CN110897918A - Polyglycerol compound emulsifier and preparation method thereof - Google Patents
Polyglycerol compound emulsifier and preparation method thereof Download PDFInfo
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- CN110897918A CN110897918A CN201911361562.8A CN201911361562A CN110897918A CN 110897918 A CN110897918 A CN 110897918A CN 201911361562 A CN201911361562 A CN 201911361562A CN 110897918 A CN110897918 A CN 110897918A
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- polyglycerol
- stearate
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- laurate
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- 239000003995 emulsifying agent Substances 0.000 title claims abstract description 57
- 229920000223 polyglycerol Polymers 0.000 title claims abstract description 28
- 150000001875 compounds Chemical class 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims abstract description 46
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 claims abstract description 38
- POULHZVOKOAJMA-UHFFFAOYSA-M dodecanoate Chemical compound CCCCCCCCCCCC([O-])=O POULHZVOKOAJMA-UHFFFAOYSA-M 0.000 claims abstract description 29
- 229940070765 laurate Drugs 0.000 claims abstract description 29
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229960000541 cetyl alcohol Drugs 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims description 29
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002537 cosmetic Substances 0.000 abstract description 5
- 230000014759 maintenance of location Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 230000035699 permeability Effects 0.000 abstract description 2
- 230000037380 skin damage Effects 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 239000000839 emulsion Substances 0.000 description 30
- 238000012360 testing method Methods 0.000 description 15
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 7
- 239000003921 oil Substances 0.000 description 7
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000002202 Polyethylene glycol Substances 0.000 description 5
- 150000002148 esters Chemical class 0.000 description 5
- 230000007794 irritation Effects 0.000 description 5
- 229920001223 polyethylene glycol Polymers 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 210000003837 chick embryo Anatomy 0.000 description 4
- 229940075529 glyceryl stearate Drugs 0.000 description 4
- 230000000475 sunscreen effect Effects 0.000 description 4
- 239000000516 sunscreening agent Substances 0.000 description 4
- 238000004945 emulsification Methods 0.000 description 3
- XYTHHAXRVHHXKO-JIUYZRCGSA-N 18-[(2r,3s,4r,5r)-4,5-dihydroxy-2-(hydroxymethyl)-6-methoxyoxan-3-yl]oxyoctadecanoic acid;ethanol Chemical compound CCO.COC1O[C@H](CO)[C@@H](OCCCCCCCCCCCCCCCCCC(O)=O)[C@H](O)[C@H]1O XYTHHAXRVHHXKO-JIUYZRCGSA-N 0.000 description 2
- 206010022998 Irritability Diseases 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229940073639 ceteareth-6 Drugs 0.000 description 2
- 210000003711 chorioallantoic membrane Anatomy 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229940100460 peg-100 stearate Drugs 0.000 description 2
- 229940032067 peg-20 stearate Drugs 0.000 description 2
- 230000002792 vascular Effects 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- 206010053567 Coagulopathies Diseases 0.000 description 1
- 241000272201 Columbiformes Species 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 206010015946 Eye irritation Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000035602 clotting Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 231100000013 eye irritation Toxicity 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- -1 polydimethylsiloxane Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 238000009751 slip forming Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 230000002110 toxicologic effect Effects 0.000 description 1
- 231100000027 toxicology Toxicity 0.000 description 1
- 239000002569 water oil cream Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/39—Derivatives containing from 2 to 10 oxyalkylene groups
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/37—Esters of carboxylic acids
- A61K8/375—Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/10—Washing or bathing preparations
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
- A61K2800/30—Characterized by the absence of a particular group of ingredients
- A61K2800/33—Free of surfactant
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/592—Mixtures of compounds complementing their respective functions
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/592—Mixtures of compounds complementing their respective functions
- A61K2800/5922—At least two compounds being classified in the same subclass of A61K8/18
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Emergency Medicine (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Dermatology (AREA)
- Cosmetics (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
The invention discloses a polyglycerol compound emulsifier and a preparation method thereof, aiming at providing a compound emulsifier which does not contain PEG and EO surfactants, does not cause skin damage in products, has the effects of mildness, cleanness, moisture retention, air permeability, oil-water commonality and the like and comprises the following components in percentage by weight: 18.0-22.0% of polyglycerol-10 stearate, 10.0-18.0% of cetyl alcohol, 45.0-55.0% of polyglycerol-10 laurate and 10.0-20.0% of glycerol stearate, wherein the sum of the components is 100%; the HLB value of the emulsifier is 9-13; belongs to the technical field of cosmetics.
Description
Technical Field
The invention discloses a compound emulsifier, in particular to a polyglycerol compound emulsifier, and also discloses a preparation method of the emulsifier.
Background
Emulsifiers are substances which improve the surface tension between the various constituent phases of an emulsion to form a uniform and stable dispersion or emulsion. The molecule of the oil-water emulsion has both hydrophilic group and lipophilic group, and the hydrophilic group and the lipophilic group are gathered on an oil/water interface, so that the interfacial tension can be reduced, the energy required for forming the emulsion can be reduced, and the energy of the emulsion can be increased.
In order to avoid cosmetic delamination and system instability, emulsifiers are usually added during the preparation of emulsion-type cosmetics. In the existing cosmetics, PEG-20 methyl glucose sesquistearate, PEG-20 stearate, PEG-100 stearate and the like are generally used as PEG (polyethylene glycol) type emulsifiers, ceteareth 6, ceteareth 25 and the like are used as emulsifiers, the emulsifiers are EO (ethylene oxide) type emulsifiers, the emulsion stability of the product is weak, the addition amount is high, the compounding cost is low, and the product contains dioxane, so that the product has irritation to skin, is easy to cause skin allergy, and has carcinogenic risk after long-term use.
The polyglycerol emulsifier has the advantages of small irritation to skin and the like, but when the single component is used as the emulsifier, the problems that the HLB value of polyglycerol-10 stearate is 9, although the microemulsion can be prepared, the moisture retention is strong, the single emulsifying property is poor, the demulsification of the product is quick, the product needs to be compounded with the polyglycerol ester emulsifier with high HLB value for use, and the effective period of the product is less than 1 year generally exist. The wax alcohol O/W type emulsion has the functions of stabilization and thickening in a matrix oil phase; the HLB value of the polyglycerol-10 laurate is 15, the cleaning capability of the polyglycerol-10 laurate is strong when the polyglycerol-10 laurate is used singly, and the prepared emulsion has bubbles, but the stability is poor and the polyglycerol-10 laurate is easy to crystallize under the low-temperature condition and needs to be compounded with a polyglycerol emulsifier with a low HLB value for use. The HLB value of the glyceryl stearate is 3.8, the glyceryl stearate is singly used to form a W/O type emulsion, the stability is poor under the low-temperature condition, and the emulsion breaking is easy, so the researchers cause great trouble in the experimental process.
Disclosure of Invention
In view of the above disadvantages, the present invention aims to provide a compound emulsifier without PEG and EO surfactants, which does not cause skin damage in products and has the effects of mildness, cleanness, moisture retention, air permeability, oil-water compatibility, etc.
Therefore, the first technical scheme provided by the invention is as follows:
a polyglycerol compound emulsifier comprises the following components in percentage by weight: 18.0-22.0% of polyglycerol-10 stearate, 10.0-18.0% of cetyl alcohol, 45.0-55.0% of polyglycerol-10 laurate and 10.0-20.0% of glycerol stearate, wherein the sum of the components is 100%; the HLB value of the emulsifier is 9-13.
Further, the polyglycerol compound emulsifier comprises the following components in percentage by weight: 10-22% of polyglycerol-10 stearate, 12-18% of cetyl alcohol, 50-55% of polyglycerol-10 laurate and 13-18% of glycerol stearate, wherein the sum of the components is 100%; the HLB value of the emulsifier is 9-13.
Further, the polyglycerol compound emulsifier comprises the following components in percentage by weight: 18.0% of polyglycerol-10 stearate, 18.0% of cetyl alcohol, 50.0% of polyglycerol-10 laurate and 14.0% of glycerol stearate.
Further, the polyglycerol compound emulsifier comprises the following components in percentage by weight: 22.0% of polyglycerol-10 stearate, 15.0% of cetyl alcohol, 45.0% of polyglycerol-10 laurate and 18.0% of glycerol stearate.
Further, the polyglycerol compound emulsifier comprises the following components in percentage by weight: 20.0% of polyglycerol-10 stearate, 12.0% of cetyl alcohol, 55.0% of polyglycerol-10 laurate and 13.0% of glycerol stearate.
The second technical scheme provided by the invention is as follows:
the preparation method of the polyglycerol compound emulsifier sequentially comprises the following steps:
1) weighing each component;
2) adding the cetyl alcohol weighed in the step 1) into a reaction kettle, stirring and heating at a speed of 15-18 r/min to 75-78 ℃, and completely dissolving and transparent for later use;
3) stirring the glycerol stearate weighed in the step 1) in a reaction kettle at a speed of 15-18 r/min, heating to 75-78 ℃ at a constant temperature, stirring for 30min until the glycerol stearate is completely dissolved, and naturally cooling to 60-62 ℃ for later use;
4) putting the polyglycerol-10 stearate weighed in the step 1) into a reaction kettle, stirring at a speed of 15-18 r/min, heating to 73-75 ℃, stirring for 30min until the polyglycerol-10 stearate is completely dissolved, and naturally cooling to 60-62 ℃ for later use;
5) weighing polyglycerol-10 laurate into a reaction kettle, stirring at a speed of 15-18 r/min, keeping the temperature at 68-73 ℃, stirring for 30min until the polyglycerol-10 laurate is completely dissolved, and naturally cooling to 60-62 ℃ for later use;
6) the stirring speed is controlled to be 15-18 r/min; uniformly mixing the cooled spare parts in the steps 2) to 5), and pouring the mixture into a mould to be rapidly cooled until the mixture is completely molded.
Compared with the prior art, the technical scheme provided by the invention has the following technical advantages:
1. the polyglycerol-10 stearate and polyglycerol-10 laurate adopted in the technical scheme provided by the invention both contain ten cyclic aggregation structures of glycerol, a film formed on the skin is a three-dimensional and air-permeable structure, the entering of water molecules is double-sided, the structure is different from that of a common oil ester film, and meanwhile, the structure is a multi-branched structure, pores cannot be blocked like other oil esters, the oil esters are continuously formed into a film but do not retain moisture, and water can retain moisture but do not form a film. Can continuously form a film on the skin. Through hydrogen bond association, the cage type water-locking material also has high moisture retention.
2. According to the technical scheme provided by the invention, polyglycerol-10 stearate, polyglycerol-10 laurate and glycerol stearate are cooperatively combined, the glycerol-10 stearate and the polyglycerol-10 laurate are linear emulsifiers with ten unit glycerol chain lengths, and the glycerol stearate is an oligomer emulsifier with a branch structure formed by polymerization of multiple glycerol, so that the HLB value is 9-13, the additive amount of 1% can be respectively 15-18% of mineral oil, 8-10% of polydimethylsiloxane silicone oil and 10-12% of ester grease, and the cleaning agent has a strong cleaning function on W/O type products.
3. The technical scheme provided by the invention is simple to prepare and convenient to produce and use.
Detailed Description
The following claims are provided to illustrate the invention in further detail with reference to specific embodiments, but not to limit the invention in any way.
Example 1
The invention provides a polyglycerol compound emulsifier which comprises the following components in percentage by weight: 18.0% of polyglycerol-10 stearate, 18.0% of cetyl alcohol, 50.0% of polyglycerol-10 laurate and 14.0% of glyceryl stearate, wherein the HLB value is as follows: 9.6
Example 2
The invention provides a polyglycerol compound emulsifier which comprises the following components in percentage by weight: 22.0% of polyglycerol-10 stearate, 15.0% of cetyl alcohol, 45.0% of polyglycerol-10 laurate and 18.0% of glycerol stearate, wherein the HLB value is as follows: 9.4
Example 3
The invention provides a polyglycerol compound emulsifier which comprises the following components in percentage by weight: 20.0% of polyglycerol-10 stearate, 12.0% of cetyl alcohol, 55.0% of polyglycerol-10 laurate and 13.0% of glycerol stearate, wherein the HLB value is as follows: 10.5
Example 4
The invention provides a polyglycerol compound emulsifier which comprises the following components in percentage by weight: 20% of polyglycerol-10 stearate, 10.0% of cetyl alcohol, 50% of polyglycerol-10 laurate and 20.0% of glyceryl stearate, wherein the HLB value of the emulsifier is 10.
Example 5
The invention provides a polyglycerol compound emulsifier which comprises the following components in percentage by weight: 22.0% of polyglycerol-10 stearate, 15% of cetyl alcohol, 53% of polyglycerol-10 laurate and 10.0% of glycerol stearate; the HLB value of the emulsifier is 10.3.
The preparation method of the polyglycerol compound emulsifier sequentially comprises the following steps:
1) weighing the components according to any one group of the weight percentages in the embodiments 1 to 5;
2) adding the cetyl alcohol weighed in the step 1) into a reaction kettle, stirring and heating at a speed of 15-18 r/min to 75-78 ℃, and completely dissolving and transparent for later use;
3) stirring the glycerol stearate weighed in the step 1) in a reaction kettle at a speed of 15-18 r/min, heating to 75-78 ℃, stirring for 30min, and completely dissolving;
4) putting the polyglycerol-10 stearate weighed in the step 1) into a reaction kettle, stirring at a speed of 15-18 r/min, heating to 73-75 ℃, stirring for 30min until the polyglycerol-10 stearate is completely dissolved;
5) weighing polyglycerol-10 laurate into a reaction kettle, stirring at a speed of 15-18 r/min, keeping the temperature at 68-73 ℃, and stirring for 30min until the polyglycerol-10 laurate is completely dissolved;
6) naturally cooling to 60-62 ℃, and controlling the stirring speed at 15-18 r/min; mixing the cooled polyglycerin, pouring into a mold, rapidly cooling, and sequentially pouring to completely mold.
In order to prove the effect of the technical scheme provided by the application, the following comparison of the polyglycerol compound emulsifier provided by the application and the emulsifier sold in the market added to the emulsion for the emulsification test is given as follows:
OZ001 represents the formulated emulsifier provided in example 1 of representative 1.
1.1 production Process of emulsions 1 to 5:
1) weighing the group A raw materials into a beaker 1, and heating to 78-83 ℃ to dissolve uniformly for later use;
2) weighing the raw materials in the group B into a beaker 2, stirring and heating at the speed of 25r/min to 85-85 ℃, and homogenizing for 1 minute to obtain transparent liquid;
3) slowly adding the dissolved raw materials of group A into group B, stirring at 30r/min, homogenizing for 3min, and keeping the temperature for 10 min;
4) cooling and stirring at the speed of 25 r/min;
5) cooling to 45 deg.C, weighing group C materials into group AB, and stirring at25 r/min for 5 min to obtain white emulsion;
6) weighing the raw materials of the group D, adding the raw materials into ABC, and stirring the mixture for 5 minutes at the speed of 25r/min to obtain white emulsion.
7) And (4) carrying out sample separation treatment on the prepared emulsion according to the inspection requirement, and reserving 100ml of samples.
The homogenizer used in the experiment was IKAT25DS25, Germany, and the stirrer was IKARW20DS25, Germany.
1.2 the results of the test according to the physical and chemical indexes of the five emulsions are as follows:
1.2.1 the test instruments were as follows:
1.2.1.1 pH meter: shanghai apparatus and Electrical science apparatus, model: PHS-3C
1.2.1.2 digital rotational viscometer: ziboson source electric limited, model: NDJ-8S, measurement Range: 1-2000000 mPa · s, measurement accuracy: 2% (newtonian liquid).
1.2.1.3 Low speed bench centrifuge: shanghai an pavilion scientific instrument factory (flying pigeon brand), model: TDL-80-2B, the highest rotating speed is 4000r/min, the maximum centrifugal force is 2325 Xg, and the specification is as follows: 20ml × 12
1.2.1.4 refrigerator: the American brand, the model: BCD-169CM (E)
1.2.1.5 electric heating constant temperature incubator: shanghai right instruments ltd, model: DHP-9082(B)
1.3 comparing the results of the physical and chemical index tests of the five emulsions, wherein the appearance and the pH value are both in a control range, and the viscosity is different according to different viscosities of the emulsifiers; in the stability centrifugal test, the emulsions 1, 2 and 3 are layered, the emulsion 4 slightly produces oil, and the emulsion 5 is not layered; the emulsions 1, 2 and 3 have the phenomenon of layering in the stability cold resistance test, the emulsion 4 has the phenomenon of micro oil yielding, and the emulsion 5 has no layering; the emulsions 1, 2 and 3 have the layering phenomenon in the stability heat resistance test, the emulsions 4 and 5 have no layering phenomenon, the emulsions 1, 2 and 3 have the color-changing layering phenomenon in the illumination, and the emulsions 4 and 5 have no layering and color-changing phenomena; by the comparison, the five emulsions were added at the same amount of 1% emulsifier, and emulsion 4 was compounded with ceteareth (EO) type emulsifier 1: 1, the most stable emulsion 5 was tested using OZ001 emulsifier.
1.3 trial experience testing
The skin feel of the five emulsion products was experienced by 16 people selected at the department of general sales, with the following results:
2.1 compatibility with chemical sunscreens
2.1.1 selection of chemical sunscreens for emulsification comparison is as follows.
2.1.2 the production process is the same as 1.1;
2.2, performing physical and chemical index inspection according to five indexes of 2.1.
2.2.1 the test equipment is the same as 1.2.1;
2.2.2 conclusion: the sunscreen solutions 1, 2, 3 and 4 are emulsified in a compounding manner, after oil-water phase emulsification, a demulsification phenomenon starts to occur when the temperature is reduced to below 55 ℃, and the sunscreen solution 5 is tested with 1% of OZ001 emulsifier and is not unstable through stability tests.
3. The polyglycerol compound emulsifier prepared by the invention and the commercially available emulsifier containing PEG and EO are tested according to the internal toxicological safety evaluation standard of the company, and the analysis center of Guangzhou Ezepine biotechnology Limited company is entrusted to test according to the SN/T2329-2009 cosmetic eye irritation/corrosiveness chick embryo chorioallantoic membrane test, and the report numbers are as follows: AZ-RP-04-1912: 001, the mildness of the product is evaluated mainly by a chick embryo chorioallantoic membrane vascular test (CAMVA), the test concentration is 3%, the action time is 3min, and the specific conclusion is as follows:
3.1 evaluation criteria: score per chick embryo-the sum of the extent of bleeding, clotting and vascular thawing observed per chick embryo; ES-the average of the mathematical sum of the scores of 6 chick embryos. The ocular irritancy of the test subjects was classified according to the ES values as follows.
| ES | Determination of results |
| ≤12 | Non/light irritability |
| 12＜ES＜16 | Moderate irritation |
| ≥16 | Strong irritation/corrosion |
3.2 conclusion: according to AZ-RP-04-1912: 001 test results 3% strength solutions, 3min duration of action, PEG-20 methyl glucose sesquistearate, PEG-20 stearate, PEG-100 stearate, ceteareth 6, with moderate irritability; ceteareth 25 is highly irritating/corrosive; the lowest ES value of the emulsifier (OZ001) of the polyglycerol combination of the invention is consistent with no/slight irritation, i.e. the product is superior to the commercial emulsifier containing PEG and EO.
Claims (6)
1. The polyglycerol compound emulsifier is characterized by comprising the following components in percentage by weight: 18.0-22.0% of polyglycerol-10 stearate, 10.0-18.0% of cetyl alcohol, 45.0-55.0% of polyglycerol-10 laurate and 10.0-20.0% of glycerol stearate, wherein the sum of the components is 100%; the HLB value of the emulsifier is 9-13.
2. The polyglycerol compound emulsifier according to claim 1, which is characterized by comprising the following components in percentage by weight: 10-22% of polyglycerol-10 stearate, 12-18% of cetyl alcohol, 50-55% of polyglycerol-10 laurate and 13-18% of glycerol stearate, wherein the sum of the components is 100%; the HLB value of the emulsifier is 9-13.
3. The polyglycerol compound emulsifier according to claim 1, which is characterized by comprising the following components in percentage by weight: 18.0% of polyglycerol-10 stearate, 18.0% of cetyl alcohol, 50.0% of polyglycerol-10 laurate and 14.0% of glycerol stearate.
4. The polyglycerol compound emulsifier according to claim 1, which is characterized by comprising the following components in percentage by weight: 22.0% of polyglycerol-10 stearate, 15.0% of cetyl alcohol, 45.0% of polyglycerol-10 laurate and 18.0% of glycerol stearate.
5. The polyglycerol compound emulsifier according to claim 1, which is characterized by comprising the following components in percentage by weight: 20.0% of polyglycerol-10 stearate, 12.0% of cetyl alcohol, 55.0% of polyglycerol-10 laurate and 13.0% of glycerol stearate.
6. The preparation method of the polyglycerol compound emulsifier of claim 1, which is characterized by sequentially comprising the following steps:
1) weighing the components according to the weight percentage of claim 1;
2) adding the cetyl alcohol weighed in the step 1) into a reaction kettle, stirring and heating at a speed of 15-18 r/min to 75-78 ℃, and completely dissolving and transparent for later use;
3) stirring the glycerol stearate weighed in the step 1) in a reaction kettle at a speed of 15-18 r/min, heating to 75-78 ℃ at a constant temperature, stirring for 30min until the glycerol stearate is completely dissolved, and naturally cooling to 60-62 ℃ for later use;
4) putting the polyglycerol-10 stearate weighed in the step 1) into a reaction kettle, stirring at a speed of 15-18 r/min, heating to 73-75 ℃, stirring for 30min until the polyglycerol-10 stearate is completely dissolved, and naturally cooling to 60-62 ℃ for later use;
5) weighing polyglycerol-10 laurate into a reaction kettle, stirring at a speed of 15-18 r/min, keeping the temperature at 68-73 ℃, stirring for 30min until the polyglycerol-10 laurate is completely dissolved, and naturally cooling to 60-62 ℃ for later use;
6) controlling the stirring speed at 15-18 r/min, uniformly mixing the cooled spare parts in the steps 2) to 5), and pouring the mixture into a mold for rapidly cooling until the mixture is completely molded.
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| CN113730294A (en) * | 2021-10-25 | 2021-12-03 | 广州市科能化妆品科研有限公司 | Makeup removing lotion and preparation method thereof |
| CN116407457A (en) * | 2023-04-07 | 2023-07-11 | 广州弗曼生物科技有限公司 | Emulsifier composition containing polyglycerol ester and sucrose ester and application thereof |
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