CN102860922B - Preparation method of cream emulsion cosmetics without surfactant - Google Patents
Preparation method of cream emulsion cosmetics without surfactant Download PDFInfo
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- CN102860922B CN102860922B CN201210379330.7A CN201210379330A CN102860922B CN 102860922 B CN102860922 B CN 102860922B CN 201210379330 A CN201210379330 A CN 201210379330A CN 102860922 B CN102860922 B CN 102860922B
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Abstract
The invention discloses a preparation method of cream emulsion cosmetics without adding surfactant and belongs to the technical field of high polymer material and applied chemistry. Amphipathy random polymer micellar solution is used as emulsifier to replace surfactant for emulsification in cosmetics, and skin irritation caused by the surfactant in cream emulsion cosmetics is avoided. Amphipathy random polymer is prepared by copolymerization of hydrophobicity monomer methyl methacrylate and hydrophilicity monomer methacrylic acid. Under pH inducement, random polymer forms micelle in aqueous phase by self-assembling. The polymer micelle water phase is mixed with oil phases such as jojoba oil, mink oil, caprylic/capric triglyceride, white oil and silicone oil, oil-in-water type cream emulsion cosmetics are formed by shearing with a high-speed dispersion instrument, and the stability of the oil-in-water type cream emulsion cosmetics meets the requirements of cosmetics.
Description
Technical field
A preparation method that does not contain the cream frost emulsion class cosmetics of surfactant, belongs to macromolecular material and applied chemistry technical field.
Background technology
Surfactant has the series of characteristics such as moistening, emulsifying, solubilising, dispersion, decontamination, infiltration, in cosmetics, has a wide range of applications, and be its indispensable ingredient.But the safety of surfactant, particularly the zest of skin, eyes, hair is merited attention.Surfactant mainly causes by stripping property, accessibility and reactive institute the zest of mucosa, and zest to skin, think the infiltration of surfactant on skin residual be immediate cause.A. the people such as Mehling has studied the potential stimulus of surfactant to eye and skin.By Red blood corpuscle test, the test of egg-allantocherion, acute ocular irritant experiment and skin wrinkle sturdyly the surfactants such as method assessment cocoa glucoside, lauryl glucoside, lauryl alcohol glucose carboxylate, sodium laureth sulfate, sodium lauryl sulfate, ammonium lauryl sulfate such as is tested and had slightly, the even zest of severe of moderate.
Micromolecule surfactant easily causes transdermal penetration, large to skin irritation; And high molecular polymer is difficult for occurring transdermal penetration problem, and due to the impact of macromolecular secondary, tertiary structure, polar group or hydrophobic chain are difficult for, with skin, direct, strong effect occurs, thereby gentleer.
Amphipathic nature polyalcohol macromole can spontaneous formation different shape in solution micelle (as: spherical, lamellar, tubulose, fibrous, bar-shaped, stratiform, cryptomere and star-like etc.), there is the effect of emulsifying, solubilising.
The people such as Liu Xiaoya have announced a kind of preparation method (Granted publication CN 101302296 B) of amphiphilic copolymer self-assembled micelle wedding agent, and its synthetic amphiphilic copolymer dropwise adds in precipitant again and makes micelle stable after self assembly formation polymer micelle solution in selective solvent; Continue stirring and displace cosolvent or adopt volatility process to steam cosolvent by dialysis after 1-3 hour, finally obtain amphipathic copolymer assembling micellar solution.Wherein selective solvent is made up of cosolvent and precipitant, and cosolvent can be selected: dimethyl formamide, dimethyl sulfoxide, dioxane, oxolane, acetone, isopropyl acetone, butanols or mixed solvent.Precipitant is selected water, ethanol or toluene.The polymer micelle relating in the present invention is prepared without organic solvent, only need to be in alkaline aqueous solution dissolve polymer, then use Fructus Citri Limoniae acid for adjusting pH to 6 ~ 8, just can induce self assembly to form.Preparation process is simple, has avoided the use of organic solvent.
The people such as Liu Xiaoya have announced a kind of preparation method (Granted publication CN 102068392 B) of sun-proof micelle emulsifier, the water miscible random copolymer P (VM-making by radical polymerization
co-AMPS), polymer micelle can be used as sunscreen agent, but this invention does not relate to the study on the stability of emulsion.The polymer micelle emulsifying agent the present invention relates to, without surfactant compound, the cosmetics such as the cream frost of preparation, emulsion, watch box dew are investigated through cold and hot stability test, meet cosmetics stability requirement.
The polymer micelle emulsifying agent the present invention relates to, adopts the synthetic random copolymer P (MMA-of radical polymerization
co-MAA), and through pH induction, in water, self assembly forms P (MMA-
co-MAA) micelle, there is good emulsifiability.This micellar solution can emulsification cosmetic in conventional multiple oiliness raw material, skin is not had to zest, the crowd who is applicable to infant and easy responsive skin quality uses.
Summary of the invention
The object of the present invention is to provide the atactic polymer micellar solution of a kind of emulsification to substitute micromolecule surfactant for cream frost emulsion class cosmetics, eliminate the cosmetics zest problem of being brought by micromolecule surfactant, the preparation method of the cream frost emulsion class cosmetics that do not contain micromolecule surfactant is provided.
Technical scheme of the present invention: a kind of preparation method of the cream frost emulsion class cosmetics without interpolation surfactant, these cream frost emulsion class cosmetics are oil-in-water type emulsion body, emulsifying agent is a kind of amphipathic atactic polymer micellar solution, water (A) and the biphase mixing of oil phase (B) use high speed dispersion instrument to shear emulsifying under the condition of 2-6min at rotating speed 2000 ~ 30000r/min afterwards, obtain cream frost emulsion class cosmetics;
In water (A), contain the atactic polymer P (MMA-that (I) plays emulsifying agent effect
co-MAA), be to be made by hydrophobic monomer methyl methacrylate MMA and hydrophilic monomer methacrylic acid MAA random copolymerization, MMA:MAA mol ratio is 80:20 ~ 50:50, number-average molecular weight is 5000 ~ 15000 g/mol; This atactic polymer under pH induction in water self assembly form micelle, keep pH value of solution 6.0 ~ 8.0 with citric acid-sodium citrate buffer, not with an organic solvent, polymer micelle concentration is 1 ~ 10mg/mL; And (II) polyacrylic acid, (III) sodium hydroxide, (IV) polyhydric alcohol;
Oil phase (B) is at (V) 25 DEG C, to be liquid oil preparation: one or more in higher alcohols high-carbon acid esters, Trivent OCG, tricaprin, white oil, squalane, Jojoba oil, ermine oil, isopropyl myristate, isopropyl palmitate, silicone oil; And (VI) higher alcohols;
The content of the each composition of cream frost emulsion class cosmetics: composition (I): 0.1% ~ 1% polymer P (MMA-
co-MAA); Composition (II) 0.3%; Composition (III) 0.8%; Composition (IV): 2% ~ 5%; Composition (V): 1% ~ 30%; Composition (VI): 1% ~ 5%, all the other components are taking water as main.
In water (A) and oil phase (B), do not add any surfactant, the polymer P (MMA-that water (A) has comprised emulsifying agent effect
co-MAA).
The cream frost emulsion class cosmetics that make, study on the stability, at-18 DEG C of freezing 24h, recovers room temperature, then at 48 DEG C of constant temperature 24h of water proof calorstat, then return to room temperature, and so circulate 2 ~ 3 times, to recover after room temperature, emulsified body is not stratified, not fuel-displaced, keeps good stability.
Present inventor finds, the polymer micelle solution of 1 ~ 10mg/mL, polyhydric alcohol, polyacrylic acid, sodium hydroxide and at 25 DEG C for after liquid oil preparation, higher alcohols mix, with shearing through high speed disperser, can obtain stable emulsified body, the stability of the emulsified body that its stability and the emulsifying of micromolecule surfactant obtain is suitable.
According to the present invention, oil-in-water type cream frost emulsion class cosmetics contain but are not limited only to following composition (I) ~ (VI):
Water (A)
(I) polymer P (MMA-
co-MAA) solution
(II) polyacrylic acid
(III) sodium hydroxide
(IV) polyhydric alcohol
Oil phase (B)
At (V) 25 DEG C, it is liquid oil preparation
(VI) higher alcohols
The content of the each composition of cream frost emulsion class cosmetics: composition (I): 0.1% ~ 1% polymer; Composition (IV): 2% ~ 5%; Composition (V): 1% ~ 30%; Composition (VI): 1% ~ 5%.
Composition (I) is to be 80:20 ~ 50:50 by MMA:MAA mol ratio, and number-average molecular weight is the atactic polymer P (MMA-of 5000 ~ 15000 g/mol
co-MAA), the micellar solution that self assembly forms in water under pH induction, keeps pH value of solution 6.0 ~ 8.0 with citric acid-sodium citrate buffer, and polymer micelle concentration is 1 ~ 10mg/mL.
Beneficial effect of the present invention: according to the present invention, can obtain exquisiteness, stable cream frost emulsion class cosmetics, its stability is suitable with the stability of conventionally adding the emulsified body that the emulsifying of micromolecule surfactant obtains.
Brief description of the drawings
Fig. 1 P (MMA-
co-MAA) the TEM image of micelle
Fig. 2 P (MMA-
co-MAA) micelle emulsifying rear stability investigate digital photograph.
Detailed description of the invention
Oil-in-water cream frost emulsion class cosmetics of the present invention contain but are not limited only to composition (I) ~ (VI).
Composition (I) is polymer micelle solution.Atactic polymer P (MMA-
co-MAA) preparation method of micellar solution is: by appropriate polymer P (MMA-
co-MAA) be dissolved in the sodium hydroxide solution of 0.025 ~ 0.1M, its polymer concentration is 1 ~ 10mg/mL, hold over night after it dissolves completely.The polymer solution of gained is regulated to its pH to 6.0 ~ 8.0 with citric acid, and hold over night obtains polymer micelle solution.Micelle particle diameter is in nanometer category.
Composition (V) is at 25 DEG C, to be liquid oil preparation.One or more in caprylic/capric triglyceride, higher alcohols high-carbon acid esters, white oil, squalane, Jojoba oil, ermine oil, isopropyl myristate, isopropyl palmitate, silicone oil.
Embodiment 1 cream frost formula
| 16, octadecanol | 3% |
| GTCC | 2% |
| Jojoba oil | 2% |
| Squalane | 2% |
| White mineral oil | 2% |
| Isopropyl myristate | 2% |
| Butanediol | 4% |
| Hyaluronate sodium | 0.1% |
| Dimethyl siloxane | 2% |
| CARBOPOL 940 | 0.3% |
| Sodium hydroxide | 0.8% |
| Essence | 0.1% |
| Phenoxyethanol | 0.6% |
| 1% polymer solution | 79.1% |
Embodiment 2 emulsion formulations
| 16, octadecanol | 1.5% |
| GTCC | 2% |
| Jojoba oil | 1% |
| Squalane | 1% |
| Isopropyl myristate | 1% |
| Butanediol | 2% |
| Hyaluronate sodium | 0.1% |
| Dimethyl siloxane | 2% |
| Polyacrylic acid 941 | 0.3% |
| Sodium hydroxide | 0.8% |
| Essence | 0.1% |
| Phenoxyethanol | 0.5% |
| 1% polymer solution | 87.7% |
Embodiment 3 watch boxes reveal formula
| 16, octadecanol | 1.5% |
| White oil | 2% |
| Jojoba oil | 2% |
| Butanediol | 3% |
| Hyaluronate sodium | 0.05% |
| Phenoxyethanol | 0.5% |
| 1% polymer solution | 90.95% |
After being mixed with oil phase, water use high speed dispersion instrument at rotating speed 2000 ~ 30000r/min, emulsifying under the condition of shearing 2 ~ 6min.
Claims (3)
1. the preparation method without the cream frost emulsion class cosmetics of interpolation surfactant, it is characterized in that these cream frost emulsion class cosmetics are oil-in-water type emulsion body, emulsifying agent is a kind of amphipathic atactic polymer micellar solution, water (A) and the biphase mixing of oil phase (B) use high speed dispersion instrument to shear emulsifying under the condition of 2-6min at rotating speed 2000 ~ 30000r/min afterwards, obtain cream frost emulsion class cosmetics;
In water (A), contain the atactic polymer P (MMA-that (I) plays emulsifying agent effect
co-MAA), be to be made by hydrophobic monomer methyl methacrylate MMA and hydrophilic monomer methacrylic acid MAA random copolymerization, MMA:MAA mol ratio is 80:20 ~ 50:50, number-average molecular weight is 5000 ~ 15000 g/mol; This atactic polymer under pH induction in water self assembly form micelle, keep pH value of solution 6.0 ~ 8.0 with citric acid-sodium citrate buffer, not with an organic solvent, polymer micelle concentration is 1 ~ 10mg/mL; And (II) polyacrylic acid, (III) sodium hydroxide, (IV) polyhydric alcohol;
Oil phase (B) is at (V) 25 DEG C, to be liquid oil preparation: one or more in Trivent OCG, tricaprin, white oil, squalane, Jojoba oil, ermine oil, isopropyl myristate, isopropyl palmitate, silicone oil; And (VI) higher alcohols;
The content of the each composition of cream frost emulsion class cosmetics: composition (I): 0.1% ~ 1% polymer P (MMA-
co-MAA); Composition (II) 0.3%; Composition (III) 0.8%; Composition (IV): 2% ~ 5%; Composition (V): 1% ~ 30%; Composition (VI): 1% ~ 5%, all the other components are taking water as main.
2. according to claim 1 without the preparation method of cream frost emulsion class cosmetics of adding surfactant, it is characterized in that in water (A) and oil phase (B), not adding any surfactant, the polymer P (MMA-that water (A) has comprised emulsifying agent effect
co-MAA).
3. according to claim 1 without the preparation method of cream frost emulsion class cosmetics of adding surfactant, it is characterized in that the cream frost emulsion class cosmetics that make, study on the stability, at-18 DEG C of freezing 24h, recovers room temperature, then at 48 DEG C of constant temperature 24h of water proof calorstat, return to again room temperature, so circulation 2 ~ 3 times, recovers after room temperature, and emulsified body is not stratified, not fuel-displaced, keep good stability.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210379330.7A CN102860922B (en) | 2012-10-09 | 2012-10-09 | Preparation method of cream emulsion cosmetics without surfactant |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210379330.7A CN102860922B (en) | 2012-10-09 | 2012-10-09 | Preparation method of cream emulsion cosmetics without surfactant |
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| CN102860922A CN102860922A (en) | 2013-01-09 |
| CN102860922B true CN102860922B (en) | 2014-08-13 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103565676B (en) * | 2013-11-08 | 2015-08-26 | 江南大学 | The coated micelle of biostearin that a kind of amphipathic nature polyalcohol is coated and cosmetic composition |
| CN108852862B (en) * | 2018-07-11 | 2021-05-11 | 江南大学 | Multiple emulsion and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87107781A (en) * | 1986-11-10 | 1988-08-31 | B·F谷德里奇公司 | Stablize and the topical skin composition of energy fast emulsion breaking |
| CN1787803A (en) * | 2003-06-13 | 2006-06-14 | 宝洁公司 | Skin care composition comprising skin lightening agent |
| CN101283958A (en) * | 2007-04-13 | 2008-10-15 | 莱雅公司 | Cosmetic composition comprising a continuous oily phase |
| CN102085162A (en) * | 2011-01-13 | 2011-06-08 | 广州环亚化妆品科技有限公司 | Face cleansing emulsion without surfactant and preparation method thereof |
-
2012
- 2012-10-09 CN CN201210379330.7A patent/CN102860922B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87107781A (en) * | 1986-11-10 | 1988-08-31 | B·F谷德里奇公司 | Stablize and the topical skin composition of energy fast emulsion breaking |
| CN1787803A (en) * | 2003-06-13 | 2006-06-14 | 宝洁公司 | Skin care composition comprising skin lightening agent |
| CN101283958A (en) * | 2007-04-13 | 2008-10-15 | 莱雅公司 | Cosmetic composition comprising a continuous oily phase |
| CN102085162A (en) * | 2011-01-13 | 2011-06-08 | 广州环亚化妆品科技有限公司 | Face cleansing emulsion without surfactant and preparation method thereof |
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