MICROCAPSULES

Abstract

The present invention relates to microcapsules comprising a capsule core and a capsule shell wherein the capsule shell comprises a core surrounding layer of a polyvinyl alcohol and an adjacent layer of a polyoxazoline, a process of their production and their use.

Claims

1.-17. (canceled)

18. A microcapsule comprising a capsule core and a capsule shell wherein the capsule shell comprises a core surrounding layer of a polyvinyl alcohol and an adjacent layer of a polyoxazoline.

19. The microcapsule according to claim 18 wherein the capsule core comprises more than 95% by weight of the core material.

20. The microcapsule according to claim 18 wherein the capsule core is liquid at room temperature.

21. The microcapsule according to claim 18 wherein the average particle size of the capsule is from 0.5 to 80 mm.

22. The microcapsule according to claim 18 wherein the weight ratio of capsule core to capsule shell is in the range from 50:50 to 95:5.

23. The microcapsule according claim 18 wherein the polyvinyl alcohol is an anionic polyvinyl alcohol.

24. The microcapsule according to claim 18 wherein the core material is selected from the group consisting of aliphatic and aromatic hydrocarbon compounds, saturated or unsaturated C.sub.6-C.sub.30-fatty acids, fatty alcohols, C.sub.6-C.sub.30-fatty amines, C.sub.4-C.sub.30-mono-, C.sub.4-C.sub.30-di- and C.sub.4-C.sub.30-polyesters, primary, secondary or tertiary C.sub.4-C.sub.30-carboxamides, fatty acid esters, natural and synthetic waxes, halogenated hydrocarbons, natural oils, C.sub.3-C.sub.20-ketones, C.sub.3-C.sub.20-aldehydes, fragrances and aroma substances, vitamins and UV-filters.

25. The microcapsule according to claim 18, wherein the core material is selected from oil soluble UV filters (o).

26. The microcapsule according to claim 18, wherein the oil soluble UV filters (o) are selected from the group consisting of (o.sub.1) p-amino benzoic acid derivatives, (o.sub.2) salicyl acid derivatives, (o.sub.3) benzophezophenone derivatives, (o.sub.4) dibenzoylmethane derivatives, (o.sub.5) diphenylacrylates, (o.sub.6) 3-imidazol-4-yl-acryl acid and their esters; (o.sub.7) benzofurane derivatives; (o.sub.8) polymeric UV filters; (o.sub.9) cinnamic acid derivatives; (o.sub.10) camphor derivatives; (o.sub.11) hydroxyphenyl triazine derivates; (o.sub.12) benzotriazole derivatives; (o.sub.13) trianilino-s-triazine derivatives; (o.sub.14) menthyl o-aminobenzoates; (o.sub.15) homosalates; (o.sub.16) benzylidene malonates; (o.sub.17) merocyaninederivatives; (o.sub.18) phenylene bis diphenyl triazines; (o.sub.19) imidazoline derivatives; and (o.sub.20) diaryl butadiene derivatives.

27. The microcapsule according to claim 18, wherein the oil soluble UV filters (o) are selected from the group consisting of (o.sub.SOL-1) Benzophenone-3 (BP3); (o.sub.SOL-2) Benzophenone-4 (BP4); (o.sub.SOL-3) 3-Benzydilene Camphor (3BC); (o.sub.SOL-4) Bis-Ethylhexyloxyphenol Methoxyphenyl Triazine (BEMT); (o.sub.SOL-5) Butyl Methoxydibenzoylmethane (BMBM); (o.sub.SOL-6) Diethylhexyl Butamido Triazone (DBT); (o.sub.SOL-7) Drometrizole Trisiloxane (DTS); (o.sub.SOL-8) Ethylhexyl Triazone (EHT); (o.sub.SOL-9) Ethylhexyl Methoxycinnamate; (o.sub.SOL-10) Benzylidene malonate (BM); (o.sub.SOL-11) Diethylamino Hydroxy Benzoyl Hexyl Benzoate (DHHB); (o.sub.SOL-12) Octocrylene; (o.sub.SOL-13) Polysilicon-15; (o.sub.SOL-14) Homosalate; and (o.sub.SOL-15) Ethylhexyl salicylate.

28. The microcapsule according to claim 18, wherein the oil soluble UV filters (o) are selected from the group consisting of (o.sub.9a) Ethylhexyl Methoxycinnamate, (o.sub.11a) Bis-Ethylhexyloxyphenol Methoxyphenyl Triazine, (o.sub.13a) Ethylhexyl Triazone and (o.sub.3a) Diethylamino Hydroxy Benzoyl Hexyl Benzoate.

29. The microcapsule according to claim 18, wherein the polyvinyl alcohol is an anionic polyvinyl alcohol which acid groups are selected from the group consisting of sulfonic acid groups, phosphonic acid groups and carboxylic acids groups having 3 to 8 carbon atoms in a molecule, and/or the alkali metal, alkaline earth metal or ammonium salts thereof.

30. The microcapsule according to claim 18, wherein the polyvinyl alcohol is an anionic polyvinyl alcohol with a degree of hydrolysis of from 60 to 100%.

31. The microcapsule according to claim 18, wherein the polyoxazoline consists in polymerized form of oxazoline monomer (A) according to formula ##STR00049## wherein R is selected from the group consisting of hydrogen, linear or branched alkyl and optional one or more further oxazoline monomer (B) of formula (I), wherein the R of monomer (B) is selected from the group consisting of hydrogen, linear or branched alkyl but is different from the R of monomer (A).

32. A process for producing microcapsules with a capsule wall and a capsule core, comprising the process steps: a) preparing an oil-in-water emulsion with a disperse phase which comprises the core material and an aqueous continuous phase and an polyvinyl alcohol and b) subsequently adding one or more polyoxazoline.

33. An aqueous dispersion comprising 5 to 50% by weight, based on the total weight of the dispersion, of microcapsules according to claim 18.

34. A process for protecting human hair and skin from the harmful effect of UV radiation which comprises applying the microcapsule according to claim 18 to the skin or the hair.

Description

EXAMPLES

[0315] The particle size of the microcapsule dispersion is determined using a Malvern Particle Sizer model 3600E or a Malvern Mastersizer 2000 in accordance with a standard measuring method which is documented in the literature. The D[v, 0.1] value means that 10% of the particles have a particle size (in accordance with the volume average) up to this value. Accordingly, D[v, 0.5] means that 50% of the particles and D[v, 0.9] means that 90% of the particles have a particle size (according to the volume average) less than/equal to this value. The span value arises from the quotient from the difference D[v, 0.9]−D[v, 0.1] and D[v, 0.5]. The D[4.3] value is the weight-average.

Measurement of the Solid Content

[0316] The fraction of nonvolatile components (solid content) of the resulting dispersion is measured with a Ohaus Halogen Moisture Analyzer. The instrument operates on the thermogravimetric principle: the sample is heated to weight constant (drying temperature: 140° C.).

Leakage Evaluation

[0317] For the leakage evaluation a known amount of capsule dispersion is stored for 3 days in 5 weight % sodium dodecyl sulfate solution (SDS) at 50° C. temperature. After this time the slurry is extracted 3 times with cyclohexane. Next, the solvent is evaporated and the residue is gravimetrically analyzed.

Capsules Dispersion Stability Shelf-Life Evaluation

[0318] The capsule dispersion is stored at room temperature (20° C.) for 3 month in the graduated measuring glass. After this time the separation of dispersion is quantitatively measured.

Viscosity

[0319] Viscosity values of PVAs are the values of a 4 weight % aqueous solution determined at 20° C. by Brookfield viscometer.

Encapsulation of Perfume Oils

Example 1

[0320] A premix (I) containing 12.5 g of itaconic acid-modified anionic PVA (Mowiol® KL-318, Kuraray with hydrolysis degree 85%-90% and visc. 20.0-30.0 mPas) and 274.2 g of water is prepared. Next it is poured into 150 g of Citronellyl isobutyrate and emulsified with the help of a Mig stirrer at room temperature for 30 minutes at a speed of 800 rpm. Premix (II) containing 19.2 g of (Poly-(ethyl-stat.-methyl)-oxazoline (4:1)) and 17.8 g of water is prepared. Premix (II) is next added to the emulsion of premix (I) and Citronellyl isobutyrate over the course of 5 minutes. The reaction mixture is then stirred at room temperature for 30 minutes resulting in the desired microcapsule dispersion with a fraction of nonvolatile components of 37.9% and a particle size distribution according to the following values: d 50=7 μm and d 90=9 μm.

Example 2

[0321] A premix (I) is prepared from 12.5 g of itaconic acid-modified anionic PVA (Mowiol® KL-318, Kuraray with hydrolysis degree 85%-90% and visc. 20.0-30.0 mPas) and 274.2 g of water. Next it is poured into 150 g of Ethyl laurate and emulsified with the support of a Mig stirrer at room temperature for 30 minutes at a speed of 700 rpm. Premix (II) is prepared from 19.2 g of (Poly-(ethyl-stat.-methyl)-oxazolin(4:1)) and 17.8 g of water. Next it is added to the formed emulsion of premix (I) and Ethyl laurate over the course of 5 minutes. The reaction mixture is then stirred at room temperature for 30 minutes resulting in the desired microcapsule dispersion with a fraction of nonvolatile components of 38.1% and a particle size distribution according to the following values: d 50=9 μm and d 90=15 μm.

Example 3

[0322] 150 g of DL-Menthol is pre-heated to 40° C. A premix (I) is prepared from 12.5 g of itaconic acid-modified anionic PVA (Mowiol® KL-318, Kuraray with hydrolysis degree 85%-90% and visc. 20.0-30.0 mPas) and 274.2 g of water. The premix (I) is heated to 40° C. and is next poured into 150 g of DL-Menthol and emulsified with help of a Mig stirrer for 50 minutes at 40° C. at a speed of 800 rpm. Premix (II) is prepared from 19.2 g of polymethyloxazoline (3.8 kg/mol) and 17.8 g of water. Next it is added to the formed emulsion of premix (I) and DL-Menthol over the course of 5 minutes. The reaction mixture is then stirred at 40° C. for 30 minutes resulting in the desired microcapsule dispersion with a fraction of nonvolatile components of 38.5% and a particle size distribution according to the following values: d 50=4 μm and d 90=9 μm.

Encapsulation of UV Filters

Example 4

[0323] A premix (I) is prepared from 12.5 g of itaconic acid-modified anionic PVA (Mowiol® KL-318, Kuraray with hydrolysis degree 85%-90% and visc. 20.0-30.0 mPas) and 274.2 g of water. Premix (II) is prepared from 58 g of Hexyl 2-[4-(diethylamino)-2-hydroxybenzoyl]benzoate (Uvinul A Plus, BASF) and 92 g of Phenoxyethylester (Tegosoft XC, Evonik). Premix (III) is prepared with 9.6 g of poly(ethyl-methyloxazoline) (Poly(ethyl-stat.-methyl)-oxazolin(4:1)), 4.2 kg/mol) and 17.8 g of water. Premix (II) is poured into Premix (I) and emulsified with help of a Mig stirrer for 30 minutes at room temperature at a speed of 800 rpm. Premix (III) is then added to the formed emulsion of premixes (I) and (II) over the course of 5 minutes. The reaction mixture is then stirred at room temperature for 30 minutes resulting in the desired microcapsule dispersion with a fraction of nonvolatile components of 36.9% and a particle size distribution according to the following values: d 50=5 μm and d 90=8 μm.

Example 5

[0324] A premix (I) is prepared from 12.5 g of itaconic acid-modified anionic PVA (Mowiol® KL-318, Kuraray with hydrolysis degree 85%-90% and visc. 20.0-30.0 mPas) and 274.2 g of water. Premix (II) is prepared from 65 g of Hexyl 2-[4-(diethylamino)-2-hydroxybenzoyl]benzoate (Uvinul A Plus, BASF) and 85 g of 2-Ethylhexylbenzoate (Finsolv EB, Innospec). Premix (III) is prepared with 19.2 g of poly(ethyl-methyloxazoline) (Poly-(ethyl-stat.-methyl)-oxazolin(4:1), 4.2 kg/mol)) and 17.8 g of water. Premix (II) is poured into Premix (1) and emulsified with help of a Mig stirrer for 30 minutes at room temperature at a speed of 800 rpm. Premix (III) is then added to the formed emulsion

of premixes (I) and (II) over the course of 5 minutes. The reaction mixture is then stirred at room temperature for 10 minutes resulting in the desired microcapsule dispersion with a fraction of nonvolatile components of 37.4% and a particle size distribution according to the following values: d 50=9 μm and d 90=17 μm.

Example 6

[0325] A premix (I) is prepared from 12.5 g of itaconic acid-modified anionic PVA (Mowiol® KL-318, Kuraray with hydrolysis degree 85%-90% and visc. 20.0-30.0 mPas) and 202.89 g of water. Premix (II) is prepared from 65 g of Hexyl 2-[4-(diethylamino)-2-hydroxybenzoyl]benzoate (Uvinul A Plus, BASF) and 85 g of 2-Ethylhexylbenzoate (Finsolv EB, Innospec). Premix (III) is prepared with 38.4 g of poly(ethyl-methyloxazoline) (Poly-(ethyl-stat.-methyl)-oxazolin(4:1)), 4.2 kg/mol) and 71.31 g of water. Premix (II) is poured into Premix (I) and emulsified with help of a Mig stirrer for 30 minutes at room temperature at a speed of 850 rpm. Premix (III) is then added to the formed emulsion of premixes (I) and (II) over the course of 5 minutes. The reaction mixture is then stirred for 10 minutes at room temperature resulting in the desired microcapsule dispersion with a fraction of nonvolatile components of 42.31% and a particle size distribution according to the following values: d 50=8 μm and d 90=13 μm.

Example 7

[0326] A premix (I) is prepared from 12.5 g of itaconic acid-modified anionic PVA (Mowiol® KL-318, Kuraray with hydrolysis degree 85%-90% and visc. 20.0-30.0 mPas) and 202.89 g of water. Premix (II) is prepared from 24 g of 2,2′-[6-(4-methoxyphenyl)-1,3,5-triazine-2,4-diyl] bis{5-[(2-ethylhexyl)oxy]phenol} (Tinosorb S, BASF) and 126 g of 2-Ethylhexylbenzoate (Finsolv EB, Innospec). Premix (III) is prepared with 9.6 g of poly(ethyl-methyloxazoline) (Poly-(ethyl-stat.-methyl)-oxazolin(4:1), 4.2 kg/mol)) and 17.8 g of water. Premix (II) is poured into Premix (I) and emulsified with help of a Mig stirrer at room temperature for 30 minutes at a speed of 800 rpm. Premix (III) is then added to the formed emulsion of premixes (I) and (II) over the course of 5 minutes. The reaction mixture is then stirred at room temperature for 10 minutes resulting in the desired microcapsule dispersion with a fraction of nonvolatile components of 43.2% and a particle size distribution according to the following values: d 50=10 μm and d 90=17 μm.

Example 8

[0327] A premix (I) is prepared from 14.1 g of polyvinyl alcohol PVA (Mowiol® 18-88, Kuraray with hydrolysis degree 86.7%-88.7% and visc. 16-20 mPas) and 193.4 g of water. Premix (II) is prepared from 42.6 g of 2,2′-[6-(4-methoxyphenyl)-1,3,5-triazine-2,4-diyl]bis{5-[(2-ethylhexyl)oxy]phenol} (Tinosorb S, BASF) and 170.4 g of 2-Ethylhexyl salicylate. Premix (III) is prepared from 14.6 g of poly(2-ethyl-2-oxazoline) (Mw=50 kDa) and 38 g of water. Premix (II) is poured into Premix (I) and emulsified with help of a Mig stirrer for 30 minutes at room temperature at a speed of 800 rpm. Premix (III) is then added to the formed emulsion of premixes (I) and (II) over the course of 5 minutes. The reaction mixture is then stirred at room temperature for 10 minutes resulting in the desired microcapsule dispersion with a fraction of nonvolatile components of 49.26% and a particle size distribution according to the following values: d 50=13 μm and d 90=21 μm.

Example 9

[0328] A premix (I) is prepared from 19.5 g of polyvinyl alcohol PVA (Mowiol® 18-88, Kuraray with hydrolysis degree 86.7%-88.7% and visc. 16-20 mPas) and 267.3 g of water. Premix (II) is prepared from 35.6 g of 4-[[4,6-bis[[4-(2-ethylhexoxy-oxomethyl)phenyl]amino]-1,3,5-triazin-2-yl]amino]benzoic acid 2-ethylhexyl ester (Uvinul T150, BASF) and 114.4 g of lauryl lactate (Exceparl LM-LC, Kao Corporation S.A.). Premix (III) is prepared from 10.3 g of poly(2-ethyl-2-oxazoline) (Mw=50 kDa) and 26.8 g of water. Premix (II) is poured into Premix (I) and emulsified with help of a Ultra Turrax high shear disperser for 5 minutes at room temperature at a speed of 20000 rpm. Premix (III) is then added to the formed emulsion of premixes (I) and (II) over the course of 5 minutes. The reaction mixture is then stirred at room temperature for 10 minutes with help of a Mig stirrer at a speed of 800 rpm resulting in the desired microcapsule dispersion with a fraction of nonvolatile components of 34.16% and a particle size distribution according to the following values: d 50=1.0 μm and d 90=1.8 μm.

Example 10

[0329] A premix (I) is prepared from 12.5 g of polyvinyl alcohol PVA (Mowiol® 18-88, Kuraray with hydrolysis degree 86.7%-88.7% and visc. 16-20 mPas) and 274.2 g of water. Premix (II) is prepared from 59 g Hexyl 2-[4-(diethylamino)-2-hydroxybenzoyl]benzoate (Uvinul A Plus, BASF) and 92 g of Phenoxyethylester (Tegosoft XC, Evonik). Premix (III) is prepared from 38.4 g of poly(2-ethyl-2-oxazoline) (Mw=50 kDa) and 36 g of water. Premix (II) is poured into Premix (I) and emulsified with help of a Mig stirrer for 30 minutes at room temperature at a speed of 800 rpm. Premix (III) is then added to the formed emulsion of premixes (I) and (II) over the course of 5 minutes. The reaction mixture is then stirred at room temperature for 10 minutes resulting in the desired microcapsule dispersion with a fraction of nonvolatile components of 37.6% and a particle size distribution according to the following values: d 50=13 μm and d 90=22 μm.

Encapsulation of Cosmetic Oils

Example 11

[0330] A premix (I) is prepared from 12.5 g of itaconic acid-modified anionic PVA (Mowiol® KL-318, Kuraray with hydrolysis degree 85%-90% and visc. 20.0-30.0 mPas) and 274.2 g of water. Next it is poured into 150 g of caprylic/capric triglyceride cosmetic oil (Myritol 318, BASF) and emulsified with help of a Mig stirrer at room temperature for 30 minutes at a speed of 700 rpm. Premix (II) is prepared from 9.6 g of polyethyl-methyloxazoline (Poly-(ethyl-stat.-methyl)-oxazolin(2:3), 4.4 kg/mol)) and 17.8 g of water. It is next added to the formed emulsion of premix (I) and caprylic/capric triglyceride cosmetic oil over the course of 1 minute. The reaction mixture is then stirred at room temperature for 30 minutes resulting in the desired microcapsule dispersion with a fraction of nonvolatile components of 37.1% and a particle size distribution according to the following values: d 50=7 μm and d 90=15 μm.

Example 12

[0331] A premix (I) is prepared from 12.5 g of itaconic acid-modified anionic PVA (Mowiol® KL-318, Kuraray with hydrolysis degree 85%-90% and visc. 20.0-30.0 mPas) and 274.2 g of water. Next it is poured into 150 g of caprylic/capric triglyceride cosmetic oil (Myritol 318, BASF) and emulsified with help of a Mig stirrer for 45 minutes at room temperature at a speed of 900 rpm. Premix (II) is prepared from 9.6 g of polymethyloxazoline (3.8 kg/mol) and 17.8 g of water. Next it is added to the formed emulsion of premix (I) and caprylic/capric triglyceride cosmetic oil over the course of 5 minutes. The reaction mixture is then stirred for 30 minutes at room temperature resulting in the desired microcapsule dispersion with a fraction of nonvolatile components of 36.9% and a particle size distribution according to the following values: d 50=3 μm and d 90=6 μm.

Example 13

[0332] A premix (I) is prepared from 12.5 g of itaconic acid-modified anionic PVA (Mowiol® KL-318, Kuraray with hydrolysis degree 85%-90% and visc. 20.0-30.0 mPas) and 274.2 g of water. Next it is poured into 150 g of modified coconut oil (Myritol 331, BASF), and emulsified with help of a Mig stirrer at room temperature for 30 minutes at a speed of 700 rpm. Premix (II) is prepared from 9.6 g of (Poly-(ethyl-stat.-methyl)-oxazolin(4:1)) and 17.8 g of water. Next it is added to the formed emulsion of premix (I) and modified coconut cosmetic oil over the course of 5 minutes. The reaction mixture is then stirred for 10 minutes at room temperature resulting in the desired microcapsule dispersion with a fraction of nonvolatile components of 36.9% and a particle size distri-distribution according to the following values: d 50=8 μm and d 90=16 μm.

Formulation Examples

[0333] Cosmetic sunscreen formulations are prepared with capsule dispersions as prepared in examples 4-10.

[0334] Formulations 1, 2 and 3 comprising a capsule dispersion containing UV-filter Uvinul A Plus:

TABLE-US-00005 amount % w/w (as supplied) Tradename INCI-Name F1 F2 F3 Part A Uvinul ® MC 80 Ethylhexyl Methoxy- 8.00 8.00 8.00 cinnamate Cetiol ® C5 Coco-Caprylate 4.00 4.00 4.00 Eumulgin Prisma Disodium Cetearyl 0.30 0.30 0.30 Sulfosuccinate Part B Water 52.3 52.3 52.3 Part C Luvigel ® EM Caprylic/Capric 4.00 4.00 4.00 Triglyceride (and) Sodium Acrylates Copolymer Part-D microcapsule dispersion according to Example 4 30.4 microcapsule dispersion according to Example 5 30.4 microcapsule dispersion according to Example 6 30.4 Protectol PE Phenoxyethanol 1.00 1.00 1.00 Specification pH start 5.89 5.82 5.86 In vitro SPF Start 12 11 10 In vitro UVA-PF Start 8.4 8.5 8.3 UVA-PF/SPF >1/3 >1/3 >1/3 Viskosity RVT, 10 rpm, Sp 6 76720 32680 32980 mPa s mPa s mPa s

General Procedure:

[0335] Part A: Heat up Uvinul MC 80 to 75° C.-80° C., add Cetiol C5 and Eumulgin Prisma under stirring.

[0336] Add Part B under stirring at 75° C.

[0337] Add Part C and homogenize using Turrax.

[0338] Finally add Part D under stirring.

TABLE-US-00006 amount % w/w (as supplied) Tradename INCI-Name F4 F5 F6 Part Cetiol ® CC Dicaprylyl Carbonate 5.00 5.00 5.00 A Cetiol B Dibutyl Adipate 4.00 4.00 4.00 Cetiol C5 Coco-Caprylate 3.00 3.00 3.00 Sensiva SC50 Ethylhexylglycerin 0.50 0.50 0.50 Uvinul ® MC 80 Ethylhexyl 10.00 10.00 10.00 Methoxycinnamate Tinosorb ® S Bis- 1.80 1.80 1.80 Ethylhexyloxyphenol Methoxyphenyl Triazine Part Water 36.49 36.49 36.49 B Glycerin 3.00 3.00 3.00 Eumulgin SG Sodium Stearoyl 0.80 0.80 0.80 Glutamate Edeta ® BD Disodium EDTA 0.20 0.20 0.20 Keltrol CG-RD Xantham Gum 0.20 0.20 0.20 Part microcapsule dispersion according 34.01 C to Example 4 microcapsule dispersion according 34.01 to Example 5 microcapsule dispersion according 34.01 to Example 6 Protectol PE Phenoxyethanol 1.00 1.00 1.00 Specification pH start 7.27 7.26 6.74 In vitro SPF Start 26.4 21.3 23.6 Viskosity RVT, 10 rpm, Sp 6 810 1050 8000 mPa s mPa s mPa s

General Procedure:

[0339] Heat Part A to 80° C. under stirring until everything is dissolved, cool down to room temperature. Mix Part B separately under stirring. Add cooled Part A to Part B under stirring, homogenize using Turrax. Finally add Part C under stirring.

[0340] Formulation 7 comprising a capsule dispersion containing UV-filter Tinosorb S:

TABLE-US-00007 amount % w/w (as Tradename INCI-Name supplied) Part Uvinul MC 80 Etlylhexyl Methoxycinnamate 8.00 A Uvinul A Plus Diethylamino Hydroxybenzoyl 4.00 Hexyl Benzoate Cetiol C5 Coco-Caprylate 4.00 Eumulgin Prisma Disodium Cetearyl 0.30 Sulfosuccinate Part Water 69.7 B Part Luvigel EM Caprylic/Capric Triglyceride 3.00 C (and) Sodium Acrylates Copolymer Part Microcapsule dispersion according to Example 7 10.00 D Protectol PE Phenoxyethanol 1.00 Specification pH start 6.01 In vitro SPF Start 9 In vitro UVA-PF Start 9.1 UVA-PF/SPF >1/3 Viskosity RVT, 10 24820 mPa s rpm, Sp 6

Manufacturing Instruction:

[0341] Part A: Heat up Uvinul MC 80 and Uvinul A Plus under stirring to 75° C.-80° C. until dissolved, add Cetiol C5 and Eumulgin Prisma under stirring. Add Part B under stirring at 75° C. Add Part C and homogenize using Turrax. Finally add Part D under stirring.

[0342] Formulation 8 comprising a capsule dispersion containing cosmetic oil Myritol 318:

TABLE-US-00008 amount % w/w (as Trade name INCI-Name supplied) Part Cetiol CC Dicaprylyl Carbonate 5.00 A Cetiol B Dibutyl Adipate 4.00 Cetiol C5 Coco-Caprylate 3.00 Sensiva SC50 Ethylhexylglycerin 0.50 Uvinul MC 80 Ethylhexyl Methoxycinnamate 10.00 Uvinul A Plus Diethylamino Hydroxybenzoyl 4.00 Hexyl Benzoate Tinosorb S Bis-Ethylhexyloxyphenol 1.80 Methoxyphenyl Triazine Part Water 31.49 B Glycerin 3.00 Eumulgin SG Sodium Stearoyl Glutamate 0.80 Edeta BD Disodium EDTA 0.20 Keltrol CG-RD Xantham Gum 0.20 Part Tinovis ADE Sodium Acrylates Copolymer 1.00 C (and) Hydrogenated Polydecene (and) PPG-1 Trideceth-6 Part Capsule dispersion according to Example 11 34.01 D Protectol PE Phenoxyethanol 1.00 NaOH 30% 0.38 Specification pH start 7.04 In vitro SPF Start 32.2 Viskosität RVT, 9880 mPa s 10 rpm, Sp 6

Manufacturing Instruction:

[0343] Heat Part A to 80° C. under stirring until everything is dissolved, cool down to room temperature. Mix Part B separately under stirring. Add cooled Part A to Part B under stirring, homogenize using Turrax. Add Part C using Turrax. Finally add Part D under stirring.

[0344] Formulation 9 comprising a capsule dispersion containing UV-filter Uvinul A Plus (prepared according to example 10):

TABLE-US-00009 Amount % w/w (as Tradename INC-Name supplied) Cetiol C5 Coco-Caprylate 4.00 Eumulgin Prisma Disodium Ceteary 0.30 Sulfosuccinate B Water 58.47 C Luvigel EM Caprylic/Capric Triglyceride 4.00 (and) Sodium Acrylates Copolymer microcapsule dispersion according to Example 10 32.23 Protectol PE Phenoxyethanol 1.00 Specification pH start 5.90 UVA-PF (ISO 24442) 8.3 UVA-PF/SPF 2.52 (passed) Viskosität RVT, 10 rpm, Sp 6 18400 mPa s

Manufacturing Instruction:

[0345] Part A: Heat up Cetiol C5 to 75° C.-80° C. and add Eumulgin Prisma under stirring.

[0346] Add Part B under stirring at 75° C.

[0347] Add Part C and homogenize using Turrax.

[0348] Finally add Part D under stirring.

[0349] Formulation 10 comprising a capsule dispersion containing UV-filter Uvinul A Plus (prepared according to example 10):

TABLE-US-00010 Amount % w/w (as Tradename INCI-Name supplied) Part Water 64.16 A Tinovis GTC Acrylates/Beheneth-25 2.00 Methacrylate Copolymer NaOH 30% ig 0.30 Part Tinosorb M Methylene Bis-Benzotriazolyl 2.00 B Tetramethylbutylphenol (nano) Tinosorb A2B Tris-Biphenyl Triazine 2.00 Part microcapsule dispersion according to Example 10 28.84 C Protectol PE Phenoxyethanol 1.00 Specification pH start 7.10 In silico SPF 9.8 In vitro SPF 6 In vitro UVAPF 20.8 (after irridiation) Colipa ratio passed SPF/UVAPF ≦3 Viskosität RVT, 14460 mPa s 10 rpm, Sp 6

Manufacturing Instruction:

[0350] Part A: Mix water with Tinovis GTC at room temperature, set pH to 7 with NaOH (10-30% ig).

[0351] Add Part B under stirring at RT, use Turrax if necessary. Control pH.

[0352] Add Part C under stirring.

[0353] Formulation 11 comprising a capsule dispersion containing UV-filter Uvinul A Plus (prepared according to Example 10):

TABLE-US-00011 Amount % w/w (as Tradename INCI-Name supplied) Part Dehymuls LE PEG-30 3.00 A Dipolyhdroxystearate Cetiol CC Dicaprylyl Carbonate 5.00 Uvinul MC 80 Ethylhexyl 10.00 Methoxycinnamate Uvinul A Plus Diethylamino 2.0 Hydroxybenzoyl Hexyl benzoate Neo Heliopan OS Ethylhexyl Salicylate 5.00 Part Water 8.30 B Glycerin 2.00 Sodium Chloride 1.00 Edeta BD Disodium EDTA 0.20 Part Tinosorb S Aqua Aqua, Bis- 5.00 C Ethylhexyloxyphenol Methoxyphenyl Triazine, Polymethyl Methacrylate, Sodium Laureth Sulfate, Aminomethyl Propanol Part microcapsule dispersion according to Example 10 34.00 D Xiameter PMX-0245 Cyclopentasiloxane 10.00 Cyclopentasiloxane Specification pH start 7.06 SPF (ISO 24444): 43.7 UVA-PF/SPF: 0.36 (passed)

Manufacturing Instruction:

[0354] Heat phase A and B to 80° C. under stirring. Without Cosmedia Gel CC.

[0355] Add Cosmedia Gel CC in phase A under turrax. Then add phase B into A under stirring, homogenize.

[0356] Add phase C under stirring.

[0357] Cool down to room temperature under stirring.

[0358] Add ingredients of phase D under stirring.

[0359] Continue stirring for a while.

[0360] Formulation 12 comprising a capsule dispersion containing UV-filter Tinosorb S (prepared according to example 8):

TABLE-US-00012 Amount % w/w (as Tradename INCI-Name supplied) Part Cetiol CC Dicaprylyl Carbonate 5.00 A Cetitol B Dibutyl Adipate 4.00 Cetiol C5 Coco-Caprylate 3.00 Sensiva SC50 Ethylhexylglycerin 0.50 Uvinul MC 80 Ethylhexyl Methoxycinnamate 10.00 Uvinul A Plus Diethylamino Hydroxybenzoyl 4.00 Hexyl benzoate Tinosorb S Bis-Ethylhexyloxyphenol 0.8 Methoxyphenyl Triazine Part Water 32.99 B Glycerin 3.00 Eumulgin SG Sodium Stearoyl Glutamate 0.80 Edeta BD Disodium EDTA 0.20 Keltrol CG-RD Xantan Gum 0.20 Part Tinovis ADE Sodium Acrylates Copolymer 0.5 C (and) hydrogenated Polydecane (and) PPG-1 Trideceth-6 Part microcapsule dispersion according to Example 8 34.01 D Protectol PE Phenoxyethanol 1.00 NaOH 30% 0.15 Specification pH start 7.06 SPF (ISO 24444): 25.7 UVA-PF/SPF: 0.46 (passed) Viskosität RVT, 10 rpm, Sp 6 4500 mPa s

Manufacturing Instruction:

[0361] Heat Part A to 80° C. under stirring until everything is dissolved, cool down to room temperature.

[0362] Mix Part B separately under stirring.

[0363] Add cooled Part A to Part B under stirring, homogenize using Turrax.

[0364] Add Part C using Turrax.

[0365] Finally add Part D under stirring.

[0366] Formulations 13 comprising a capsule dispersion containing UV-filter Tinosorb S (prepared according to example 8):

TABLE-US-00013 Amount % w/w (as Tradename INCI-Name supplied) Part Eumulgin SG Sodium Stearoyl Glutamate 2.00 A Cetiol AB C12-15 Alkyl Benzoate 5.00 Cetiol B Dibutyl Adipate 5.00 Uvinul N 539T Octocrylene 10.00 Neoheliopan OS Ethylhexyl Salicylate 5.00 Parsol 1789 Butyl 5.00 Methoxydibenzoylmethane Uvinul A Plus Diethylamino Hydroxybenzoyl 4.90 Hexyl benzoate Thinosorb S Bis-Ethylhexyloxyphenol 3.00 Methoxyphenyl Triazine Preservative qs Part Water 28.80 B Rheocare TTA Acrylates Copolymer 0.50 Edeta BD Disodium EDTA 0.20 Pemulen TR-2 Acrylates/C10-30 Alkyl 0.10 Polymeric Emulsifier Acrylate Crosspolymer C Water Aqua 5.00 Eusolex 232 Phenylbenzimidazole 1.50 Sulfonic Acid Tris Amino Ultra PC Tromethamine qs D microcapsule dispersion according to Example 8 20.00 Cetiol Ultimate Undecane, Tridecane 4.00 Specification pH start 7.0-7.4 SPF (ISO 24444): 57.3 UVA-PF/SPF: 0.77 (passed) Viskosität RVT, 280 mPas 10 rpm, Sp 6

Manufacturing Instruction:

[0367] Heat phase A and B to 80° C. under stirring. Add phase A into B under stirring, homogenize. Add phase C previously mixed under homogenizer. Cool down to room temperature under stirring. Then add part D and continue stirring for a while.

Specifications:

[0368] Formulations 14 comprising a capsule dispersion containing UV-filter Uvinul T 150 (example 9):

TABLE-US-00014 Amount % w/w (as Tradename INCI-Name supplied) Part Lanette O Cetyl Stearyl Alcohol 1 A Eumulgin SG Sodium Stearoyl Glutamate 2 Cetiol B Dibutyl Adipate 2 Uvinul MC80 Ethylhexyl Methoxycinnamate Uvinul A Plus Diethylamino Hydroxybenzoyl 7 Hexyl benzoate Part Water, demin. 35.8 B Glycerin 3 Edeta BD Disodium EDTA 0.2 Part Tinovis ADE Sodium Acrylates Copolymer 2 C (and) hydrogenated Polydecane (and) PPG-1 Trideceth-6 Part microcapsule dispersion (example 9) 40.00 D Protectol PE Phenoxyethanol 1 NaOH 30% ig 1.50 Specification Formulation 14 pH start 6.78 In vitro SPF 26.5 Viskosität RVT, 10 rpm, Sp 6 18600 mPa s

Manufacturing Instruction:

[0369] Warm up Part A and Part B separately to 80° C. until dissolution. Add Part A under stirring to Part B. Add Part C using Turray. Add Part D under stirring. Set pH to appr. 6.5.