DD283027A7 - PROCESS FOR PRODUCING CONSISTENCY REGULATED EMULSIONS - Google Patents

Abstract

The invention relates to a process for the preparation of consistency-regulated emulsions. The invention relates to a process for the preparation of consistency-regulated emulsions for cosmetics, with which W / O and O / W emulsions of desired consistency and stability can be produced. The object was achieved by the fact that in the period of emulsion formation to completion of the preparation in the emulsion, an electroneutral compound in concentrations of 0.10 to 5% of suitable anion and cationic surfactants or organic high polymers carrying acidic or basic groups, or from Combinations of them are prepared with the ionic surfactants or added as a waerzrige dispersion. The invention can be applied in the fields of cosmetics, pharmacy and technical emulsions, where desired material-rich emulsions with the most diverse performance properties are desired. Emulsion, consistency-regulated; Electric Neutral connection; Cosmetic; surfactant; High polymer, ionic; dispersion}

Description

Field of application of the invention

The invention relates to a process for the preparation of consul-regulated emulsions for cosmetics.

Characteristic of the known technical solutions

Emulsions for cosmetics are complicated systems. They must meet a variety of special usage characteristics. They are therefore burdened with a wide variety of auxiliary and active substances that severely impair their consistency and stability. This is particularly evident in emulsion bases for hair dyes and hairdressing agents, which must either absorb large amounts of alkali, electrolytes, surfactants and dyes. Of all these additives is known that they can affect the stability and consistency of the emulsions even in low concentrations strong negative. Another problem is the thickening and so-called ripening of emulsions, which lead to difficulties in filling or require additional technological measures. The emulsions are ^dns: alb added for consistency regulate and stabilize various adjuvants. In O / W emulsions, they are usually fatty alcohols, glycerin fatty acid esters, spermaceti or synthetic esters of fatty alcohols and fatty acids; in W / O emulsions beeswax, paraffin, microcrystalline waxes or metal stearates.

That this task can be fulfilled for both types of emulsion by a Hiifsstoff, a co-emulsifier, which arises only in the emulsion production, is shown in DD-PS 228956 A3 and DD-PS 221922 A1, both a process for the preparation of co-emulsifiers in emulsion production. Thereafter, suitable anionic, cationic and nonionic surface-active compounds are mixed in such amounts at 60 to 110 ° C for up to minutes until the co-emulsifier in the molar ratio 1: 1: 2 could form.

In these processes for the formation of co-emulsifiers in the production of emulsions, however, relatively long mixing times or high temperatures and intensively operating stirring units are required, so that the expenditure of time, energy and apparatus equipment is high.

Object of the invention

It is the object of the invention to develop a process for the preparation of consistency-regulated emulsions, with which W / O emulsion and O / W emulsions can be prepared and which does not have the disadvantages of the known processes.

Explanation of the essence of the invention

The object was to develop a process for the preparation of consistency-regulated emulsions which is suitable for W / O and O / W emulsions, which allows work with energy-saving emulsification methods and manages with conventional, simple stirring units.

The object has been achieved according to the invention in such a way that in the period of emulsion formation to completion of the preparation of the emulsion an electroredeutic compound is added in concentrations of 0.10 to 5% as an aqueous dispersion or prepared in this period in the system by cation and anionic surfactants and / or organic high polymers bearing acidic or basic groups are brought together by known method steps with stirring. The emulsions produced in this way have a high viscosity, consistency and stability, which means that they can save considerable amounts of emulsifier and consistency-providing auxiliaries as compared with conventionally prepared emulsions. For the construction of the emulsions according to the invention, the usual emulsifiers and lipid combinations can be used, the Arboit for time and energy-saving emulsification,: t. The so-called "low-energy emulsification" is possible, and it can also be applied in slow-stirring anchor stirring works.Only surprisingly, these effects are only obtained if the electroneutral compound obtained by reaction from the anionic and cationic surfactants or the organic high polymers, the acidic or basic groups, or combinations of them with the ionic surfactants, is produced in the forming or finished emulsion or is added as an aqueous dispersion and does not exceed a concentration in the final emulsion of 5% This was not predictable because according to DE-AS 1147351 electron-neutral salts, which are obtained by reacting equimolar amounts of anionic compounds and cation-active quaternary ammonium compounds, Sognr al s sole ointment base have been proposed, which are known to have a firm, just spreadable consistency.

With the use ve ι Elektroneutralverbindungen obtained by equimolar precipitation of colloidal anionic ur d cationic electrolytes, for the production of technical emulsions of the textile, leather and Papierindus'rie is also already the DRP 668889. The cribed there production method is but not transferable to modern emulsification methods, it requires complex purification processes and leads to emulsions which are completely unsuitable for cosmetic purposes. Although the use of electroneutral compounds of anionic and cationic surfactants can certainly lead to interesting bases, as also DE-PS 972164 shows, no methods are known which could also have been implemented in practice and in the standard works of cosmetics and pharmacy Would have found input. The electroneutral compound can be prepared in the emulsion in various ways. Thus, it is possible to optionally add the anionic or cationic surfactant or the corresponding organic high polymer in the oil phase and the remaining Tonsid or ionic high polymers later emulsion add. It is also possible to add both surfactants or ionic high polymers at the same time the forming or finished emulsion to adjust these compounds at the expense of the required water phase to a certain concentration, they bring a jf a desired temperature, etc. Alone by this variation possibilities can inventive method can be easily adapted to the respective technological and equipment requirements. It is also possible to prepare the electroneutral compound per se as an aqueous dispersion and then to add it at a given time to the forming or finished emulsion. This is expediently carried out in such a way that Wosser and pin surfactant or one of the ionic high polymers are initially charged in a vessel and that each other is blended odor that the ionic surfactants and high polymers selected for the formation of the electroneutral compound, optionally with water to a certain concentration adjusted, immediately by correspondingly long stirring. Pumps or recirculation are merged and precipitated. The concentration of the dispersion of insoluble electroneutral compound and water thus prepared can be selected on a purely practical basis. It should be easy to pump, not sediment, retain its structure and, if necessary, remain homogeneously storable, so that not only a batch-wise work is possible. Concentrations of from 5 to 50% solids in the dispersion proved to be advantageous in the experiments carried out. The desired utility value of the finished product can be influenced both by the chosen time at which the dispersion is added or the electroneutral compound is prepared, as by the concentration of the anionic and cationic surfactants or organic high polymers carrying acidic or basic groups the formation of the electroneutral compound were selected. Is z. For example, if the emulsion has cooled sufficiently far that its consistency has increased strongly, it is very easy to incorporate air when mixing in a more turbid component and to create an inhomogeneous system.

If, however, in the temperature range of the melting point of the oily phase or at the beginning of the Ernulgierurig added the dispersion of the electroneutral or the electroneutral compound formed, it may happen that the consistency-regulating effects can not form optimally, since the desired structures are destroyed or do not form can.

In the process according to the invention, in principle, all known anion and cationic surfactants or organic high polymers which carry acidic or basic groups, or corresponding combinations, are suitable for the formation of the electron outbond compound. However, particularly advantageous for the anionic surfactants are carboxylic acids or their salts, alkylsulfonates, alkyl sulfates, alkyl ether sulfates, sulfosuccinic acid monoesters of fatty alcohols or fatty alcohol polyglycol ethers, acidic alkylphosphoric acid esters, condensation products of fatty acid halides with protein hydrolysates, sacrosin or methyltaurine, in which the alkyl radicals on which they are based have chain lengths of from C 10 to Have C22, saturated or unsaturated and the alkyl polyglycol ethers contain up to 8MoI EO, or acidic groups containing organic

High polymers, such as carboxymethyl cellulose or carboxymethyldextran proven. The cationic surfactants are preferably alkyltrimethyl-, dialkyldimethyl-, alkyldimethylbenzyl-, alkyldihydroxyethylmethyl- and alkyldipolyethoxymethylammonium halides or methosulfates or alkylpyridinium halides, in which the alkyl radicals on which they have chain lengths of C12 to CiO, saturated or unsaturated and the alkylamine polyglycol ethers up to 12 mol EO contain as well as basic groups containing organic high polymers, such as quaternized polyvinylpyrrolidone copolymers, Polydialkylammoniumchloride, with trimethyl quaternized hydroxycellulose or Epichlorhydrin quaternized with polyaminoamides and guar hydroxypropyltrimethylammonium chlorides.

The electro-neutral compound which can be used as aqueous dispersion can be prepared by mixing from the anion and cationic surfactants or the organic high polymers bearing acidic or basic groups or combinations of them with the ionic surfactants. Their concentration should not be higher than 500g / l.

The compounds mentioned can be used alone or in a mixture for the formation of the electroneutral compound.

The consistency control effect of the chosen electroneutral compound on the emulsion can be demonstrated by a simple experiment. The quantities are Ma .-%.

emulsion 1 2 3 4 ELN ELN ELN verb verb verb I Il III Alcohol, emulsific. non ionogeni, 2.ABd.DDR 4.00 5.00 5.50 4.00 Laurins.octanolester 5.00 5.00 5.00 5.00 ELN verb. each - - - 0.50 3 706 3840 2453 ELN verb. or - - 1.00 7 586 5900 3 203 ELN verb. or _ - _ 1.50 7210 8823 2 040 Water ad 100 100 100 100 Viscosity (mPas) 3200 3500 4363

If increasing amounts of an electroneutral compound are added to an emulsion in such a way that the proportions of the oil phase remain comparable, the influence on the consistency can be clearly recognized. By intensive mixing of appropriate amounts of stearyltrimethylammonium chloride in Lau. Ether / ether sulfate with 3EO was a 10% aqueous dispersion of the electroless neutral compound (ELN-Verb. I) Herge and added to the emulsion 4 at the end of the emulsification at 40 ° C. Already with 1.00% of the ELN verb. I has a maximum viscosity of more than twice that of the comparable emulsion (7588 to 3500 mPas). In the ELN verb. Il was replaced with the same procedure, the anionic surfactant against a entsorechendes alkyl sulfonate. Even with 1.50% of the ELN verb. Il the consistency maximum has not yet been reached. This & emulsions allow a significant reduction of the emulsifier content or are highly dilutable. If the anionic surfactant used is an oleic acid sarcosinate (ELN-Verb. III), the viscosity is reduced slightly. At the same time, the emulsions become more finely dispersed, creamier and more stable. Thus, by choosing and amount of the electroneutral compound in the same emulsion, the consistency can be adjusted differently. This has an extraordinary importance for technological matters, the filling and the use value of the emulsion.

embodiments

In the exemplary embodiments, the raw materials and auxiliaries are named by their chemical or pharmaceutical names. It goes without saying that in the production-wise implementation of the corresponding commercial products are used and the final products according to their intended use special active ingredients, perfume compositions, preservatives, dyes, etc. included. The mass information is in grams.

base emulsion

No. 12 3 4 5 6

Glycerinsor-

bitanoleate 2.00

Stearic acid 30.00

Myristic acid 10.00

stearic

ammonium glyceride 0.50

Ölsäuredi-

Ethanolaniid 2.50 0.30 1.50

Lanolin 0.80 1.00 0.30 1.80

Paraffinum

molle 4,00

Vaselire 8.00

Paraffimumsubl. 12,00

stearyl

+ 100ΕΌ 1.50 0.50 0.1C 1.50

Continued table

Base emulsion no.

Cholesterol 0.50

Cotylstearyl-

alcohol 14,00 5,00 5,00 8,00

Distearyldimelhylammo-

ammonium chloride 2.00

Palmitins.-

octanolester 3.50

Sunflower oil 2.00

ELN verb. 1.50 0.50 1.00 0.35 0.10 5.00

Glycerin 8.00 1.50

KOH "8.00

NaOH 1.52

Citric. 1.20

NH ₄ OH (22%) 7.42 4.50

1,2-propylene

glycol 5,00 3,50 2,50 2,00

Colorant shade 1.50 1.10 Water bath 100 100 100 10C 100 100

Emulsion base 1

is a cream hair color that can be produced by the "low energy emulsification technology." The emulsifiers are melted and emulsified with about 25% of the water phase of the same temperature, after which the rest of the water phase is added cold.The oxidation dyes are dissolved in 10% of the water phase. dissolved together the Propylenglykot and ammonia water with a reducing agent and added at 4O ⁰ C the emulsion. at the same temperature, the 15% dispersion of the electric neutral compound is introduced, which was prepared by one hour mixing the aqueous solutions of Stearyltrimethylammoniummethosulfat and Tetradecansulfonat in a separate container at room temperature The result is a final product that can be more than doubled in spite of smooth consistency without loss of consistency.

Emulsion base 2

Bine is a body lotion containing 0.50% of an electroneutral compound of stearyl sulfate and carboxymethyldextran (2: 1) and polydimethyldiallylammonium chloride. For this, the alkyl sulfate and the dextran derivative are added to the water phase and emulsified as known. The cationic high polymer is pumped at the time of adding perfume at 30 to 35 ⁰ C. The lotion is extremely finely dispersed and hardly changes its consistency during storage. It can be bottled immediately.

Emulsion base 3

is a shaving cream, which is manufactured according to known technology. The saponification is carried out so that about 5% of the fatty acids are present as free acids. Some of these acids are used to form the electroneutral compound which is formed after quenching of the saponification (neutralization) in the scrap, that with slow stirring a homogeneous solution of cetyltrimethyl- and cetyldimethylbenzylammonium chloride (1: 1) and the oleic acid diethanolamide and glycerol at about 45 ⁰ C is added to the cream. The electroneutral compound causes a well-finished final product to be obtained, which need not be subjected to long maturation.

Emulsion base 4

is a hair rinse containing 0.35% of an electroneutral compound of guar hydroxypropyltrimethylammonium chloride and the sulfosuccinic acid monoester of a fatty alcohol polyglycol ether. The oil phase is heated to Hb ⁰ C and η it with the proportionate water phase containing the propylene glycol, distearyldimethyl / ammonium chloride and 1ie citric acid, emulsified at about 7O ⁰ C starting temperature. The electroneutral compound is obtained in such a way that the cationic high polymer is swollen and dissolved in 30% of the amount of water in accordance with the formulation and the addition of the anionic surfactant then takes place with stirring. The resulting dispersion is introduced into the high-viscosity emulsion. It is an elegant viscous emulsion obtained, which can be prepared immediately and can be diluted with a high excess of water easily and without lumps.

Emulsion base 5

is a W / O skin protection cream in which the oil phase is heated to 7O ⁰ C and emulsified with the 75 ⁰ C hot water phase with simultaneous cooling.

The electroneutral compound of dimethyldistearylammonium chloride and a low molecular weight carboxymethylsilicate is formed in the emulsification such that the CMC was swollen and dissolved in the water phase and the cationic surfactant was in the oil phase. After homogenisation, a smooth, soft cream is used, which no one has to rub ^; i.

Emulsion base 6

Is an O / W emulsion that can be used as a hair tonic. The emulsifiers are melted and emulsified with about 50% of the water phase of the same temperature. After formation of the emulsion and its cooling to 5O ⁰ C dissolved in about 5% of the set ammoniacal water phase dyes are added. With further stirring and cooling, the 20% aqueous dispersion of an electroneutral compound stored at room temperature is pumped in, which was obtained by reaction of stearyltrimethylammonium chloride and sodium dodecyl ether sulfate (3EO) at 45 to 50 ° C. by intensive stirring. The result is a supple color cream that foams easily when applied and does not drip off the wet hair even after a long period of application.

Claims (4)

A process for the preparation of consistency-controlled emulsions containing an electroneutral compound formed from anionic and cationic surfactants and / or organic high polymers bearing acidic or basic groups or combinations thereof with the ionic surfactants, characterized in that in the period of emulsification until the completion of the preparation of the emulsion, the electroneutral compound is added in concentrations of 0.10 to 5% as an aqueous dispersion or made in the system during this period, by the cationic and anionic surfactants and / or the organic high polymers, the acidic or basic groups are brought together by known method steps with stirring. 2. A process for the preparation of consistency-regulated emulsions according to claim 1, characterized in that the anionic surfactants used to form the electroneutral compound carboxylic acids or their salts, alkyl sulfonates, alkyl sulfates, alkyl ether sulfates, sulfosuccinic monoesters of fatty alcohols or fatty alcohol polyglydol ethers, acid Alkyiphosphorsäureester, condensation products of Fbttsäurohalogeniden with protein hydrolysates, sarcosine or Are methyl taurine in which the underlying alkyl radicals chain lengths of C10 to C22, are saturated or unsaturated and the alkyl polyglycol ethers contain up to 8MoI EO or the organic high polymers which carry acidic groups, carboxymethyl cellulose and / or carboxymethyldextran. 3. A process for preparing consistency-regulated emulsions according to claim 1, characterized in that the cationic surfactants used to form the electroneutral compound alkyltrimethyl, dialkyldimethyl, alkyldimethylbenzyl, Alkyldihydroxyethylmethyl- and Alkyldipolyethoxymethylammoniumhalogenide or Methosulfate or Alkylpyridiniumhalogenide are in which the underlying alkyl radicals chain lengths of Or the organic high polymers bearing basic groups, quantitated Poi / vinylpyrrolidone copolymers, Polydialkyldiallylammoniumchloride, with trimethylated reaction products of hydroxycellulose and epichlorohydride or with epichlorohydrin quaternized polyamides and / or guar hydroxypropyltrimethylammonium chloride. 4. A process for the preparation of consistency-controlled emulsions according to claim 1 to 3, characterized in that the added as aqueous dispersion Elektroneutralverbindung by mixing from the anion and cationic surfactants or the acidic or basic groups bearing organic high polymers or combinations of them with the ionic surfactants is prepared and adjusted to a concentration not higher than 500g / l.