EP1599176A1

EP1599176A1 - O/w emulsifier and o/w emulsions containing potassium cetyl phosphate and method for the production thereof

Info

Publication number: EP1599176A1
Application number: EP04714278A
Authority: EP
Inventors: Bernd Schröder
Original assignee: Symrise AG
Current assignee: Symrise AG
Priority date: 2003-02-25
Filing date: 2004-02-25
Publication date: 2005-11-30
Also published as: WO2004075868A1; JP2006519686A; CN1753655A; US20060171913A1; DE10308565A1; CN100418507C; KR20050100653A

Abstract

The invention relates to O/W emulsifiers comprising: (a) hardened palm oil glycerides, and; (b) potassium cetyl phosphate, whereby the proportion of potassium cetyl phosphate ranges from 40 to 80 % by weight with regard to the total mass of the emulsifier. The invention also relates to corresponding O/W emulsions containing a water phase, an oil phase dispersed in the water phase, and 0.25 to 15 percent by weight of the aforementioned O/W emulsifier. The invention finally relates to a method for producing an O/W emulsion of this type.

Description

20

25

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O / W EMULSIFIER, AND O / W EMULSIONS CONTAINING POTASSIUM CETYL PHOSPHATE AND METHOD

N FOR THEIR PRODUCTION

35

Emulsions are usually formed from two liquid phases that are immiscible. When producing an emulsion, one phase is dispersed in finely divided form in the other phase. There are two main types of emulsions, namely "water-in-oil" and "oil-in"

40 water emulsions. In the oil-in-water emulsion (O / W emulsion), the oil is the inner phase, which is dispersed in the outer (water) phase. The properties of the corresponding emulsion are essentially determined by the outer phase, so that water-in-oil emulsions (W / O emulsions) tend to look more like oils and oil-in-water emulsions (O / W emulsions)

45 behave like aqueous solutions. In specific embodiments, the present invention relates to a multifunctional oil-in-water emulsifier (O / W emulsifier) for the production of O / W emulsions which is free of polyethylene glycol (PEG). When using emulsions of this type, it is difficult to obtain a stable O / W emulsion and in particular a stable, low-viscosity O / W emulsion even at a low use concentration (<10% by weight).

It was the object of the present invention to provide an O / W emulsifier which requires only a low dosage, is universally suitable for the production of emulsions with different viscosities (for example lotions, milks and creams), in a wide pH range (from eg pH 3 to 11) can be used and has excellent skin tolerance. The O / W emulsifier to be specified should preferably also be PEG-free.

Corresponding O / W emulsions and processes for their preparation should also be specified.

According to a first aspect of the present invention, the object is achieved by specifying an O / W emulsifier comprising: (a) hardened palm oil glycerides and (b) potassium cetyl phosphate, the proportion of potassium cetyl phosphate being in the range from 40 to 80% by weight .-%, based on the total mass of the emulsifier.

Potassium cetyl phosphate (CAS-No .: 19035-79-1) has the empirical formula C ₁₆ H ₃₄ 0 ₄ PK and the structural formula

It can also be called the potassium salt of phosphoric acid monohexadecyl ester (1: 1). The invention is based on the surprising discovery that potassium cetyl phosphate, hardened at ^'the simultaneous presence of palm oil glycerides (mono-, di- and triglycerides of fatty acids contained in palm oil, eg the mono-, di- and triglycerides of oleic acid, the Palmitic acid, stearic acid, myristic acid, lignoceric acid and palmitoleic acid) can be used at a low dosage to produce stable, skin-smoothing O / W emulsions.

The O / W emulsifier according to the invention preferably contains no polyethylene glycol (PEG) and / or no other glycol and / or no paraffin and / or no isoparaffin.

The O / W emulsifier according to the invention usually comprises (a) hardened palm oil glycerides, (b) potassium cetyl phosphate,

(c) cetyl alcohol and

(d) water, the proportion of potassium cetyl phosphate being in the range from 40-80% by weight, preferably 50-70% by weight, based on the total mass of components (a) and (b).

The cetyl alcohol can result from the production process for the potassium cetyl phosphate. This is because cetyl alcohol is first esterified with phosphoric acid and then neutralized (fully neutralized) with potassium hydroxide, i.e. one acidic proton per molecule is neutralized by potassium hydroxide and the resulting negative charge is neutralized by a potassium ion. If an excess of cetyl alcohol over phosphoric acid is used, cetyl alcohol remains in the product mixture after the esterification.

O / W emulsifiers according to the invention, which consist of:

(a) 30-50% by weight hardened palm oil glycerides,

(b) 40-50% by weight potassium cetyl phosphate, (c) 8-15% by weight cetyl alcohol, (d) 4-8 wt% water and

(e) 0-18% by weight of further additives, in particular inorganic salts, the percentages by weight relating to the total mass of the O / W emulsifier.

The O / W emulsifier according to the invention, in particular in its preferred configurations, enables thermostable emulsions even at low use concentrations (<10% by weight).

The applicability of O / W emulsifiers according to the invention is versatile; in particular, they can be used for high-viscosity creams, medium-viscosity milks and lotions as well as low-viscosity, spray-resistant lotions.

The use of the O / W emulsifiers according to the invention enables good dispersion of solids in the resulting emulsion systems.

When using the O / W emulsifiers according to the invention, the dispersibility of incorporated active ingredients is increased regularly.

The emulsions formulated with the aid of the O / W emulsifiers according to the invention are notable for their largely pH-independent behavior.

When using the O / W emulsifiers according to the invention, formulations (emulsions) can be prepared using polar and non-polar oils.

The O / W emulsifiers according to the invention are compatible with hydrogel formers and hydrocolloids.

A combination of the O / W emulsifiers according to the invention with UV / A and UV / B filters is particularly advantageous. The use of emulsifiers regularly leads to an improvement in the water resistance of corresponding sun protection products. Commercial and logistical advantages are particularly advantageous since only one emulsifier has to be procured and stored in order to produce lotions and creams.

The O / W emulsifier according to the invention has very good skin compatibility.

A particular advantage of the O / W emulsifier according to the invention in comparison with previously conventional O / W emulsifiers is that the emulsifier according to the invention can be in the form of a lozenge. The pastille shape is also the preferred form of packaging the O / W emulsifier according to the invention.

Due to the chemical composition of the O / W emulsifiers according to the invention, their physical and chemical properties are largely determined, but certain variations are nonetheless possible. O / W emulsifiers according to the invention which have met one, more or preferably all of the following conditions have proven to be particularly advantageous:

after dissolving in neutralized water at a concentration of 10% by weight, based on the finished solution, the pH is in the range of 5.0 -

6.5;

the saponification number with a saponification time of 1 hour is in the range of 125.0 -155.0 (test method 21 1)

the acid number when using the solvent system diethyl ether: ethanol: water 1: 1: 1 (v / v / v) is in the range of 50.0 - 80.0 mg KOH / g (test method 228).

With regard to the specified test methods 211 and 228, we refer to the examples below.

The melting point of an O / W emulsifier according to the invention is preferably set so that it is in the range from 75 to 80 ° C. The setting of the Melting point is controlled in particular by the content of cetyl alcohol in the O / W emulsifier.

The incorporation of an O / W emulsifier according to the invention into an emulsion can optionally take place via the water phase or the oil phase; incorporation via the water phase is often preferred since this generally gives a better emulsion image (better visual assessment).

According to a second aspect, the object on which the invention is based is achieved by an O / W emulsion, comprising:

a water phase an oil phase dispersed in the water phase and

0.25-15% by weight, preferably 1-15% by weight, of an O / W emulsifier according to one of the preceding claims, the percentage by weight being based on the total mass of the O / W emulsion.

A proportion of 0.25 to 0.50% by weight of the O / W emulsifier according to the invention is often sufficient to stabilize emulsions.

Use concentrations which are in the range from 0.5 to 3.0% by weight are typically used to prepare O / W emulsions.

0.5 to 4.0% by weight, preferably between 1.0 and 2.0% by weight, of the O / W emulsifier according to the invention is frequently used for medium-viscosity lotions.

For ointments, creams and hair gels, between 1.0 and 15.0% by weight, but preferably between 2.0 and 3.0% by weight, are used as the O / W emulsifier according to the invention.

It can be particularly practical to process the O / W emulsifier according to the invention in the water phase and at the same time to process propylene glycol and / or pentylene glycol (Hydrolite-5). In this way, the Solution temperature of the O / W emulsifier according to the invention can be reduced in the water phase. In this case, the O / W emulsifier according to the invention is preferably predissolved in the raw material (propylene glycol and / or pentylene glycol), the solution temperature being approximately 75 ° C. The liquid phase consisting of the O / W emulsifier and raw material (solvent) is then preferably subsequently mixed with the other constituents of the water phase, it being sufficient to heat the entire water phase to approximately 65 ° C. (provided the other constituents of the water phase permit this) ,

Alternatively, propylene glycol and / or pentylene glycol can also be incorporated into the water phase beforehand, the O / W emulsifier according to the invention then being added to the resulting water phase. With this procedure, however, the influence on the solution temperature of the O / W emulsifier is not so high; the solution temperature is then around 80-83 ° C.

The O / W emulsions according to the invention are distinguished, inter alia, by: good viscosity stability, high pH stability or pH-independent stability, good temperature stability, a very fine and homogeneous emulsion structure with a glossy finish

Surface, as well as commercial and logistical advantages, since only an emulsifier has to be procured and stored in order to produce lotions and creams.

An O / W emulsion according to the invention advantageously comprises a water phase, an oil phase dispersed in the water phase and 0.25-15% by weight, preferably 1-15% by weight, of an O / W emulsifier according to the invention, the percentage by weight being based on the Total mass of the O / W emulsion is related. In addition, preferred O / W emulsions additionally comprise 0.1-10% by weight of a stabilizing agent and / or 1-10% by weight of a co-emulsifier, the percentage by weight being based on the total mass of the O / W emulsion.

The pH of an O / W emulsion according to the invention can vary within wide limits. The pH is advantageously set to a value between 3 and 11, preferably between 4 and 9, more preferably between 4 and 7.

As co-emulsifiers e.g. Glycerol monostearates or other glycerol monoesters of fatty acids, steric acid or other fatty acids (unsaponified or partially saponified), waxes or fatty alcohols are used.

Hydrogel formers such as e.g. Carbomers, acrylate cross-polymers, xantans, alginates etc. can be used.

As already mentioned, preferred O / W emulsions are free from ethylene glycol (PEG), other glycols, paraffin and / or isoparaffin.

The O / W emulsion according to the invention can comprise further constituents, in particular: dispersed solids and / or

UV-A and / or UV-B filters and / or an antioxidant, and / or

Perfume oils and / or other excipients.

In the case of the combination of the emulsifiers according to the invention in the emulsions according to the invention with light protection filters (UV / A and / or UV / B filters), their distributability on the skin is improved and increased water resistance compared to other emulsions is achieved. The emulsifier according to the invention has the following effect in an emulsion according to the invention, alone or together with other cosmetic auxiliaries:

Increasing the sun protection factor of UV filters (UVA and / or UVB protection); Stabilization of UV filters (improved photo stabilization); Improvement of the solubility and / or suspension of solid UV filters; Increasing the water resistance of sun protection products; Support in the formation of a gel network structure; Increasing the effectiveness of active substances, e.g. Antioxidants, preservatives, skin lighteners and tanning agents, perfume oils, chelating agents; Increasing the substantivity of active ingredients on the skin and / or hair; Improving the distribution of cosmetic oils (vegetable oils, mineral oils, emollients), active ingredients, vitamins, perfume oils and essential oils on the skin; Support for an even distribution of repellent agents; Contribution to an optimal distribution of conservation systems in the water phase; Support the barrier function of the skin; Reduction of the agglomeration rate of inorganic UV filters (titanium dioxide, zinc oxide) and color pigments; Supporting the distribution of aluminum salts in antiperspirant products; Compatibility with alcohols, including ethanol; improved stabilization of emulsions as main or co-emulsifier.

Formulation examples: skin care cream (O / W), body lotion, sun protection cream (O / W), sun protection milk (O / W), sprayable sun milk (O / W), sensitive balm roll-on and cream (O / W), sprayable deodorant Lotion, antiperspirant lotion, hair conditioner, hair gel wax for men, hair cream, tinted day cream, mascara, care lotion for wet wipes.

The emulsifier according to the invention can be combined with the following raw materials: The emulsifier according to the invention can be formulated together with light stabilizers. Suitable light stabilizers are, for example, organic UV absorbers from the class of 4-aminobenzoic acid and derivatives, salicylic acid derivatives, benzophenone derivatives, dibenzoylmethane derivatives, diphenylacrylates, 3-imidazol-4-yl-acrylic acid and their esters, benzofuran derivatives, Benzylidene malonate derivatives, polymeric UV absorbers (containing one or more organic silicon residues), cinnamic acid derivatives, camphor derivatives, trianilino-s-triazine derivatives, 2-hydroxyphenylbenzotriazole derivatives, 2-

Phenylbenzimidazole-5-sulfonic acid and its salts, Anthranilsäurementhylester, benzotriazole derivatives.

The emulsifier according to the invention can also be incorporated into cosmetic and / or dermatological preparations which contain pigments, preferably finely divided pigments. These can be organic or inorganic pigments. Preferred organic pigment is 2,2'-methylene-bis- [6- (2H-benzotriazol-2-yl) -4- (1, 1, 3,3tetramethylbutyl) phenol] (Tinosorb ^® M). Suitable inorganic pigments or micropigments based on metal oxides and / or other metal compounds which are sparingly soluble or insoluble in water are, in particular, oxides of titanium (Ti0 ₂ ), zinc (ZnO), iron (eg Fe ₂ 0 ₃ ), zirconium (Zr0 ₂ ), silicon (Si0 ₂ ), manganese (eg MnO), aluminum (Al ₂ 0 ₃ ), cerium (eg Ce ₂ 03), mixed oxides of the corresponding metals and mixtures of such oxides. These pigments are X-ray amorphous or non-X-ray amorphous. Finely divided pigments based on Ti 0 ₂ and ZnO are particularly preferred.

The emulsifier according to the invention can also be incorporated into cosmetic and / or dermatological preparations (emulsions) which are composed as usual and the cosmetic and / or dermatological light protection, further for the treatment, care and cleaning of the skin and / or hair and as Make-up product used in decorative cosmetics. Accordingly, preparations of this type, depending on their structure, can be used, for example, as skin protection cream, cleansing milk, sunscreen lotion, nutritional cream, day or night cream, etc. Such preparations (emulsions) can be present, for example, as a lotion, milk, cream, hydrodispersion gel, balm, spray, foam, hair shampoo, hair care product, hair conditioner, roll-on, stick or make-up.

It may be possible and advantageous to use such preparations as the basis for pharmaceutical formulations. Are preferred in particular those cosmetic and dermatological preparations which are in the form of a skin care or make-up product.

For use, the cosmetic and dermatological preparations mentioned by way of example are applied to the skin and / or the hair in a sufficient amount in the manner customary for cosmetics.

The lipid phase can advantageously be selected from the following group of substances:

Mineral oils, mineral waxes; - Oils, such as triglycerides of capric or caprylic acid, more natural

Oils such as Castor oil;

Fats, waxes and other natural and synthetic fat bodies, preferably esters of fatty acids with alcohols of low C number (<10), e.g. with isopropanol, propylene glycol or glycerin, or esters of fatty alcohols with low C number alkanoic acids (<10) or with fatty acids;

benzoates;

Silicone oils such as dimethylpolysiloxane, diethylpolysiloxane, diphenylpolysiloxane and mixed forms thereof.

The lipid phase of the emulsions, oleogels or hydrodispersions or lipodispersions within the meaning of the present publication are advantageously selected from the group of esters from saturated and / or unsaturated, branched and / or unbranched alkane carboxylic acids with a chain length of 3 to 30 carbon atoms and saturated and / or unsaturated, branched and / or unbranched alcohols with a chain length of 3 to 30 carbon atoms, from the group of esters from aromatic carboxylic acids and saturated and / or unsaturated, branched and / or unbranched alcohols with a chain length of 3 to 30 carbon atoms. atoms. Such ester oils can then advantageously be selected from the group of isopropyl myristate, palmitate, stearate, oleate, n-butyl stearate, n-hexyl laurate, n-decyl oleate, isooctyl stearate, isononyl stearate, isononyl isononateate, 2-ethylhexyl palateate, ethyl 2-hexylurate, ethyl 2-hexylurate, ethyl 2-ethyl-acrylate , 2-octyldodecyl palmitate, oleyl oleate, olerlerucate, erucyl oleate and synthetic, semisynthetic and natural mixtures of such esters, for example jojoba oil, 2-ethylhexyl-2-ethylhexanoate, cetearyl-2-ethylhexanoate, diisopropyl adipate, triisonananoin. Furthermore, the lipid phase can advantageously be selected from the group of branched and unbranched hydrocarbons and waxes, silicone oils, dialkyl ethers, the group of saturated or unsaturated, branched or unbranched alcohols, and also fatty acid triglycerides, especially the triglycerol esters of saturated and / or unsaturated, branched and / or unbranched alkane carboxylic acids with a chain length of 8 to 24, in particular 12 to 18, carbon atoms. The fatty acid triglycerides can, for example, advantageously be selected from the group of synthetic, semisynthetic and natural oils, for example olive oil, sunflower oil, soybean oil, peanut oil, rapeseed oil, almond oil, palm oil, coconut oil, palm kernel oil and the like.

Any mixtures of such oil and wax components can also be used advantageously for the purposes of the present invention.

Cyclomethicone (octamethylcyclotetrasiloxane) is advantageously used as the silicone oil to be used. However, other silicone oils can also be used with similar advantages, for example hexamethylcyclotrisiloxane, polydimethylsiloxane, poly (methylphenylsiloxane).

Mixtures of cyclomethicone and isotridecyl isononanoate, of cyclomethicone and 2-ethylhexyl isostearate are also particularly advantageous.

The aqueous phase of preparations in the sense of this publication optionally advantageously contains water-soluble plants extracts, alcohols, diols or polyols (lower alkyl), and their ethers, preferably ethanol, isopropanol, propylene glycol, glycerol, ethylene glycol monoethyl or monobutyl ether, propylene glycol monomethyl, monoethyl or monobutyl ether,

Diethylene glycol monomethyl or monoethyl ether and similar products, furthermore alcohols (lower alkyl), for example ethanol, 1, 2-propanediol, glycerol and in particular one or more thickeners, which one or more can advantageously be selected from the group consisting of silicon dioxide, aluminum silicates, polysaccharides and the like Derivatives, for example hyaluronic acid, xanthan gum, hydroxyropylmethyl cellulose, particularly advantageously from the group of the polyacrylates, preferably a polyacrylate from the group of the so-called Carbopole, for example carbopole types 980, 981, 1382, 2984, 5984, each individually or in combination.

The cosmetic and dermatological preparations (emulsions) within the meaning of this text can contain cosmetic auxiliaries as are usually used in such preparations, e.g. Preservatives, antioxidants, vitamins, bactericides, perfumes, substances to prevent foaming, dyes, pigments that have a coloring effect, thickeners, surfactants, emollients, emulsifiers, moisturizing and / or moisturizing substances, moisturizers, fats, oils, waxes, plant extracts or other customary components of a cosmetic or dermatological formulation such as alcohols, lower alkyl alcohols, polyols, lower alkyl polyols, polymers, foam stabilizers, complexing agents, electrolytes, organic solvents, propellant gases, silicones or silicone derivatives.

The amounts of cosmetic or dermatological auxiliaries and carriers and perfume to be used in each case can easily be determined by a person skilled in the art, depending on the type of product.

An additional level of antioxidants is generally preferred. Favorable antioxidants which can be used are all antioxidants which are suitable or customary for cosmetic and / or dermatological applications.

The amount of the antioxidants (one or more compounds) in the preparations is preferably 0.001 to 30% by weight, particularly preferably 0.05 to 20% by weight, in particular 1 to 10% by weight, based on the total weight the preparation.

The antioxidants are advantageously chosen from the following group: amino acids (eg glycine, histidine, 3,4-dihydroxyphenylalanine, tyrosine, tryptophan) and their derivatives, imidazoles (eg urocanic acid) and their derivatives, peptides (D, L-camosine, D-carnosine, L-carnosine, anserine) and their derivatives, carotenoids, carotenes (e.g. alpha-carotene, beta-carotene, lycopene) and their derivatives, chlorogenic acid and their derivatives, lipoic acid and their derivatives, aurothioglucose, propylthiouracil and other thiols ( eg thioredoxin, Glutathione, cysteine, cystine, cystamine and their glycosyl ^'and N-acyl derivatives or alkyl esters thereof) and also salts thereof, dilauryl thiodipropionate, distearyl thiodipropionate, thiodipropionic acid and derivatives thereof and Phenolsäureamide phenolic benzylamines (eg Homovanillinsäure-, 3,4 Dihydroxyphenylessigsäure-, Ferulasäure- , Sinapic acid, caffeic acid, dihydroferulic acid, dihydrocaffeic acid, vanillomandelic acid or 3,4-dihydroxymandelic acid amides of 3,4-dihydroxybenzyl-, 2,3,4-trihydroxybenzyl- or 3,4,5-trihydroxybenzylamine), Catecholoximes or catecholoxime ethers (e.g. 3,4-dihydroxybenzaldoxime or 3,4-dihydroxybenzaldehyde-O-ethyloxime), 2-hydrazino-1,3thiazoles and derivatives, also (metal) chelators (e.g. 2-hydroxy fatty acids, phytic acid, lactoferrin), humic acid , Bile acids, bile extracts, bilirubin, biliverdin, folic acid and its derivatives, ubiquinone and ubiquinol and their derivatives, vitamin C and its derivatives (eg ascorbyl palmitate, magnesium ascorbylphos phate, ascorbyl acetate), tocopherols and derivatives (e.g. vitamin E acetate), vitamin A and derivatives (e.g. vitamin A palmitate), rutinic acid and its derivatives, flavonoids (e.g. quercetin, alpha-glucosylrutin) and their derivatives, phenolic acids ( e.g. gallic acid, ferulic acid) and their derivatives (e.g. propyl gallic acid, ethyl ester, octyl ester), furfurylidene glucitol, dibutylhydroxytoluene, butylhydroxyanisole, uric acid and its derivatives, mannose and its derivatives, zinc and its derivatives (e.g. ZnO, ZnS0), selenium and its derivatives (e.g. selenomethionine), stilbenes and their derivatives (e.g. stilbene oxide, resveratrol).

Also advantageous antioxidants are described in EP-A 900781, EP-A 1 029 849, EP-A 1 066 821, WO-A 01/43712, WO-A 01/70176, WO-A 01/98235 or also in WO A 01/98258.

If vitamin E and / or its derivatives represent the antioxidant (s), it is advantageous to choose their respective concentrations from the range from 0.001 to 10% by weight, based on the total weight of the formulation.

If vitamin A or vitamin A derivatives or carotenes or their derivatives represent the antioxidant or antioxidants, it is advantageous to use their respective Concentrations from the range of 0.001 to 10 wt .-%, based on the total weight of the formulation to choose.

Further preferred configurations of the invention result from the attached patent claims and the publication in Research Disciosure No. 468115 of May 2003; No. 469, pages 641-644, which is part of this application by reference.

The invention is explained in more detail below with the aid of examples:

Example 1: Sun protection milk (O / W); Example 2: Sun protection lotion (O / W); Example 3: Face cream (O / W) with sun protection; Example 4: Sunscreen milk

(1, 2, 3) Manufacturing process: Part A: Heat to approx. 85 ° C. Part B: Weigh raw materials without Carbopol and Keltrol. Disperse Carbopol and Keltrol with Ultra Turrax. Heat to approx. 85 ° C. Add B to A. Part C: Add immediately to A / B and then homogenize hot (Ultra Turrax). Let cool while stirring. Part D: Add and stir.

(4) Manufacturing process: Part A: Heat to approx. 85 ° C (without Keltrol and zinc oxide). Disperse Keltrol and zinc oxide with the Ultra Turrax in the hot lipid phase. Part B: Heat to approx. 85 ° C. Add B to A. Cool to 60 ° C while stirring and homogenize (Ultra Turrax). Then allow to cool to room temperature while stirring. Part C: Add and homogenize. Examples 1-4 are to be understood as standard formulations since, in the sense of this publication, other sun filters alone or as sun filter compositions also benefit from a combination with the emulsifier according to the invention.

Example (5): Hair gel wax for men- DGHST 0086/01; Example (6): hair cream (O / W) DCHST 0087/00; Example (7): Hair conditioner rinsing (O / W) with Dragoderm DLHCR 0088/00; Example (8): Sensitive Balsam Roll-on (O / W) DRDEO 0089/00; Example (9): care lotion for wet wipes (O / W) DDTSS 009 1/00; Example (10): Skin care cream (O / W) DCSKN 0092/00

Production notes:

(5): Heat phases A and B separately from each other to approx. 75 ° C. Combine with moderate stirring until the gel wax is homogeneous. Then allow to cool, add phase C at approx. 40 ° C and stir until homogeneous. pH: approx. 5.2.

(6) Mix all raw materials of phase A, heat to 80 ° C and homogenize with an Ultra Turrax. Stir cold with a blade stirrer, reducing the stirring speed as the temperature decreases. Add phase C at approx. 35 ° C. pH: approx. 5.9.

(7/8) Heat phases A and B separately to approx. 80 ° C. Add phase B to A (Ultra-Turrax) and emulsify. Stir cold with a paddle, making the

Reduce stirring speed with decreasing temperature. Phase C at approx.

Add 30 ° C. pH: approx.4.2 for (7) and 5.2 for (8). (9/10) Pemulen TR-2 or

Soak Keltrol F in water under an Ultra-Turrax. Heat phases A and B separately to approx. 80 ° C. Add phase B to A (Ultra-Turrax) and emulsify. Add phase C and homogenize again. With a

Stir the blade stirrer, the stirring speed decreasing

Reduce temperature. Add phase D at approx. 35 ^C C. pH: approx.5.5 for (9) and

5.2 for (10).

Examples 7, 8 and 9 above are formulation examples for low-viscosity and sprayable emulsions. Another formulation example for a low viscosity, namely sprayable formulation, is given with Example 11 below.

Example 11 (DDSUN 0090/00) Sprayable sun milk

Formulation examples for high-viscosity and very solid emulsions result from Examples 12 and 13 below

Example 12 (DCSUN 0093/00) sun protection cream (O / W)

Example 13 (DCSKN 0092/00) skin care cream (O / W)

Example 14 below gives extracts from the technical product specification of a preferred emulsifier according to the invention, to which the name "Emulsiphos" has been assigned.

Example 14:

Product name:

2/918520 Emulsiphos

Application note:

Emulsiphos is suitable for the production of creams and lotions in the pH range of 4 - 9. Polar and non-polar oils can be processed with this emulsifier without any problems. The incorporation can take place either over the water phase or oil phase.

Product features:

sensors:

223 Smell: pure on a neutral surface

608 color white to off-white

611 shape pastilles

Chemistry, physics:

method

119 pH 5.0 - 6.5

Test medium: neutralized

water

Test 10.0% concentration

21 1 saponification number 125.0 - 155.0 mg KOH / g saponification time: 1.0 hour

228 acid number 50.0 - 80.0 mg KOH / g solvent = ether ethanol water 1: 1: 1 v / v / v Flash point> 212 ° F / 100 ° C

Microbiology:

Due to the product properties, growth of microorganisms is not expected.

Shelf life:

In the original packaging (protected from light), 15 months at + 20 ° C

Packaging:

plastic containers

Processing information:

Use opened containers as soon as possible or close them well again.

Application areas:

skin cosmetics

Dosage: for O / W emulsions: 1, 0 - 3% to stabilize emulsions: 0.25 - 0.50%

INCI name:

Potassium Cetyl Phosphate, Hydrogenated Palm Glycerides

Example 15: Test method 211 for determining the saponification number

Approximately 2.5 g of the substance to be investigated are weighed exactly into a 300 ml wide-necked Erlenmeyer flask, mixed with 50 ml of a mixture of equal parts by volume ether / ethanol / water (neutralized against phenolphthalein) and gently heated on a water bath (max. 35 ° C) largely solved. The Erlenmeyer flask is covered with a watch glass. The substance is not completely dissolved, only a cloudy dispersion results. Immediately after dissolving, titrate with a 0.1 N KOH solution until a slight pink color appears.

Calculation: ,, Ö * 5.61 acid number = - wa = number of milliliters used 0.1 N potassium hydroxide solution w = weight of substance in grams

Example 16: Test Method 211 Determination of the Saponification Number

Approximately 1.5 g of the sample are weighed exactly and 25.00 ml of 0.5 N ethanolic potassium hydroxide solution are added. After the addition of a boiling stone, the mixture is kept boiling under reflux for 1 hour. Then the excess of lye is titrated in the still warm mixture after adding a few drops of a 0.1% ethanolic thymolphthalein solution at 40 ° C with intensive stirring with 0.5 N sulfuric acid until the indicator changes. After adding a little more thymolphthalein solution, stirring is continued at 40 ° C. for 2 minutes. The liquid, which may become colored again, is titrated again with 0.5 N sulfuric acid until it decolorises.

A blind test should be carried out in the same way. The saponification number is calculated from the difference between the 0.5 N sulfuric acid consumed in the blind test and the main test.

Calculation:

_vz (B - H) * 28 w VZ = saponification number

B = milliliter of the 0.5 N sulfuric acid consumed in the blind test H = milliliter of the 0.5 N sulfuric acid consumed in the main test w = sample weight of the sample in grams.

Claims

claims

1. O / W emulsifier comprising: (a) hardened palm oil glycerides and (b) potassium cetyl phosphate, the proportion of potassium cetyl phosphate being in the range of 40-80% by weight, based on the total mass of the emulsifier.

2. O W emulsifier according to claim 1, wherein the emulsifier contains no polyethylene glycol (PEG) and / or no other glycol and / or no paraffin and / or no isoparaffin.

3. O / W emulsifier according to one of the preceding claims, comprising: (a) hardened palm oil glycerides, (b) potassium cetyl phosphate,

(c) cetyl alcohol and

(d) water, the proportion of potassium cetyl phosphate being in the range from 40-80% by weight, preferably 50-70% by weight, based on the total mass of the emulsifier.

4. O / W emulsifier according to one of the preceding claims, consisting of:

(a) 30-50% by weight hardened palm oil glycerides, (b) 40-50% by weight potassium cetyl phosphate,

(c) 8-15% by weight cetyl alcohol,

(d) 4-8 wt% water and

(e) 0-18% by weight of further additives, the percentages by weight relating to the total mass of the O / W emulsifier.

5. O / W emulsifier according to one of the preceding claims, wherein the O / W emulsifier is in pastille form.

6. O / W emulsifier according to one of the preceding claims, wherein the emulsifier fulfills one, more or all of the following conditions: after dissolving in neutralized water at a concentration of 10% by weight, based on the finished solution, the pH is Value in the range of 5.0 - 6.5; the saponification number at a saponification time of 1 hour is in the range of 125.0 -155.0 (test method 211) the acid number when using the solvent system diethyl ether: ethanol: water 1: 1: 1 (v / v / v) is in the range of 50.0 - 80.0 mg KOH / g (test method 228)

7. O / W emulsion comprising: a water phase, an oil phase dispersed in the water phase and

8. O / W emulsion according to claim 7, additionally comprising 0.1-10% by weight of a stabilizing agent and / or - 1-10% by weight of a co-emulsifier, the percentage by weight being based on the total mass of the O / W- Emulsion is related.

9. O / W emulsion according to claim 7 or 8, wherein the pH of the emulsion is adjusted to a value between 3 and 11, preferably between 4 and 9, more preferably between 4 and 7.

10. O / W emulsion according to any one of claims 7-9, further comprising: dispersed solids and / or

UV-A and / or UV-B filters and / or an antioxidant, and / or Perfume oils and / or other auxiliary substances

11. A method for producing an O / W emulsion according to any one of claims 7-10, comprising the following steps:

Providing a water and an oil phase providing an emulsifier according to any one of claims 1-6, incorporating the emulsifier in the water and / or in the oil phase; - After working in the emulsifier, mix the water and oil phases until the O / W emulsion is formed.