CN112691065A - Moisturizing emulsion and preparation method thereof - Google Patents

Moisturizing emulsion and preparation method thereof Download PDF

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Publication number
CN112691065A
CN112691065A CN202110169831.1A CN202110169831A CN112691065A CN 112691065 A CN112691065 A CN 112691065A CN 202110169831 A CN202110169831 A CN 202110169831A CN 112691065 A CN112691065 A CN 112691065A
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stirring
homogenizing
extract
phase
minutes
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张俊芬
黄艺芬
黄燕红
郑福专
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Fujian Pientzehuang Cosmetics Co ltd
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Fujian Pientzehuang Cosmetics Co ltd
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Abstract

The invention belongs to the daily chemical industry, and discloses moisturizing emulsion and a preparation method thereof, wherein the moisturizing emulsion comprises pentaerythritol tetra (ethyl hexanoate), polyglycerol-10 myristate, phytosterol/octyldodecanol lauroyl glutamate; tocopherol acetate, methyl glucitol polyether-10, small molecular hyaluronic acid, Tremella fuciformis fruiting body extract, yeast/rice fermentation product filtrate, etc. The preparation method of the moisturizing emulsion can realize good dispersion of silicon elastomers in the system, and can achieve the effects of moisturizing, moistening and the like by matching with active matters in the system, thereby obviously improving the moisturizing capability of skin.

Description

Moisturizing emulsion and preparation method thereof
Technical Field
The invention relates to the field of cosmetic daily chemical skin care, in particular to a preparation method of a moisturizing emulsion.
Background
The skin is an important and largest organ covering the whole body surface, is positioned on the body surface, is not only a simple human body protection covering layer, but also has a special toxicological function; the stratum corneum is located in the outermost layer of the epidermis and one of the main functions is to prevent the loss of water, protect the structure from damage, and act as a barrier. The demand for skin care products with moisturizing effect is steadily increasing. Therefore, it is important to develop an emulsion having moisturizing effect from the viewpoint of moisturizing effect. With the attention of consumers on the skin care moisturizing function, the demand of skin care products with moisturizing effect is steadily increasing. Therefore, it is important to develop an emulsion having moisturizing effect from the viewpoint of moisturizing effect. The conventional emulsion usually contains less oil phase and moisture-retaining components, and mostly adopts a single plant-derived humectant, so that the skin feel is fresh, but usually only the cuticle of the epidermis is wetted, and the deep moisture-retaining effect is difficult to achieve; the commercial emulsion is limited by the technology, and silicon elastic substances are difficult to add to adjust the skin feel; if the content of related components such as oil phase, polyhydric alcohol and the like is increased, the problems of poor stability, sticky skin feel and the like can be caused.
Based on the above, from the aspect of moisturizing efficacy, a moisturizing emulsion which has moisturizing efficacy, refreshing skin feel and no stickiness is developed, and the problem of silicon elastic dispersion can be solved by adding the moisturizing emulsion.
Disclosure of Invention
The invention aims to provide the moisturizing emulsion capable of improving the water content of skin, and in order to overcome the defect of insufficient moisturizing of the conventional emulsion, the moisturizing formula is added, the oil phase content is increased, the silicone elasticity is increased, and the sticky feeling of the system is improved; in order to solve the problem of dispersion of the silicon bomb in an emulsion system, the invention adjusts the emulsification process, changes the adding temperature of the neutralizer potassium hydroxide and ensures the effective suspension of the silicon bomb.
In order to achieve the purpose, the embodiment of the invention is realized by the following technical scheme:
the moisturizing emulsion comprises the following raw materials in percentage by weight, the sum of the raw materials is 100 percent:
0.5-3% of pentaerythritol tetra (ethyl hexanoate), 0.2-3% of polyglycerol-10 myristate, 0.1-2% of behenyl alcohol and 0.01-2% of phytosterol/octyldodecanol lauroyl glutamate; 0.01-1% of tocopherol acetate, 101-10% of methyl glucitol polyether-101 and 0.1-10% of polyglycerol-2 stearate; 0.2-0.7% of glyceryl stearate, 0.1-3% of cetearyl alcohol, 0.01-1% of stearyl alcohol, 0.01-1% of stearic acid, 1-7% of cyclopentadimethylsiloxane, 50.5-6% of DMCM (dimethyl formamide), 1-10% of butanediol, 0.5-5% of trehalose, 0.01-0.6% of carbomer, 0.01-0.1% of disodium EDTA (ethylene diamine tetraacetic acid), 0.0005-0.1% of panax notoginseng saponins, 0.01-0.3% of micromolecular hyaluronic acid, 0.001-0.1% of tremella entity extract, 0.01-0.12% of potassium hydroxide, 0.01-0.5% of dipotassium glycyrrhizinate,
Figure BDA0002938642670000011
K3500.1-1.6%, dendrobium officinale stem extract 0.001-1%, polygonatum extract 0.001-1%, poria cocos extract 0.001-1%, radix scrophulariae extract 0.001-1%, radix ophiopogonis extract 0.001-1%, yeast/rice fermentation product filter 0.1-5%, p-hydroxyacetophenone 0.00001-0.2%, 1, 2-hexanediol 0.00001-0.2%, 1, 2-pentanediol 0.0001-0.2%, daily-use essence 0.01-1%, and the balance of deionized water 20-90%.
The preparation method of the moisturizing emulsion comprises the following steps:
preparation before operation
1) Accurately weighing the panax notoginseng saponins in a certain amount, and preparing 5-10 wt% of water solution by using deionized water solution which is boiled and cooled to room temperature for later use;
2) preparing 5-10 wt% aqueous solution C phase from potassium hydroxide by using boiled and cooled deionized water solution for later use;
heating water and oil phase
1) Putting pentaerythritol tetra (ethyl hexanoate), polyglycerol-10 myristate, behenyl alcohol, phytosterol/octyldodecanol lauroyl glutamate, tocopheryl acetate, methyl gluceth-10, polyglycerol-2 stearate, glyceryl stearate, cetostearyl alcohol, stearyl alcohol, stearic acid and DMCM-5 into an oil pan, heating to 85 +/-2 ℃ while stirring (stirring speed of 200-800 revolutions per minute), uniformly mixing, and keeping the temperature for 10-30 minutes; after the heat preservation is finished, adding cyclopentadimethylsiloxane, and uniformly stirring to obtain an oil phase A;
3) putting the rest boiled and cooled deionized water, butanediol, trehalose, carbomer, EDTA disodium, panax notoginseng saponins, micromolecular hyaluronic acid and tremella entity extract into a water pot, heating to 90 +/-2 ℃ while stirring (stirring speed is 400-800 revolutions per minute), uniformly mixing, preserving heat for 10-30 minutes, and uniformly mixing to obtain a water phase B;
homogenizing and emulsifying
1) Preheating an emulsifying pot jacket to 45-55 ℃, vacuumizing, pumping the phase A into an emulsifying pot under the stirring condition (the vacuumizing stirring speed is 20-80 rpm), and maintaining the temperature at 80-85 ℃ to perform internal circulation homogenizing stirring for 5-15 minutes (the homogenizing speed is 1000-2000 rpm, and the stirring speed is 20-80 rpm);
2) after the homogenization of the phase A is finished, starting internal circulation and vacuumizing to pump the phase B into an emulsifying pot from an upper feed inlet, carrying out external circulation homogenization after the feeding is finished, keeping the temperature of the emulsifying pot at 80-85 ℃, and stirring for 10-20 minutes (the homogenization speed is 2000-3000 r/min, and the stirring speed is 40-80 r/min);
3) after homogenizing, continuing stirring and external circulation, vacuumizing, adding the C-phase potassium hydroxide into an emulsifying pot, and homogenizing and stirring for 1-10 minutes (the homogenizing speed is 2000-3000 r/min, and the stirring speed is 40-80 r/min);
4) after homogenization, stirring is continued, the vacuumizing value is-400 to-700 mbar, and the temperature is reduced;
5) and when the temperature is reduced to 47-53 ℃, continuously stirring, starting external circulation and homogenizing (the homogenizing speed is 1000-2000 r/min, and the stirring speed is 20-80 r/min), and slowly adding the phase D from an upper feeding port: dipotassium glycyrrhizinate,
Figure BDA0002938642670000021
K350, a dendrobium officinale stem extract, a polygonatum extract, a poria cocos extract, a radix scrophulariae extract, a radix ophiopogonis extract, a yeast/rice fermentation product filter, p-hydroxyacetophenone, 1, 2-hexanediol, 1, 2-pentanediol and (daily) essence, and homogenizing for 2-8 minutes (the homogenizing speed is 1000-2000 r/min, and the stirring speed is 40-80 r/min); after homogenizing, vacuumizing to minus 600 to minus 900mbar, and continuously stirring for 2 to 10 minutes (the stirring speed is 20 to 40 revolutions per minute);
6) after homogenizing, vacuumizing to minus 600 to minus 900mbar, and continuously stirring and cooling for 2 to 10 minutes (the stirring speed is 20 to 40 revolutions per minute); discharging through 100 meshes, putting into a designated container, and warehousing for storage to obtain the finished product.
The invention has the beneficial effects that: in terms of components: the moisturizing emulsion disclosed by the invention adopts a polyglycerol emulsifier, so that the moisturizing emulsion is mild and has no stimulation; particularly, a moisturizing formula consisting of dendrobium, polygonatum, figwort, dwarf lilyturf tuber, pseudo-ginseng and tuckahoe is added to deeply moisten the skin basement; tocopherol acetate, dipotassium glycyrrhizinate and panax notoginseng saponins are added to help improve the antioxidant barrier of the skin; the yeast/rice fermentation product filter is used as a metagen to help solidify the skin micro-ecological barrier; the micromolecular hyaluronic acid can form a water-wet protective film on the surface of the skin, and the skin is repaired by permeating layer by layer; the addition of the phytosterol, behenyl alcohol and other oil and the tremella entity extract can form a protective film on the surface of the skin, help to improve physical barriers, nourish the skin in all aspects, and achieve the effects of moisturizing, refreshing and not greasy. In the aspect of the process: according to experimental verification, the emulsifier 2W with the water phase and the oil phase both soluble is added into the oil phase, so that the consistency of the product can be effectively increased, the appearance texture is improved, and the stability of the system is improved in the aspect of thickening; the potassium hydroxide is used as a neutralizer to open the chains of the carbomer, so that the effects of increasing the viscosity of the product and assisting in emulsification by suspension are achieved. Compared with the conventional emulsification process, the addition time of the neutralizer is advanced, and the neutralizer is added after being emulsified by water and oil, so that the emulsion particle size can be maintained, emulsified silicon elastomers can be suspended, and the stability of the moisturizing emulsion system is improved.
Detailed Description
In order to achieve the above purpose, the embodiment of the invention is realized by the following technical scheme.
Example 1
The moisturizing emulsion comprises the following raw materials in percentage by weight, the sum of the raw materials is 100 percent: pentaerythritol tetra (ethyl hexanoate) 0.5%, polyglycerol-10 myristate 1.5%, behenyl alcohol 1%, phytosterol/octyldodecanol lauroyl glutamate 1%; tocopherol acetate 0.05%, methyl glucitol polyether-106%, polyglycerol-2 stearate 0.1%; 0.6% of glyceryl stearate, 0.1% of cetearyl alcohol, 0.01% of stearyl alcohol, 0.05% of stearic acid, 7% of cyclopentadimethylsiloxane, DMCM-54%, 3% of butanediol, 0.5% of trehalose, 0.1% of carbomer, 0.01% of disodium EDTA, 0.005% of panax notoginseng saponins, 0.02% of micromolecular hyaluronic acid, 0.05% of tremella entity extract, 0.01% of potassium hydroxide, 0.01% of dipotassium glycyrrhizinate,
Figure BDA0002938642670000031
K3501.5%, Dendrobium officinale stem extract 0.001%, Polygonatum odoratum extract 0.001%, Poria cocos extract 0.001%, radix scrophulariae extract 0.001%, radix Ophiopogonis extract 0.001%, yeast/rice fermentation product filter 3.5%, p-hydroxyacetophenone 0.00001%, 1, 2-hexanediol 0.00001%, 1, 2-pentanediol 0.0001%, daily essence 0.01%, and the balance 69.37% deionized water.
The raw materials are operated as follows:
preparation before operation
1) Accurately weighing Panax notoginsenosides according to a certain amount, and preparing into 5 wt% water solution with deionized water solution boiled and cooled to room temperature;
2) preparing 5 wt% aqueous solution C phase of potassium hydroxide by using boiled and cooled deionized water solution for later use;
heating water and oil phase
1) Putting pentaerythritol tetra (ethyl hexanoate) ester, polyglycerol-10 myristate, behenyl alcohol, phytosterol/octyldodecanol lauroyl glutamate, tocopheryl acetate, methyl gluceth-10, cetostearyl alcohol, stearic acid and DMCM-5 into an oil pan, heating to 85 +/-2 ℃ while stirring (stirring speed of 200-800 revolutions per minute), uniformly mixing, and keeping the temperature for 10 minutes; after the heat preservation is finished, adding cyclopentadimethylsiloxane, and uniformly stirring to obtain an oil phase A;
3) putting the rest boiled and cooled deionized water, butanediol, trehalose, carbomer, EDTA disodium, panax notoginseng saponins, micromolecular hyaluronic acid, a tremella entity extract, polyglycerol-2 stearate, glycerol stearate and stearyl alcohol into a water kettle, heating to 90 +/-2 ℃ while stirring (stirring speed of 800 revolutions per minute), uniformly mixing, keeping the temperature for 10 minutes, and uniformly mixing to obtain a water phase B;
homogenizing and emulsifying
1) Preheating an emulsifying pot jacket to 45 ℃, vacuumizing, pumping the phase A into an emulsifying pot under the stirring condition (the vacuumizing stirring speed is 20 revolutions per minute), and keeping the temperature at 85 ℃ for internal circulation homogenizing stirring for 15 minutes (the homogenizing speed is 1000 revolutions per minute, and the stirring speed is 20 revolutions per minute);
2) after the homogenization of the phase A is finished, starting internal circulation and vacuumizing to pump the phase B into an emulsifying pot from an upper feed inlet, carrying out external circulation homogenization after the feeding is finished, keeping the temperature of the emulsifying pot at 85 ℃, and stirring for 10 minutes (the homogenization speed is 2000 rpm, and the stirring speed is 40 rpm);
3) after homogenization, vacuumizing to-400 mbar, and cooling;
4) after homogenization, when the temperature is reduced to 47 ℃, stirring and external circulation are continued, vacuumizing is performed, the C-phase potassium hydroxide is added into an emulsifying pot, and homogenization stirring is performed for 1 minute (the homogenization speed is 3000 r/min, and the stirring speed is 80 r/min);
5) while stirring was maintained, phase D was slowly added by homogenization with external circulation (homogenization rate 1000 rpm, stirring rate 80 rpm) from the upper feed port: dipotassium glycyrrhizinate,
Figure BDA0002938642670000041
K350, herba Dendrobii stem extract, rhizoma Polygonati Odorati extract, Poria extract, radix scrophulariae extract, radix Ophiopogonis extract, yeast/rice fermentation product filter, p-hydroxyacetophenone1, 2-hexanediol, 1, 2-pentanediol and (daily) essence, and homogenizing for 2 minutes (the homogenizing speed is 2000 rpm, and the stirring speed is 40 rpm); after homogenizing, vacuumizing to minus 600mbar, and continuing stirring for 2 minutes (the stirring speed is 40 revolutions per minute);
6) after homogenizing, vacuumizing to minus 600mbar, and continuously stirring and cooling for 2-minutes (stirring speed is 40 r/min); discharging through 100 meshes, putting into a designated container, and warehousing for storage to obtain the finished product.
Example 2
The moisturizing emulsion comprises the following raw materials in percentage by weight, the sum of the raw materials is 100 percent: pentaerythritol tetra (ethyl hexanoate) 0.5%, polyglycerol-10 myristate 1.5%, behenyl alcohol 1%, phytosterol/octyldodecanol lauroyl glutamate 1%; tocopherol acetate 0.05%, methyl glucitol polyether-106%, polyglycerol-2 stearate 0.1%; 0.6% of glyceryl stearate, 0.1% of cetearyl alcohol, 0.01% of stearyl alcohol, 0.05% of stearic acid, 7% of cyclopentadimethylsiloxane, DMCM-54%, 3% of butanediol, 0.5% of trehalose, 0.1% of carbomer, 0.01% of disodium EDTA, 0.005% of panax notoginseng saponins, 0.02% of micromolecular hyaluronic acid, 0.05% of tremella entity extract, 0.01% of potassium hydroxide, 0.01% of dipotassium glycyrrhizinate,
Figure BDA0002938642670000052
K3501.5%, Dendrobium officinale stem extract 0.001%, Polygonatum odoratum extract 0.001%, Poria cocos extract 0.001%, radix scrophulariae extract 0.001%, radix Ophiopogonis extract 0.001%, yeast/rice fermentation product filter 3.5%, p-hydroxyacetophenone 0.00001%, 1, 2-hexanediol 0.00001%, 1, 2-pentanediol 0.0001%, daily essence 0.01%, and the balance 69.37% deionized water.
The raw materials are operated as follows:
preparation before operation
1) Accurately weighing Panax notoginsenosides according to a certain amount, and preparing into 5 wt% water solution with deionized water solution boiled and cooled to room temperature;
2) preparing 5 wt% aqueous solution C phase of potassium hydroxide by using boiled and cooled deionized water solution for later use;
heating water and oil phase
1) Putting pentaerythritol tetra (ethyl hexanoate) ester, polyglycerol-10 myristate, behenyl alcohol, phytosterol/octyldodecanol lauroyl glutamate, tocopheryl acetate, methyl gluceth-10, cetostearyl alcohol, stearic acid and DMCM-5 into an oil pan, heating to 85 +/-2 ℃ while stirring (stirring speed of 200-800 revolutions per minute), uniformly mixing, and keeping the temperature for 10 minutes; after the heat preservation is finished, adding cyclopentadimethylsiloxane, and uniformly stirring to obtain an oil phase A;
3) putting the rest boiled and cooled deionized water, butanediol, trehalose, carbomer, EDTA disodium, panax notoginseng saponins, micromolecular hyaluronic acid, Tremella entity extract polyglycerol-2 stearate, glycerol stearate and stearyl alcohol into a water kettle, heating to 90 +/-2 ℃ while stirring (stirring speed of 800 revolutions per minute), uniformly mixing, keeping the temperature for 10 minutes, and uniformly mixing to obtain a water phase B;
homogenizing and emulsifying
1) Preheating an emulsifying pot jacket to 45 ℃, vacuumizing, pumping the phase A into an emulsifying pot under the stirring condition (the vacuumizing stirring speed is 20 revolutions per minute), and keeping the temperature at 85 ℃ for internal circulation homogenizing stirring for 15 minutes (the homogenizing speed is 1000 revolutions per minute, and the stirring speed is 20 revolutions per minute);
2) after the homogenization of the phase A is finished, starting internal circulation and vacuumizing to pump the phase B into an emulsifying pot from an upper feed inlet, carrying out external circulation homogenization after the feeding is finished, keeping the temperature of the emulsifying pot at 85 ℃, and stirring for 10 minutes (the homogenization speed is 2000 rpm, and the stirring speed is 40 rpm);
3) after homogenizing, continuing stirring and external circulation, vacuumizing, adding the C-phase potassium hydroxide into an emulsifying pot, and homogenizing and stirring for 1 minute (the homogenizing speed is 3000 r/min, and the stirring speed is 80 r/min);
4) after homogenizing, continuing stirring, and beginning cooling with a vacuum value of-400 mbar;
5) when the temperature drops to 47 ℃, stirring is continued, and phase D is slowly added from an upper feeding port by starting external circulation homogenization (the homogenization speed is 1000 revolutions per minute, and the stirring speed is 80 revolutions per minute): dipotassium glycyrrhizinate,
Figure BDA0002938642670000051
K350, dendrobium officinale stem extract, polygonatum extract, poria cocos extract, radix scrophulariae extract, radix ophiopogonis extract, yeast/rice fermentation product filter, p-hydroxyacetophenone, 1, 2-hexanediol, 1, 2-pentanediol and (daily) essence, and homogenizing for 2 minutes (homogenizing speed is 2000 revolutions per minute, and stirring speed is 40 revolutions per minute); after homogenizing, vacuumizing to minus 600mbar, and continuing stirring for 2 minutes (the stirring speed is 40 revolutions per minute);
6) after homogenizing, vacuumizing to minus 600mbar, and continuously stirring and cooling for 2-minutes (stirring speed is 40 r/min); discharging through 100 meshes, putting into a designated container, and warehousing for storage to obtain the finished product.
Example 3
The moisturizing emulsion comprises the following raw materials in percentage by weight, the sum of the raw materials is 100 percent: pentaerythritol tetra (ethyl hexanoate) 0.5%, polyglycerol-10 myristate 1.5%, behenyl alcohol 1%, phytosterol/octyldodecanol lauroyl glutamate 1%; tocopherol acetate 0.05%, methyl glucitol polyether-106%, polyglycerol-2 stearate 0.1%; 0.6% of glyceryl stearate, 0.1% of cetearyl alcohol, 0.01% of stearyl alcohol, 0.05% of stearic acid, 7% of cyclopentadimethylsiloxane, DMCM-54%, 3% of butanediol, 0.5% of trehalose, 0.1% of carbomer, 0.01% of disodium EDTA, 0.005% of panax notoginseng saponins, 0.02% of micromolecular hyaluronic acid, 0.05% of tremella entity extract, 0.01% of potassium hydroxide, 0.01% of dipotassium glycyrrhizinate,
Figure BDA0002938642670000061
K3501.5%, Dendrobium officinale stem extract 0.001%, Polygonatum odoratum extract 0.001%, Poria cocos extract 0.001%, radix scrophulariae extract 0.001%, radix Ophiopogonis extract 0.001%, yeast/rice fermentation product filter 3.5%, p-hydroxyacetophenone 0.00001%, 1, 2-hexanediol 0.00001%, 1, 2-pentanediol 0.0001%, daily essence 0.01%, and the balance 69.37% deionized water.
The raw materials are operated as follows:
preparation before operation
1) Accurately weighing Panax notoginsenosides according to a certain amount, and preparing into 5 wt% water solution with deionized water solution boiled and cooled to room temperature;
2) preparing 5 wt% aqueous solution C phase of potassium hydroxide by using boiled and cooled deionized water solution for later use;
heating water and oil phase
1) Putting pentaerythritol tetra (ethyl hexanoate), polyglycerol-10 myristate, behenyl alcohol, phytosterol/octyldodecanol lauroyl glutamate, tocopheryl acetate, methyl gluceth-10, polyglycerol-2 stearate, glyceryl stearate, cetostearyl alcohol, stearyl alcohol, stearic acid and DMCM-5 into an oil pan, heating to 85 +/-2 ℃ while stirring (stirring speed of 200-800 r/min), uniformly mixing, and keeping the temperature for 10 minutes; after the heat preservation is finished, adding cyclopentadimethylsiloxane, and uniformly stirring to obtain an oil phase A;
3) putting the rest boiled and cooled deionized water, butanediol, trehalose, carbomer, EDTA disodium, panax notoginseng saponins, micromolecular hyaluronic acid and tremella entity extract into a water pot, heating to 90 +/-2 ℃ while stirring (stirring speed of 800 revolutions per minute), uniformly mixing, preserving heat for 10 minutes, and uniformly mixing to obtain a water phase B;
homogenizing and emulsifying
1) Preheating an emulsifying pot jacket to 45 ℃, vacuumizing, pumping the phase A into an emulsifying pot under the stirring condition (the vacuumizing stirring speed is 20 revolutions per minute), and keeping the temperature at 85 ℃ for internal circulation homogenizing stirring for 15 minutes (the homogenizing speed is 1000 revolutions per minute, and the stirring speed is 20 revolutions per minute);
2) after the homogenization of the phase A is finished, starting internal circulation and vacuumizing to pump the phase B into an emulsifying pot from an upper feed inlet, carrying out external circulation homogenization after the feeding is finished, keeping the temperature of the emulsifying pot at 85 ℃, and stirring for 10 minutes (the homogenization speed is 2000 rpm, and the stirring speed is 40 rpm);
3) after homogenizing, continuing stirring and external circulation, vacuumizing, adding the C-phase potassium hydroxide into an emulsifying pot, and homogenizing and stirring for 1 minute (the homogenizing speed is 3000 r/min, and the stirring speed is 80 r/min);
4) after homogenizing, continuing stirring, and beginning cooling with a vacuum value of-400 mbar;
5) when the temperature is reduced to 47 ℃, stirring is adjusted, external circulation is started for homogenization (the homogenization speed is 1000 rpm, the stirring speed is 80 rpm), and phase D is slowly added from an upper feeding port: dipotassium glycyrrhizinate,
Figure BDA0002938642670000071
K350, dendrobium officinale stem extract, polygonatum extract, poria cocos extract, radix scrophulariae extract, radix ophiopogonis extract, yeast/rice fermentation product filter, p-hydroxyacetophenone, 1, 2-hexanediol, 1, 2-pentanediol and (daily) essence, and homogenizing for 2 minutes (homogenizing speed is 2000 revolutions per minute, and stirring speed is 40 revolutions per minute); after homogenizing, vacuumizing to minus 600mbar, and continuing stirring for 2 minutes (the stirring speed is 40 revolutions per minute);
6) after homogenizing, vacuumizing to minus 600mbar, and continuously stirring and cooling for 2-minutes (stirring speed is 40 r/min); discharging through 100 meshes, putting into a designated container, and warehousing for storage to obtain the finished product.
Example 4
The moisturizing emulsion comprises the following raw materials in percentage by weight, the sum of the raw materials is 100 percent: pentaerythritol tetra (ethyl hexanoate) 2.5%, polyglycerol-10 myristate 2%, behenyl alcohol 0.1%, phytosterol/octyldodecanol lauroyl glutamate 0.2%; 0.1% of tocopherol acetate, 104% of methyl glucitol polyether and 2% of polyglycerol-2 stearate; 0.2% of glyceryl stearate, 2% of cetearyl alcohol, 0.5% of stearyl alcohol, 0.7% of stearic acid, 2% of cyclopentadimethylsiloxane, 50.5% of DMCM (dimethyl formamide), 8% of butanediol, 2% of trehalose, 0.2% of carbomer, 0.08% of disodium EDTA (ethylene diamine tetraacetic acid), 0.002% of panax notoginseng saponins, 0.2% of micromolecular hyaluronic acid, 0.001% of tremella entity extract, 0.1% of potassium hydroxide, 0.1% of dipotassium glycyrrhizinate,
Figure BDA0002938642670000072
K3501%, herba Dendrobii stem extract 0.002%, rhizoma Polygonati Odorati extract 0.002%, Poria extract 0.002%, radix scrophulariae extract 0.002%, radix Ophiopogonis extract 0.002%, yeast/rice fermentation product filter 2.5%, p-hydroxyacetophenone0.00002 percent of deionized water, 0.00005 percent of 1, 2-hexanediol, 0.01 percent of 1, 2-pentanediol, 0.6 percent of (daily) essence and the balance of 68.39 percent of deionized water.
The raw materials are operated as follows:
preparation before operation
1) Accurately weighing Panax notoginsenosides according to a certain amount, and preparing into 7.5 wt% water solution with deionized water solution boiled and cooled to room temperature;
2) preparing 5-10 wt% aqueous solution C phase from potassium hydroxide by using boiled and cooled deionized water solution for later use;
heating water and oil phase
1) Placing pentaerythritol tetra (ethyl hexanoate), polyglycerol-10 myristate, behenyl alcohol, phytosterol/octyldodecanol lauroyl glutamate, tocopheryl acetate, methyl gluceth-10, polyglycerol-2 stearate, glyceryl stearate, cetearyl alcohol, stearyl alcohol, stearic acid and DMCM-5 into an oil pan, heating to 85 +/-2 ℃ while stirring (stirring speed 500 revolutions per minute), uniformly mixing, and keeping the temperature for 20 minutes; after the heat preservation is finished, adding cyclopentadimethylsiloxane, and uniformly stirring to obtain an oil phase A;
3) putting the rest boiled and cooled deionized water, butanediol, trehalose, carbomer, EDTA disodium, panax notoginseng saponins, micromolecular hyaluronic acid and tremella entity extract into a water pot, heating to 90 +/-2 ℃ while stirring (stirring speed of 600 revolutions per minute), uniformly mixing, preserving heat for 20 minutes, and uniformly mixing to obtain a water phase B;
homogenizing and emulsifying
1) Preheating an emulsifying pot jacket to 50 ℃, vacuumizing, pumping the phase A into an emulsifying pot under the stirring condition (the vacuumizing stirring speed is 20-80 r/min), and keeping the temperature at 82 ℃ for internal circulation homogenizing stirring for 5-15 min (the homogenizing speed is 1500 r/min, and the stirring speed is 50 r/min);
2) after the homogenization of the phase A is finished, starting internal circulation and vacuumizing to pump the phase B into an emulsifying pot from an upper feed inlet, carrying out external circulation homogenization after the feeding is finished, keeping the temperature of the emulsifying pot at 80-85 ℃, and stirring for 15 minutes (the homogenization speed is 1500 rpm, and the stirring speed is 60 rpm);
3) after homogenizing, continuing stirring and external circulation, vacuumizing, adding the C-phase potassium hydroxide into an emulsifying pot, and homogenizing and stirring for 5 minutes (the homogenizing speed is 2500 rpm, and the stirring speed is 60 rpm);
4) after homogenizing, continuing stirring, and beginning cooling with a vacuum value of-550 mbar;
5) when the temperature is reduced to 50 ℃, stirring is continued, and external circulation is started for homogenization (the homogenization speed is 1500 rpm, the stirring speed is 50 rpm), and phase D is slowly added from an upper feeding port: dipotassium glycyrrhizinate,
Figure BDA0002938642670000081
K350, dendrobium officinale stem extract, polygonatum extract, poria cocos extract, radix scrophulariae extract, radix ophiopogonis extract, yeast/rice fermentation product filter, p-hydroxyacetophenone, 1, 2-hexanediol, 1, 2-pentanediol and (daily) essence, and homogenizing for 5 minutes (homogenizing speed is 1500 revolutions per minute, and stirring speed is 60 revolutions per minute); after homogenization, vacuumizing to minus 750mbar, and continuing stirring for 6 minutes (the stirring speed is 30 revolutions per minute);
6) after homogenization, vacuumizing to minus 750mbar, and continuously stirring and cooling for 6 minutes (stirring speed is 30 revolutions per minute); discharging through 100 meshes, putting into a designated container, and warehousing for storage to obtain the finished product.
Example 5
The moisturizing emulsion comprises the following raw materials in percentage by weight, the sum of the raw materials is 100 percent: pentaerythritol tetra (ethyl hexanoate) 1.5%, polyglycerol-10 myristate 0.5%, behenyl alcohol 2%, phytosterol/octyldodecanol lauroyl glutamate 1.2%; tocopherol acetate 0.02%, methyl glucitol polyether-103%, polyglycerol-2 stearate 5%; 0.5% of glyceryl stearate, 1.5% of cetearyl alcohol, 0.1% of stearyl alcohol, 0.5% of stearic acid, 1% of cyclopentadimethylsiloxane, DMCM-52%, 5% of butanediol, 4% of trehalose, 0.4% of carbomer, 0.05% of disodium EDTA, 0.001% of panax notoginseng saponins, 0.1% of micromolecular hyaluronic acid, 0.08% of tremella entity extract, 0.05% of potassium hydroxide, 0.2% of dipotassium glycyrrhizinate,
Figure BDA0002938642670000082
K3500.2%, dendrobium officinale stem extract 0.002%, radix polygonati officinalis extract 0.002%, poria cocos extract 0.002%, radix scrophulariae extract 0.002%, radix ophiopogonis extract 0.002%, yeast/rice fermentation product filter 0.5%, p-hydroxyacetophenone 0.00005%, 1, 2-hexanediol 0.00002%, 1, 2-pentanediol 0.05%, daily essence 0.2%, and the balance of 70.34% deionized water.
The raw materials are operated as follows:
preparation before operation
1) Accurately weighing Panax notoginsenosides according to a certain amount, and preparing into 10wt% water solution with deionized water solution boiled and cooled to room temperature;
2) preparing the potassium hydroxide into a 10wt% aqueous solution C phase by using a boiled and cooled deionized water solution for later use;
heating water and oil phase
1) Placing pentaerythritol tetra (ethyl hexanoate), polyglycerol-10 myristate, behenyl alcohol, phytosterol/octyldodecanol lauroyl glutamate, tocopheryl acetate, methyl gluceth-10, polyglycerol-2 stearate, glyceryl stearate, cetearyl alcohol, stearyl alcohol, stearic acid and DMCM-5 into an oil pan, heating to 85 +/-2 ℃ while stirring (stirring speed of 800 revolutions per minute), uniformly mixing, and keeping the temperature for 30 minutes; after the heat preservation is finished, adding cyclopentadimethylsiloxane, and uniformly stirring to obtain an oil phase A;
3) putting the rest boiled and cooled deionized water, butanediol, trehalose, carbomer, EDTA disodium, panax notoginseng saponins, micromolecular hyaluronic acid and tremella entity extract into a water pot, heating to 90 +/-2 ℃ while stirring (stirring speed of 800 revolutions per minute), uniformly mixing, preserving heat for 30 minutes, and uniformly mixing to obtain a water phase B;
homogenizing and emulsifying
1) Preheating an emulsifying pot jacket to 55 ℃, vacuumizing, pumping the phase A into an emulsifying pot under the stirring condition (the vacuumizing stirring speed is 20-80 r/min), and keeping the temperature at 85 ℃ for internal circulation homogenizing stirring for 5 minutes (the homogenizing speed is 3000 r/min, and the stirring speed is 80 r/min);
2) after the homogenization of the phase A is finished, starting internal circulation and vacuumizing to pump the phase B into an emulsifying pot from an upper feed inlet, carrying out external circulation homogenization after the feeding is finished, keeping the temperature of the emulsifying pot at 80 ℃, and stirring for 20 minutes (the homogenization speed is 3000 r/min, and the stirring speed is 80 r/min);
3) after homogenizing, continuing stirring and external circulation, vacuumizing, adding the C-phase potassium hydroxide into an emulsifying pot, and homogenizing and stirring for 10 minutes (the homogenizing speed is 2000 rpm, and the stirring speed is 40 rpm);
4) after homogenizing, continuing stirring, and beginning cooling with a vacuum value of-700 mbar;
5) when the temperature drops to 53 ℃, stirring is continued, and phase D is slowly added from the upper feeding port by starting external circulation homogenization (the homogenization speed is 2000 rpm, the stirring speed is 20 rpm): dipotassium glycyrrhizinate,
Figure BDA0002938642670000091
K350, dendrobium officinale stem extract, polygonatum extract, poria cocos extract, radix scrophulariae extract, radix ophiopogonis extract, yeast/rice fermentation product filter, p-hydroxyacetophenone, 1, 2-hexanediol, 1, 2-pentanediol and (daily) essence, and homogenizing for 8 minutes (homogenizing speed is 1000 revolutions per minute, and stirring speed is 80 revolutions per minute); after homogenizing, vacuumizing to-900 mbar, and continuing stirring for 10 minutes (the stirring speed is 80 rpm);
6) after homogenizing, vacuumizing to minus 900mbar, and continuously stirring and cooling for 10 minutes (the stirring speed is 20 revolutions per minute); discharging through 100 meshes, putting into a designated container, and warehousing for storage to obtain the finished product.
The test results are detailed in tables 1,2 and 3
TABLE 1 moisturizing emulsion preparation and stability, skin feel evaluation results
Figure BDA0002938642670000101
As can be seen from Table 1, examples 3-5 are stable and meet the requirements of product development.
Skin feel evaluation is carried out on the skin feel evaluation of the examples 3-5, the final formula is screened out from the skin feel evaluation, and long-acting efficacy test research is carried out, and the skin feel evaluation result is detailed in a table 2. Skin feel evaluation method: taking a proper amount of moisturizing cleanser, sequentially comparing and trying the products of examples 3-5, and then evaluating the products (taking a proper amount of products, uniformly applying the products on the face, massaging until the products are absorbed); the full score is 7 points, and the higher the score is, the better the satisfaction is.
Table 2 skin feel evaluation results
Index (I) Example 3 Example 4 Example 5
Appearance of the paste 5.9 5.7 5.7
Thickness of paste 5.8 6.0 4.2
Hand feeling during painting 6.1 5.7 5.3
Absorption rate 5.9 6.2 4.7
Instant moisturizing effect 5.9 6.0 6.4
Refreshing feeling of skin 6.0 5.2 5.4
General evaluation 5.9 5.8 5.3
As can be seen from the results of the evaluation in Table 2, the sample of example 3 had a high score of body, hand feeling during application, and refreshing feeling of the skin after absorption, and the overall preference was the highest. Example 2 the slightly greater amount of oil remaining on the skin surface after absorption due to the higher amount of pentaerythritol tetra (ethyl hexanoate) added, resulted in a lower refreshing feel score; in example 5, the addition amount of the emulsifier polyglycerol-2 stearate and the like is high, so that the consistency of the sample is increased, the difficulty in spreading is increased, and the skin feel in use is reduced.
In summary, example 3 is the most stable and preferred protocol, and example 3 was used as the final formulation to study moisturizing performance
The moisturizing lotion obtained in example 3 was used for a 2-week long-term efficacy test, and the subjects before and after use were measured for gray idx (3D gray scale map of the skin deep layer) and gray idxt.
Evaluating the graphical information of the moisture distribution and the micro-morphology of the skin surface by using C-Cube, wherein GrayIdx refers to a gray index, and the higher the gray index is, the better the moisture distribution is; GrayIdxT is a threshold set at 20% gray scale index to cut off background pixel interference, with higher values indicating more moisture and higher skin moisture. The results are shown in Table 3:
TABLE 3 deep skin moisture after moisturizing lotion
Time GrayIdx GrayIdxT
Base value 234.26±19.79 184.48±17.12
1 week 243.4±9.91** 192.77±9.14**
2 weeks 242.9±13.02* 190.43±8.09*
As can be seen from the results in Table 3, the water distribution in the deep layer of the skin is more uniform for 1-2 weeks, which means that the water distribution is improved by 3.9%, which is significantly higher than the base value, and the threshold value is increased, which indicates that the water distribution of the skin becomes uniform and the skin humidity is increased.
Finally, it should be noted that the above mentioned embodiments are merely preferred examples in the present invention, and not intended to limit the present invention, and all modifications and variations made according to the claims of the present invention shall fall within the scope of the present invention.

Claims (8)

1. A moisturizing emulsion characterized by: the compound fertilizer is prepared from the following basic components in percentage by weight, wherein the sum of the raw materials is 100 percent: the grease is 0.5-3% of pentaerythritol tetra (ethyl hexanoate), 0.2-3% of polyglycerol-10 myristate, 0.1-2% of behenyl alcohol and 0.01-2% of phytosterol/octyldodecanol lauroyl glutamate; 0.01-1% of tocopherol acetate, 101-10% of methyl glucitol polyether-101 and 0.1-10% of polyglycerol-2 stearate; 0.2-0.7% of glyceryl stearate, 0.1-3% of cetearyl alcohol, 0.01-1% of stearyl alcohol, 0.1-1% of stearic acid, 1-7% of cyclopentadimethylsiloxane and 50.5-6% of DMCM-L; the moisturizing component comprises 1-10% of butanediol, 0.5-5% of trehalose, 0.001-0.1% of tremella fruiting body extract, 0.001-1% of dendrobium officinale stem extract, 0.001-1% of polygonatum odoratum extract, 0.001-1% of poria cocos extract, 0.001-1% of radix scrophulariae extract, 0.001-1% of radix ophiopogonis extract and 0.1-5% of saccharomycetes/rice fermentation product filtrate; the thickening agent is 0.01-0.6% of carbomer; other components are 0.01 to 0.1 percent of EDTA disodium, 0.0005 to 0.1 percent of panax notoginseng saponins, 0.01 to 0.3 percent of micromolecular hyaluronic acid, 0.01 to 0.12 percent of potassium hydroxide, 0.01 to 0.5 percent of dipotassium glycyrrhizinate, 0.8 to 1.6 percent of euxyl K3500.1, 0.00001 to 0.2 percent of p-hydroxyacetophenone, 0.00001 to 0.2 percent of 1, 2-hexanediol, 0.0001 to 0.2 percent of 1, 2-pentanediol, 0.01 to 1 percent of essence and the balance of 20 to 90 percent of deionized water.
2. The method of preparing a moisturizing emulsion according to claim 1, comprising the steps of:
1) preparing 5-10 wt% of water solution of panax notoginseng saponins by using boiled and cooled deionized water solution for later use;
2) placing pentaerythritol tetra (ethyl hexanoate), polyglycerol-10 myristate, behenyl alcohol, phytosterol/octyldodecanol lauroyl glutamate, tocopheryl acetate, methyl gluceth-10, polyglycerol-2 stearate, glyceryl stearate, cetearyl alcohol, stearyl alcohol, stearic acid and DMCM-5 into an oil pan, heating to 85 +/-2 ℃ while stirring, uniformly mixing, and keeping the temperature for 10-30 minutes; after the heat preservation is finished, adding cyclopentadimethylsiloxane, and uniformly stirring to obtain a phase A;
3) putting the rest boiled and cooled deionized water, butanediol, trehalose, carbomer, EDTA disodium, panax notoginseng saponins, micromolecular hyaluronic acid and tremella entity extract into a water pot, heating to 90 +/-2 ℃ while stirring, uniformly mixing, preserving the heat for 10-30 minutes, and uniformly mixing to obtain a phase B;
4) preparing 5-10 wt% aqueous solution of potassium hydroxide by using boiled and cooled deionized water solution for later use to obtain a C phase;
5) vacuumizing under the stirring condition, pumping the phase A into an emulsifying pot, and keeping the temperature of 80-85 ℃ for internal circulation homogenizing stirring for 5-15 minutes;
6) after the homogenization of the phase A is finished, starting internal circulation and vacuumizing to pump the phase B into the emulsifying pot from the upper feed inlet, carrying out external circulation homogenization after the feeding is finished, keeping the temperature of the emulsifying pot at 80-85 ℃, and stirring for 10-20 minutes;
7) after homogenizing, continuing stirring and external circulation, vacuumizing, adding the C-phase potassium hydroxide into an emulsifying pot, and homogenizing and stirring for 1-10 minutes;
8) after homogenizing, continuously stirring, and beginning to cool with the vacuum value of-400 to-700 mbar;
9) and (3) when the temperature is reduced to 47-53 ℃, continuing stirring, and slowly adding the phase D from an upper feeding port under external circulation homogenization: dipotassium glycyrrhizinate, euxyl K350, dendrobium officinale stem extract, polygonatum extract, poria cocos extract, radix scrophulariae extract, radix ophiopogonis extract, yeast/rice fermentation product filter, p-hydroxyacetophenone, 1, 2-hexanediol, 1, 2-pentanediol and essence, and homogenizing for 2-8 minutes; after homogenizing, vacuumizing to minus 600 to minus 900mbar, and continuously stirring for 2-10 minutes;
10) after homogenizing, vacuumizing to minus 600 to minus 900mbar, and stirring for 2-10 minutes; and continuously cooling to 40 ℃, filtering by 100 meshes, discharging, filling into a specified container, and warehousing for storage to obtain a finished product.
3. The method of claim 2, wherein the emulsifier (polyglyceryl-2 stearate, glyceryl stearate, stearyl alcohol) of step 2 is added to the oil phase.
4. The method for preparing a moisturizing emulsion according to claim 2, wherein the vacuumizing and stirring speed in the step 5 is 20-80 rpm.
5. The method for preparing a moisturizing emulsion according to claim 2, wherein in the step 6, the homogenizing speed is 1000-2000 rpm, and the stirring speed is 20-80 rpm.
6. The method of claim 2, wherein the step 7 is carried out at an elevated temperature; the homogenizing speed is 2000-3000 r/min, and the stirring speed is 40-80 r/min.
7. The method for preparing a moisturizing emulsion according to claim 2, wherein the external circulation homogenizing speed in the step 9 is 1000-2000 rpm, the stirring speed is 20-80 rpm, and the homogenizing speed in the homogenizing 2-8 minutes is 1000-2000 rpm, and the stirring speed is 40-80 rpm.
8. The method for preparing a moisturizing emulsion according to claim 2, wherein the stirring speed in the step 10 is 20-40 rpm.
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