
Analytical data: DS 83%
TOT 5 0
Cat. SO3 acid 13.3
Application testinq
Application testing was carried out according to the test methods customary in this field as follows:
Preparation of final-rinse fabric softener
The examples listed below in the table were prepared as follows:
To tap water of 9 German hardness at 20C were added with thorough stirring 0.625 g of SANDOLANR milling blue NBL-150 1~ (from Sandoz), 0.250 g of DOW antifoam
DB-lOA (from DOW Chemicals) and then the amount specified in the examples of substance according to the present invention i9 dissolved therein. Thereafter the batch was adjusted if necessary to about pH 3 with HCl in the case of the quaternary compounds and with lactic acid in the case of the salts.
Verification of remoisture capability and soft hand
Test fabric: standard milling terry fabric 100% cotton size: 80 x 50 cm from Mowe, Reutlingen 3 kg of the test fabric were washed 2 times with 100 g each time of detergent (test detergent from
WFK-Testgewebe GmbH Krefeld) and then twice without detergent (each time by the 95C wash program without prewash).
The test fabrics dried at room temperature were then dipped into the fabric softener solution containing 0.025% by weight of compound according to the present invention or of commercial fabric softener in tap water of 9 German hardness 15-20C for 10 min.
The fabrics dried at room temperature were rated by 9 test persons in respect of their softness. They were assigned ratings on a scale from 0 to 5, where 0 means harsh and 5 means very soft = good. The final assessment is the arithmetic average.
The remoisture capability was measured on the lines of German Standard Specification DIN 53 924, except that the strips of the test pieces are 1.5 cm in width.
Final-rinse fabric softener
Component according to the invention
Example Assessment Remoisture Soft as per Amount per capability hand
Example 100 g of total mixture 1 2 31 g clear solution of lOOX good low viscosity 2 2 6.3 g clear solution of lOOX good low viscosity 3 4 30.5 g clear solution of 100% good low viscosity 4 4 6 g clear solution of lOOZ good low viscosity 3 24.2 g clear solution of lOOX good low viscosity 6 6 31 g clear solution of 97Z good low viscosity 7 6 6 g clear solution of 97X good low viscosity 8 7 38 g clear solution of 98X good low viscosity 9 7 18.8 g clear solution of 98X good low viscosity 8 35.1 g clear solution of 97X good low viscosity 11 8 7 g clear solution of 97X good low viscosity 12a 10 29.3 g clear solution97X good 13A 10 6 g clear solution of 97X good low viscosity 14 12 28.5 g clear solution of lOOX good low viscosity 12 5.7 g clear solution of lOOZ good low viscosity
Component according to the invention
Example ~ AssessmentRemoisture Soft as per Amount per I Icapability hand
Example 100 g of mixture _
16 11 28.4 g clear solution of 99X Igood ! low viscosity 17 11 5.7 g clear solution of 99Z Igood low viscosity 18 2 37.1 g clear solution of 100% Igood l low viscosity 19 6 ~37.1 g clear solution of ¦ 97Z good low viscosity 7 1(30%) clear, thin ' 98Xgood solution
Comparative experiments i l sonb) dispersion 77Zgood 2 .~ 25.1 g dispersion , 77X' good 3 Com- 6.7 g dispersion ' 64X, very pari- ' good 4 ~ ~ ~ ~ fac _ component according to the invention preheated to 50C and incorporated at a water temperature of 40C ) - comparative experiment: commercially available quaternary ammonium compound (3-alkoxyloxy-2-hydroxypropyl)-trimethylammonium chloride ) - REUOQUATR W 90: quaternary imidazolinium derivative from
REUO Chemische Uerke, Steinau an der Strain.
The compounds according to the present invention can also be used with success in cosmetic recipes: in the hair care sector, depending on the recipe, not only for cleaning, i.e. as shampoo, but also for conditioning the hair to improve the combability.
Used in shampoos, they have the considerable advantage over conventional cationic compounds that they give clear solutions in water even in the presence of anionic surfactants, whereas prior art products give only dispersions. The advantage of solutions over dispersions in respect of storage life over a wide temperature range is known.
A further advantage is that the simultaneous presence of anionic and cationic compounds in a recipe makes this recipe not only cleaning but also conditioning .
In addition, these recipes accord with the modernview of a multipurpose agent, since they have a cleaning and conditioning effect not only on the hair but also on the skin. By using the compounds according to the present invention it is thus possible to meet the consumer's demand for body-hair care shampoos without problem.
The cosmetic formulations may additionally include the customary cosmetic surfactants, scents, preservatives, dyes, plant extracts or other cosmetic additives.
Suitable surfactants, besides the known betaines,
amphoteric and nonionic compounds, include for the cleaning recipes in particular anionic surfactants such as carboxylates, alkyl sulfates, alkyl ether sulfates, alkyl sulfonates, alkyl ether sulfonates, alkyl sulfosuccinates. According to the invention preference is given to alkylamidobetaines such as REWOTERICR 1) AM B 13 and AM B 14, carboxyglycinates such as REWOTERICR
AM 2 C NM, carboxypropionates such as REWOTERICR
AM KSF 40, sulfobetaines such as REWOTERICR AM CAS, anionic surfactants such as ether sulfate REWOPOLR 2)
NL 3, ether carboxylates such as REWOPOLR CLN 100, sulfosuccinates such as REWOPOLR SB FA 30, REWOPOLR SBZ,
REWODERMR 31 SPS ~ nonionic surfactants such as glycerol fatty acid ester ethoxylates such as REWODERMR ES 90, glycerol monostearate such as REWOMULR 4) MG, cetyl alcohol (1) 20 ~ 3)' 4~ = trademarks of REWO Chemische Werke
GmbH, Steinau an der Strain).
In addition to the compounds according to the present invention, which are used in amounts of 0.5-10 parts by weight, in particular 1-8 parts by weight, preferably 1-3 parts by weight, in the case of shampoo and 1-7 parts by weight, preferably 1-5 parts by weight, in the case of rinses and conditioners, the other surfactants are customarily used in amounts of 1-20 parts by weight, preferably 5-15 parts by weight, in shampoos and in amounts of 0.1-10 parts by weight, preferably 1-5 parts by weight, in rinses and conditioners.
The thickeners used are 1-8 parts by weight of the customary compounds such as glycerol fatty acid ester ethoxylates, fatty alcohol ethoxylates, fatty acid alkylolamides and the customary alkali metal, alkaline earth metal and ammonium salts which are soluble in water in amounts of at least 1% by weight at 20C, in particular NaCl, NH4Cl.
Cosmetic formulations
The following shampoos for body and hair can be produced by simply mixing the ingredients in water.
Recipe No. 1: Conditioning shampoo parts of REWOPOLR NL 3-28 parts of REWOTERICR AM KSF 402 2 parts of REWOMINOXR B 2043~ parts of Examples 6 and 10 according to the invention 0.3 part of citric acid 3.0 parts of sodium chloride ad 100 parts demineralized water
R = trademark of REWO Chem. Werke GmbH 1) = sodium lauryl ether sulfate 2) = amphoteric surfactant, salt-free 3) = alkylamidopropyldimethylamine oxide
Recipe No. 2: Conditioning shampoo parts of REWOPOLR NL 3-28 parts of REWOPOLR SB FA 304 2 parts of REWOMINOXR B 2043) 1.3 parts of Examples 6 and 10 according to the invention 0.1 part of citric acid 4.0 parts of sodium chloride ad 100 parts demineralized water 4) = fatty alcohol polyglycol ether sulfosuccinate
Recipe No. 6: Shower and hair shampoo with conditioning effect 1.5 parts of Example 2 according to the invention 2 parts of REWODERMR ES 906' 2 parts of REWODERMR LIS 75 parts of REWOTERICR AM B 13 parts of REWOPOLR) NL 3-281' 8 parts of REWOpoLR~ sBz12~ ad 100 parts demineralized water = fatty acid monoglyceride polyglycol ether, modif. = alkylamidobetaines 12~ = fatty acid polyglycol ester sulfosuccinate.
All the recipes were examined in respect of improvement in the ease of combing the hair and recipe 6 additionally in respect of the skin smoothness feel after showering. The tests were carried out by 10 experienced examiners, the final report result being the statistical average.
The ease of combing was rated for all the recipes as good with reduced comb resistance. The average values achieved on the scale from 1 to 7 were 4-7.
The feeling on the skin in the case of recipe 6 is assessed as creamily soft in the case of wet skin and as smoothly soft in the case of dry skin.
The following recipes were prepared as follows:
Recipe No. 3: Hair rinse, preparable cold 1.0 part of NATROSOLR 1) 250 HHR7 1.0 part of REWOQUATR RTM 505~ 2.0 parts of Examples 6 and 10 according to the invention 1.0 part of REWODERMR ES 906) 0.4 part of citric acid ad 100 parts demineralized water 5) = ricinoleic acid propylamidotrimethylammonium methosulfate 6) = fatty acid monoglyceride polyglycol ether 7) = hydroxyethylcellulose
R 1) = registered trademark of Aqualon
Recipe No. 4: Hair conditioner hase A: 5.5 parts of Examples 6 and 10 according to the invention 1.5 parts of cetyl alcohol 3.0 parts of REWOMULR MG9
Phase B: 2.0 parts of REWODERMR ES 906 2. a parts of REWOPOLR SB FA 304 0.2 part of citric acid 85.8 parts demineralized water = glycerol monostearate
Recipe No. 5: Hair rinse hase A: 3.0 parts of Example 10 according to the invention 1.0 part of cetyl alcohol 1-0 part of TEGINACIDR 2) 9)
hase B: 0.2 part of citric acid ad 100 parts demineralized water
R 2) = registered trademark of Goldschmidt = glycerol monostearate, acid-stable.
The hair rinse of recipe 3 is produced by preswelling NATROSOLR 250 HHR in demineralized water at room temperature and then adding the remaining components with intensive stirring. A clear solution of medium viscosity with a long storage life is obtained.
The hair rinse of recipe 5 and the hair conditioner of recipe 4 are prepared by preparing two phases A) and
B) separately in advance by respective mixing with heating to 65C and simultaneous thorough stirring and subsequently dispersing phase A) in phase B).
These recipes were examined in respect of wet and dry combability as specified above.
Not only the wet but also the dry combability scored the maximum attainable 10 points with the majority of testers. The statistical average was 8.
Evaluation scale: 1-3 difficult to comb 4-7 readily combable, hardly any resistance to comb 8-10 very readily combable, even less resistance to combing.