DE2943521A1 - Aerosol compsn. contg. hydrophilic and hydrophobic components - in which hydrophobic components are filled into aerosol container as soln. in hydrophobic propellant - Google Patents

Abstract

In a new process for the prodn. of an aerosol compsn. contg. (1) a hydrophobic propellant, (2) at least one hydrophobic component which is soluble in the propellant, opt. (3) hydrophilic components and/or (4) solid, insoluble components, (A) the hydrophobic components are dissolved in the hydrophobic propellant before filling, and (B) the resulting soln. is compressed into a pressure container. Used in prodn. of aerosol compsns. such as aerosol permanent wave, fixative, dry shampoo or dry deodorant compsns., medicaments in aerosol form, door lock de-icer aerosols, over cleaner aerosols, and polishing and cleaning compsns. in aerosol form. Dissolution of the hydrophobic components in the propellant simplifies the filling procedure, and permits small amts. of hydrophobic components to be accurately measured.

Description

Process for the production of aerosol compositions

The invention relates to a process for production of propellant-containing aerosol compositions in which the hydrophobic components of these compositions prior to the filling of the hydrophobic propellant therein be solved.

Aerosol compositions, the production of which is the subject of this application is, have at least A) a gas phase consisting essentially of gaseous Propellants and, if appropriate, other volatile components and B) a liquid hydrophobic phase, consisting of liquid propellant and in this propellant soluble ingredients.

In addition, these compositions can optionally also C) a liquid hydrophilic phase, consisting of the hydrophilic components and / or D) a solid phase, consisting of insoluble, preferably powdery components, contain.

The main propellants used are volatile hydrocarbons and halogenated hydrocarbons and mixtures thereof use.

Hydrophobic constituents of the aerosol compositions which are soluble in these propellants are for example hydrophobic perfume oils, hydrophobic dyes, hydrophobic preservatives, Silicone oils, paraffins and terpenes.

It is known to fill such aerosol compositions in such a way that that one t. optionally present hydrophilic constituents and / or solid, insoluble ones Filling components one after the other or together in a pressure vessel, then 2. adding the hydrophobic constituents one after the other or together, then closes the pressure vessel with a valve and 3. the hydrophobic propellant through the valve under pressure.

This known filling method for propellant-containing aerosol compositions Has the following disadvantages: For the filling of hydrophobic components an elgener work step required. At the same time, the exact filling is very small amounts of hydrophobic stock parts, such as of hydrophobic Preservatives, perfume oils and dyes, in the manufacture of cosmetic Funds problematic. On the other hand, oil-soluble dyes, silicone oils, Perfume oils and terpenes are insoluble, sparingly soluble in the mostly aqueous active ingredient phase or difficult to emulsify. These substances can therefore not be included in the hydrophilic Incorporate aqueous phase. There are no other components in the hydrophilic phase resistant. For example, esters can be saponified in the hydrophilic phase.

In addition, it has so far not been possible to prevent the spraying of certain aerosol compositions, such as aerosol permanent waving and fixing agents, foam is created in staining in a satisfactory manner.

The foam is colored, for example, for aesthetic reasons to cover up the unwanted coloration caused by certain active ingredients aimed at the foam. But what is also important is that made possible by staining Distinguishability of foams. For example, mistaking a hair-shaping agent with a fixative during application, each with a different color Foam, hardly possible anymore. Furthermore, the color deepening that occurs during the exposure time of the colored foam to the hair to determine the required Duration of treatment can be used.

According to the previously customary processes, the foam had to be colored large amounts of hydrophilic dyes are used in aerosol preparations, that the color was drawn onto the hair and stained it at the same time. But if you wanted to Using hydrophobic dyes, a large amount of solubilizers had to be used at the same time can be used to enable their incorporation in the hydrophilic phase. However, such high concentrations of solution can mediate in many aerosol preparations cannot be used without this resulting in disadvantages with regard to the properties of the preparation.

In contrast, it has now been found that a process for the preparation an aerosol composition containing a) a hydrophobic propellant, b) at least a hydrophobic component which is soluble in this propellant and, if appropriate c) hydrophilic constituents and / or d) solid insoluble constituents, characterized in that that before filling the hydrophobic propellant, the hydrophobic constituents dissolves in it and presses the resulting solution into a pressure vessel, the does not have the disadvantages described above and according to this invention Aerosol compositions produced by the method have advantageous properties.

If necessary, this can be present in the pressure vessel after filling Mixture additionally at 200 C and a pressure of 4 to 8 bar, preferably 6 bar, be saturated with N20 or N2.

The hydrophilic components can, for example, in the form of an aqueous Solution available.

In the case of aerosol hair styling agents, this is generally the case an aqueous alkaline solution of a suitable mercaptan, especially the salt the thioglycolic acid, or the aqueous, weakly acidic, neutral or alkaline Solution of an ammonium or alkali sulfite. In addition, this solution can for example Ammonium carbonate, ammonium hydrogen carbonate and surface-active substances such as contain ethoxylated alkylphenols and other hydrophilic substances.

The hydrophilic ingredients of hair fixatives come in aerosol form especially aqueous solutions of hydrogen peroxide, alkali bromates, surface-active Substances such as fatty acid ethylene glycol ether sulfates, ethoxylated Alkylphenols or other suitable hydrophilic substances, into consideration.

Further hydrophilic components of cosmetic preparations are ammonium and alkali hydroxides, salts, organic and inorganic acids, polyhydric alcohols such as glycerine, monohydric alcohols, especially ethanol, n-propanol and i-propanol, and, for example, as a component of hairsprays, aqueous-alcoholic solutions of synthetic and natural resins.

Dry shampoos produced by the process of the invention and dry aerosol deodorants contain as a solid insoluble component in particular a powder made from rice starch, corn starch or talc; corresponding foot Yrper and baby powder, on the other hand, are mostly finely ground kaolin.

As hydrophobic components of cosmetic products in aerosol form paraffins, isoparaffins, methylsiloxanes, Pclysllexanes, ParfXmole, essential oils such as anise oil, bergamot oil, camphor oil, citronella oil lavender oil lemon oil, Rose oil, bitter orange oil, wintergreen oil and hydrophobic care substances such as Cholesterol and lanolin, hydrophobic bactericidal substances such as trichlorocarbanilide and hexachlorophene in consideration of the preferred field of application of the one described herein However, the process is the production of such cosmetic and other aerosol preparations, which are considered hydrophobic Component of at least one hydrophobic dye contain. Of these, in turn, is the production of such aerosol preparations preferred subject of the application, which when sprayed a colored foam result. Suitable hydrophobic for use in the process described Dyes are, for example, Solvent Yellow 56 (C.I. 11 021), Solvent Yellow 5 (C.I. 11 380), Solvent Yellow 6 (C.I. 11 390), Solvent Yellow 29 (C.I. 21 230), Solvent Orange 7 (C.I. 12 140), Solvent Red 1 (C.I. 12 150), Solvent Violet 13 (C.I. 60 725), Solvent Blue 63 (C.I. 61 520), Solvent Blue 11 (C.I. 61 525), Solvent Blue 35 (C.I. 61 554), Solvent Green 3 (C.I. 61 565), azulene and β-carotene.

Particularly suitable hydrophobic blowing agents are hydrocarbons and halogenated hydrocarbons with a boiling point between about -820 C and + 250 C such as butane, isobutane, propane, monofluorotrichloromethane, difluorodichloromethane, Tetrafluoromethane, difluorodichloroethane, tetrafluorodichloroethane, difluoroethane, but also low-boiling ethers such as dimethyl ether, methyl ethyl ether and mixtures to name this propellant.

The inventive method is not aimed at the manufacture of cosmetic Aerosol compositions are limited but can be used in numerous areas of technology Find application. The production of pharmaceuticals in Aerosol form, which as hydrophobic components soluble in the propellant, for example Salicylic acid derivatives, nicotinic acid esters, iodine, iodoform, carotenoids, ichthyol, cholesterol, essential oils, camphor, menthol, balsam of Peru, birch tar, wintergreen oil, bitter orange oil, Contain wheat germ oil, perfume oils, or vitamin F by applying what is described here Procedure can be simplified considerably.

Further aerosol preparations with a content of a hydrophobic propellant and hydrophobic constituents soluble therein which are obtained by the process according to the invention Can be produced more easily and with better properties are for example Door lock deicer in aerosol form, oven cleaner in aerosol form as well as cleaning and Care products in aerosol form.

The following examples are intended to further illustrate the subject matter of the invention explain.

Examples Example 1 Process for the preparation of hair styling agents in A solform> which, when sprayed from a pressure vessel, produces a colored foam result in I) solution 1, consisting of the hydrophilic components: 19.7 g ammonium thioglycolate, 50% aqueous solution 1.0 g ammonium carbonate 5.0 g ammonium hydrogen carbonate 0.8 g of octylphenol, ethoxylated with 10 moles of ethylene oxide 1.0 g of p-nonylphenol, with 10 Mol of ethylene oxide ethoxylated 72.5 g of water 100.0 g The pH of this aqueous active ingredient solution is 8.7.

II) solutions consisting of the hydrophobic propellant and the hydrophobic Ingredients: Solution A 38.00 g difluorodichloromethane 58.00 g tetrafluorodichloroethane 2.00 g perfume oil 2.00 g azulene 100.00 g solution B 31.00 g difluorodichloromethane 46.00 g tetrafluorodichloroethane 2.87 g perfume oil 20.00 g diethylene glycol diethyl ether 0.13 g of Solvent Red 1 dye (C.I. 12 150) 100.00 g Solution C 27.00 g difluorodichloromethane 36.00 g tetrafluorodichloroethane 27.00 g n-butane 3.00 g perfume oil 7.00 g carotene oil 100.00 g solution D 30.00 g difluorodichloromethane 40.00 g tetrafluorodichloroethane 27.00 g n-butane 2.75 g perfume oil 0.25 g dye Solvent Blue 35 (C.I. 61 554) 100.00 g For the production of the deforming agents i) to 4) given below the amounts of solution I specified there, consisting of the hydrophilic components, each filled into a pressure vessel, dle pressure vessel with one valve each provided and then the specified amounts of solutions A to D, consisting of S the hydrophobic Treund the hydrophobic constituents dissolved therein, through the valves pressed in.

Amounts of solution I and solutions A to D to be used: Medium 1) 84 g solution I / 16 g solution A medium 2) 82 g solution 1 1 18 g solution B medium 3) 84 g of solution I J 16 g of solution C Medium 4) 85 g of solution I 1 15 g of solution D the The amounts given for these agents are each for one hair-shaping treatment certainly. The perfume oil dissolved in the propellant remains even after filling largely dissolved in this and is therefore due to the hydrophilic active ingredient components not changed.

The foam emerging from the pressure vessel during spraying is at the hair shaping agents 1) and 4) blue, with the hair shaping agent 2) pink and colored yellow in the case of the hair shaping agent 3).

The ones contained in these hair shaping agents for coloring the foam Dyes are not absorbed by the hair, do not dye the hair and can therefore serve as a characteristic feature of the respective remedy.

Example 2 Process for the preparation of fixatives in aerosol form I) Solution I, consisting of the hydrophilic components: 6.0 g sodium bromate 0.7 g sodium lauryl diethylene glycol ether sulfate 3.0 g nonylphenol polyglycol ether, with 8-12 moles of ethylene oxide ethoxylated 90.3 g of water 100.0 g The pH of this aqueous active ingredient solution is 6.5.

II) solutions consisting of the hydrophobic propellant and therein dissolved hydrophobic components: solution A 40.00 g difluorodichloromethane 56.00 g tetrafluorodichloroethane 4.00 g perfume oil 100.00 g solution B 36.00 g difluorodichloromethane 41.00 g tetrafluorodichloroethane 4.87 g perfume oil 18.00 g diethylene glycol diethyl ether g g Dye Solvent Red 1 (C.I. 12 150) 100.00 g To make the following specified fixing agents 1) and 2) are the amounts of the solution specified there Is composed of the hydrophilic components, each filled into a pressure vessel, each pressure vessel is provided with a valve and then the specified quantities of Solutions A and B consisting of the hydrophobic propellant and the dissolved therein hydrophobic components, each pressed in through the corresponding valve Finally the mixture is saturated with N20 while shaking at 200 ° C. and a pressure of 6 bar.

Medium 1) 85 g solution I / 15 g solution A Medium 2) 82 g solution I / 18 g of solution B The foam that escapes from the pressure vessel when it is sprayed is at Medium 2) colored red.

Example 3 Method of making a dry shampoo in aerosol form I) Solid insoluble component: rice starch in powder form II) solution, consisting from the hydrophobic propellant and the hydrophobic constituents dissolved therein: 42.00 g difluorodichloromethane 52.00 g tetrafluorodichloroethane 0.20 g perfume oil 5.80 g mixture from isoparaffins with a boiling point between 170 and 1900 C 100.00 g 10 g rice starch are filled into a pressure vessel, the pressure vessel with a valve provided and then 90 g of the above-mentioned solution of the hydrophobic components pressed into the hydrophobic propellant through the valve.

According to the conventional method, the filling would have to be done in three steps be done since about 6% of the hydrophobic components are not in let the rice starch work in without losing the flowability of the powder goes.

Example 4 Process for the preparation of deodorants in aerosol form I) Solid, insoluble component: Talcum powder II) Solutions consisting of the hydrophobic propellant and the hydrophobic components dissolved therein: solution A 49.50 g difluorodichloromethane 49.50 g trichlorofluoromethane 0.16 g perfume oil 0.10 g isopropyl myristate 0.04 g trichlorocarbanilide 0.10 g polyethylene glycol (molecular weight = 570 - 630) 0.0 g diethylene glycol diethyl ether 100.00 g solution B 49.00 g difluorodichloromethane 49.00 g trichlorofluoromethane 0.20 g perfume oil 0.10 g hexachlorophene 1> 20 g hexadecyl alcohol 0.50 g lauric acid hexyl ester 100.00 g Deodorant powder spray 10 g talc powder are filled into a pressure vessel, the pressure vessel with a Provided a valve and then 90 g of solutions A or B pressed in through the valve.

Dry deodorant 100 g of the are pressed in a single operation Solution A or B into a valved pressure vessel and obtained such a ready-to-use dry deodorant spray.

Example 5 Process for the preparation of a hair setting solution I, consisting of the hydrophilic components: 30.00 g of ethanol 2.00 g of copolymer 60% vinyl pyrrolidone / 40% vinyl acetate 68.00 g water 100.00 g solution II, consisting of from the hydrophobic propellant and the hydrophobic constituents dissolved therein: 81.00 g difluorodichloromethane 16.00 g hexamethylsiloxane 3.00 g perfume oil 100.00 g 64 g of the aqueous solution I are placed in a pressure vessel, the pressure vessel provided with a valve and then injected 36 g of solution II through the valve.

Because the hexamethylsiloxane and the perfume oil are in the aqueous solution would not solve, the production of this preparation would be according to the previously known methods very difficult.

Example 6 Process for the production of a pre-moistening and winding aid for the permanent wave treatment solution 1, consisting of the hydrophilic components: 0.30 g of dimethylaminoethyl methacrylate homopolymer, 75% quaternized 0.110 g of 2-coconut-1-sodium carboxymethyl) -1- (2-hydroxyethyl) imidazolinium hydroxide 0.2 µg hexadecyltrimethylammonium chloride 99.40 g of water 100.00 g of solution II, consisting of the hydrophobic propellant and hydrophobic constituents dissolved therein: 50.00 g of difluorodichloromethane 48.00 g of hexamethylsiloxane 2.00 g of perfume oil 100.00 g of 50 g of the aqueous solution I will be filled into a pressure vessel, the pressure vessel provided with a valve and then injected 50 g of solution II through the valve.

This pre-moistening and wrapping aid for permanent wave treatment in aerosol form is intended for multiple treatments.

Hexamethylsiloxane and perfume oil do not dissolve in the aqueous solution I and would therefore have to be filled separately using the known method.

Example 7 Method of making an oven cleaner in aerosol form Solution I, consisting of the hydrophilic components: 5.00 g sodium hydroxide 3.00 g of stearyl alcohol ethoxylated with 10 moles of ethylene oxide 92.00 g of water 100.00 g solution II, consisting of the hydrophobic propellant and the hydrophobic ones dissolved therein Ingredients: 70.00 g n-butane 10.00 g propane 20.00 g decamethyltetrasiloxane 100.00 90 g of aqueous solution I are placed in a pressure vessel, the container provided with a valve and then injected 10 g of solution II through the valve.

Since the decamethyltetrasiloxane is difficult to incorporate into an aqueous solution lets, the production of such preparations according to the method according to the invention considerably learned.

Example 8 Method of making a door lock deicer in aerosol form Solution I, consisting of the hydrophilic components: 70.00 g ethanol, 96% 25.00 5 g glycerol> 00 g stearyl alcohol ethoxylated with 10 mol ethylene oxide 100.00 g solution II, consisting of the hydrophobic propellant and the hydrophobic ones dissolved therein Ingredients: 15.00 g n-butane 20.00 g propane 65.00 g paraffin 100.00 g 80 g der Solution I is filled into a pressure vessel and the vessel is provided with a valve and then injected 20 g of solution II through the valve.

Put all percentages given in the present application Percentages by weight.

Claims (5)

Claims 1. A method for producing an aerosol composition, containing a) a hydrophobic propellant, b) at least one in this propellant soluble hydrophobic constituent and optionally c) hydrophilic constituents and / or d) solid insoluble constituents, characterized in that before the Filling the hydrophobic propellant dissolves the hydrophobic constituents in this and injecting the resulting solution into a pressure vessel. 2. The method according to claim 1, characterized in that as hydrophobic component used at least one hydrophobic dye. 3. The method according to claim 1 and 2, characterized in that one as the hydrophobic dye, a dye selected from Solvent Yellow 56 (C.I. 11 021), Solvent Yellow 5 (C.I. 11 380), Solvent Yellow 6 (C.I. 11 390), Solvent Yellow 29 (C.I. 21 230), Solvent Orange 7 (C.I. 12 140), Solvent Red 1 (C.I. 12 150), Solvent Violet 13 (C.I. 60 725), Solvent Blue 63 (C.I. 61 520), Solvent Blue 11 (C.I. 61 525), Solvent Blue 35 (C.I. 61 554), Solvent Green 3 (C.I. 61 565), azulene and ß-carotene are used. 4. The method according to claim 1, characterized in that as hydrophobic component selected from the paraffins class, Isoparaffins, methylsiloxanes, salicylic acid derivatives, nicotinic acid esters, terpenes, ethereal ble, carotenoids and the substances diethylene glycol diethyl ether2 trichlorocarbanilide, Hexachlorophene, ichthyol, Peru balsam, birch tar, camphor, menthol, winter green oil, Bitter orange oil, cholesterol, vitamin F, wheat germ oil, iodine, iodoform and perfume oil are used. 5 The method according to claim i rch 4, characterized in that one the mixture present in the pressure vessel additionally at 200 C and a pressure of 4 to 8 bar, preferably 6 bar, saturated with N20 or N2.