CN112121001B - Non-irritant essence with whitening and moisturizing functions and preparation method thereof - Google Patents

Non-irritant essence with whitening and moisturizing functions and preparation method thereof Download PDF

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CN112121001B
CN112121001B CN202011119382.1A CN202011119382A CN112121001B CN 112121001 B CN112121001 B CN 112121001B CN 202011119382 A CN202011119382 A CN 202011119382A CN 112121001 B CN112121001 B CN 112121001B
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essence
parts
stirring
whitening
mass
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CN112121001A (en
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不公告发明人
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Guangzhou Meili Cosmetics Co.,Ltd.
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Guangdong Chuangmei Anti Aging Research Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/98Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
    • A61K8/987Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • A61K8/365Hydroxycarboxylic acids; Ketocarboxylic acids
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/40Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/42Amides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/46Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
    • A61K8/466Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfonic acid derivatives; Salts
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/58Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing atoms other than carbon, hydrogen, halogen, oxygen, nitrogen, sulfur or phosphorus
    • A61K8/585Organosilicon compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives thereof
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/67Vitamins
    • A61K8/673Vitamin B group
    • A61K8/675Vitamin B3 or vitamin B3 active, e.g. nicotinamide, nicotinic acid, nicotinyl aldehyde
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/02Preparations for care of the skin for chemically bleaching or whitening the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/412Microsized, i.e. having sizes between 0.1 and 100 microns

Abstract

The invention discloses a non-irritant essence with whitening and moisturizing functions and a preparation method thereof, and the preparation method comprises the following steps: step one, heating and dissolving: adding deionized water, modified pearl powder, a humectant, essence, xylitol, caprolactam silicon oil, trehalose, citric acid and nicotinamide into a reaction kettle 1 subjected to high-temperature sterilization according to the parts by weight, starting stirring at the stirring speed of 200-85 r/min, heating to 75-85 ℃, stirring for 1-3h to obtain a clear and transparent mixed solution, then scattering a thickening agent into the mixed solution while stirring, stirring for 0.5-1h, cooling the mixed solution to normal temperature after full dissolution, filtering the solution through a sterilized filter to remove undissolved impurities into a reaction kettle 2 subjected to high-temperature sterilization to obtain a solution; step two, dissolving at normal temperature: adding the nymphaea hybrid extract and the preservative into the solution, stirring for 30-60min at normal temperature, and discharging to obtain the non-irritant essence with whitening and moisturizing functions. By the method, the non-irritant essence is obtained, and the obtained essence has excellent whitening and moisturizing functions for people with dry, neutral and oily skins.

Description

Non-irritant essence with whitening and moisturizing functions and preparation method thereof
Technical Field
The invention relates to a cosmetic technology, and particularly relates to a non-irritant essence with whitening and moisturizing functions and a preparation method thereof.
Background
With the improvement of the living standard of people, people pay more and more attention to the appearance of the people, and the investment of skin care is more and more, and at present, the skin care is mainly focused on the aspects of whitening, moisturizing and the like. The concept of white-covering clown is to let consumers have unique feelings about whitening products. However, many whitening and moisturizing products currently on the market are specific to skin, cannot be applied to various skins, or irritate the skin, do not perform whitening and moisturizing effects on the skin, and cause skin problems.
CN201510799279.9 discloses a whitening and moisturizing essence and a preparation method thereof. The whitening and moisturizing essence comprises the following raw materials in parts by weight: 0.2-0.5 part of thickening agent, 3-12 parts of polyhydric alcohol, 15-35 parts of traditional Chinese medicine extract, 1-2 parts of honey, 0.3-2 parts of pearl powder, 0.1-0.3 part of essence and 40-70 parts of water, wherein the preparation raw materials of the traditional Chinese medicine extract comprise eucommia bark, cochinchnese asparagus root, coix seed and blueberry fruit. The whitening and moisturizing essence has good permeability and easy absorption, and has the effects of whitening and moisturizing, repairing skin wrinkles, improving skin darkness, improving skin luster and delaying skin aging.
CN201610866005.1 discloses a needle mushroom essence and a preparation method thereof, wherein the formula of the needle mushroom essence comprises needle mushroom polysaccharide, glycerol, 1, 2-propylene glycol, sodium hyaluronate, trehalose, citric acid, D-panthenol, nicotinamide, a stabilizer, a preservative and water. The needle mushroom essence prepared by the invention takes natural needle mushroom polysaccharide as a core component, has the effects of moisturizing, resisting oxidation, resisting aging, tightening skin and the like, and has the effects of maintaining beauty and keeping young, wherein sodium hyaluronate is a natural high-moisturizing factor, and is supplemented with trehalose, nicotinamide, D-panthenol and the like, so that the needle mushroom essence has the effects of maintaining moisture, whitening and tightening skin, and can also keep the cell activity of the skin in severe environments such as high temperature, high cold, strong ultraviolet radiation and the like, and improve the stress resistance.
CN201510793611.0 discloses a whitening anti-aging essence and a preparation method thereof. The whitening and anti-aging essence comprises polyethylene glycol, polydimethylsiloxane, sodium polyglutamate, glycerol, hyaluronic acid, xylitol, C20-22 alcohol phosphate/C20-22 alcohol, a ginkgo leaf extract, an ophiopogon root extract, a purslane extract, a suberect spatholobus stem extract, milk protein and the like. The whitening and anti-aging essence provided by the invention has good permeability, is easy to absorb, can effectively replenish water, moisturize and whiten skin, repair skin wrinkles, reduce fine lines and delay skin aging.
Although the technology related to whitening and moisturizing essence is available at present, most of the essence prepared by the prior art cannot be simultaneously applied to people with various skins, and side effects such as skin irritation are easily caused.
Disclosure of Invention
The invention provides non-irritant essence with whitening and moisturizing functions and a preparation method thereof.
The non-irritant essence with whitening and moisturizing functions and the preparation method thereof are characterized by comprising the following steps:
step one, heating and dissolving: adding 100 parts by mass of deionized water, 1-3 parts by mass of modified pearl powder, 5-15 parts by mass of humectant, 0.1-0.5 part by mass of essence, 5-10 parts by mass of xylitol, 1-3 parts by mass of caprolactam silicon oil, 1-2 parts by mass of trehalose, 0.1-0.2 part by mass of citric acid and 1-2 parts by mass of nicotinamide into a reaction kettle 1 subjected to high-temperature sterilization, starting stirring at a stirring speed of 200-300r/min, heating to 75-85 ℃, stirring for 1-3 hours to obtain a clear and transparent mixed solution, then scattering 0.1-1.0 part by mass of thickener into the mixed solution while stirring, stirring for 0.5-1 hour, cooling the mixed solution to normal temperature after full dissolution, filtering the solution through a sterilized filter to remove undissolved impurities into a reaction kettle 2 subjected to high-temperature sterilization, obtaining a solution;
step two, dissolving at normal temperature: adding 10-15 parts of nymphaea hybrid extract and 0.05-0.10 part of preservative into the solution, stirring for 30-60min at normal temperature, and discharging to obtain the non-irritant essence with whitening and moisturizing functions.
Preferably, the preparation method of the modified pearl powder in the step one comprises the following steps:
according to the mass portion, 10-20 portions of pearl powder which is ball-milled to 1-10 microns and 100 portions of deionized water are evenly mixed, added into a three-neck flask, stirred at the speed of 100 plus 200r/min and simultaneously subjected to ultrasonic treatment with the ultrasonic power of 1.5-2.0kw and the ultrasonic time of 60-90min to obtain pearl powder slurry, then 1-5 portions of glycerol are dripped into the slurry, the dripping speed is controlled to be 30min, the reaction temperature is controlled to be 60-80 ℃, after the dripping is finished, the reaction is continued for 2-3h, after the reaction is finished, the aging is carried out for 2-3h, and the product is centrifuged, washed and dried to obtain the modified pearl powder.
Preferably, the humectant in the step one is a composition of one or more of glycerol, sorbitol, 1, 2-propylene glycol, butylene glycol and hyaluronic acid.
Preferably, the essence in the step one is one or a combination of orchid essence, rosemary essence, sandalwood essence and green tea essence.
Preferably, the preparation method of caprolactam based silicone oil described in the first step comprises:
according to the mass parts, 70 parts of methacryloyl ethyl sulfobetaine, 40 parts of N-vinyl caprolactam, 100 parts of hydrogen-containing silicone oil and 0.03-0.06 part of chloroplatinic acid are added into a dry three-neck flask, stirring is carried out at 300r/min of 200-85 ℃, the reaction temperature is controlled to be 80-85 ℃, nitrogen protection is introduced during the reaction process, the reaction time is 4-5h, a small amount of product is taken to measure the conversion rate of the hydrogen-containing silicone oil, when the conversion rate reaches more than 95%, 5-10 parts of N-propanol is added to react for 30min, then vacuumizing is carried out, the vacuum degree is 0.09MPa, the temperature is 85 ℃, unreacted substances are removed, and the caprolactam silicone oil is obtained.
Preferably, the thickener in step one is one or a combination of polyethylene glycol, hydroxyethyl cellulose, carbomer 940 and xanthan gum.
Preferably, the preparation method of the nymphaea hybrid extract in the step two comprises the following steps:
taking 100 parts of nymphaea hybrid petals according to the parts by mass, washing off impurities, drying, crushing, and sieving by a 60-80-mesh sieve to obtain powder; placing the powder in a supercritical carbon dioxide extraction device, adding 30-40 parts of absolute ethyl alcohol, controlling the flow of supercritical carbon dioxide at 15-20L/h, the extraction pressure at 15-20MPa, the extraction temperature at 40-50 ℃, the extraction time at 2-3h, and performing reduced pressure separation after extraction to obtain the nymphaea hybrid extract.
Preferably, the preservative in the second step is one or a combination of potassium sorbate, sorbic acid, sodium benzoate, benzoic acid and salicylic acid.
Part of reaction mechanism in the pearl powder modification process is shown as follows:
Figure GDA0003070020360000031
the method is characterized in that methacryloyl ethyl sulfobetaine, N-vinyl caprolactam and hydrogen-containing silicone oil are subjected to hydrosilylation, and part of reaction mechanism in the preparation process of the caprolactam silicone oil is as follows:
Figure GDA0003070020360000032
Figure GDA0003070020360000041
compared with the prior art, the invention has the beneficial effects that:
1. the modified pearl powder is added into the system, so that the pearl powder reaches the micron level, and the surface of the pearl powder is coated with the glycerol, so that the pearl powder exists in the essence more stably, and can penetrate into skin pores to play a better whitening role;
2. by adding methacryloyl ethyl sulfobetaine, N-vinyl caprolactam and hydrogen-containing silicone oil to perform hydrosilylation reaction, the compatibility of caprolactam silicone oil and skin is better, and a good moisturizing effect is achieved;
3. by adding the lotus extract into the essence, the essence has better whitening and moisturizing effects.
Drawings
FIG. 1 is a Fourier infrared spectrum of the modified pearl powder obtained in example 1:
at 1425cm-1An antisymmetric telescopic absorption peak of carbonate ions exists nearby and is at 885cm-1An out-of-plane bending absorption peak of carbonate ions is nearby and is 714cm-1The in-plane bending absorption peak of carbonate ions exists nearby, which indicates that the pearl powder participates in the reaction; at 2911cm-1The expansion and contraction absorption peak of hydrocarbon exists nearby and is 3357cm-1A stretching absorption peak of hydroxyl exists nearby and is 1094cm-1An out-of-plane rocking absorption peak of hydrocarbon exists nearby and is 914cm-1An out-of-plane bending absorption peak of hydroxyl exists nearby, so that the glycerol participates in the reaction;
Detailed Description
The raw materials used in the following examples are all commercially available products, and the examples are further illustrative of the present invention and do not limit the scope of the present invention;
the performance test methods are as follows:
in order to test the whitening and moisturizing effects of the essence, 90 persons of dry skin, oily skin and neutral skin volunteers in the same area are selected and divided into 9 groups (each group comprises 10 persons of dry skin, 10 persons of neutral skin and 10 persons of oily skin trial volunteers), A, B, C, D products are subjected to use investigation experiments respectively, after the face of each group of trial volunteers is cleaned, the products are applied to the face for 15min, the face is used once a day for 28 days, and the trial effects are observed and investigated.
1. Whitening effect: the whitening effect is divided into three categories of good, general and poor, and the number of people with each grade of the whitening effect is counted;
2. the moisturizing effect is as follows: the moisturizing effect is divided into three categories, namely good, general, poor and the like, and the number of people with the moisturizing effect in each grade is counted;
3. and (3) allergic reaction: the allergic reactions were classified into the presence and absence, and the number of people in both categories was counted.
Example 1
Step one, heating and dissolving: adding 100g of deionized water, 20g of modified pearl powder, 5g of glycerol, 0.1g of orchid essence, 5g of xylitol, 1g of caprolactam silicon oil, 1g of trehalose, 0.1g of citric acid and 1g of nicotinamide into a reaction kettle 1 subjected to high-temperature sterilization, starting stirring at the stirring speed of 200r/min, heating to 75 ℃, stirring for 1h to obtain a clear and transparent mixed solution, then scattering 0.1g of polyethylene glycol into the mixed solution while stirring, stirring for 0.5h, cooling the mixed solution to normal temperature after full dissolution, filtering the solution through a sterilized filter to remove undissolved impurities into a reaction kettle 2 subjected to high-temperature sterilization to obtain a solution;
step two, dissolving at normal temperature: adding 10g of nymphaea hybrid extract and 0.05g of sorbic acid into the solution, stirring for 30min at normal temperature, and discharging to obtain the non-irritant essence with whitening and moisturizing functions.
The preparation method of the modified pearl powder in the step one comprises the following steps:
uniformly mixing 10g of pearl powder ball-milled to 1 micron and 100g of deionized water, adding the mixture into a three-neck flask, stirring at 100r/min, carrying out ultrasonic treatment at the same time, wherein the ultrasonic power is 1.5kw, and the ultrasonic treatment time is 60min to obtain pearl powder slurry, then dripping 1g of glycerol into the slurry, controlling the dripping speed to be 30min, controlling the reaction temperature to be 60 ℃, continuing to react for 2h after the dripping is finished, aging for 2h after the reaction is finished, and centrifuging, washing and drying the product to obtain the modified pearl powder.
The preparation method of the caprolactam silicon oil comprises the following steps:
adding 60g of methacryloyl ethyl sulfobetaine, 30g of N-vinyl caprolactam, 100g of hydrogen-containing silicone oil and 0.03g of chloroplatinic acid into a dry three-neck flask, stirring at 200r/min, controlling the reaction temperature at 80 ℃, introducing nitrogen for protection in the reaction process, reacting for 4h, taking a small amount of product to measure the conversion rate of the hydrogen-containing silicone oil, adding 5g of n-propanol for reacting for 30min when the conversion rate reaches over 95%, vacuumizing, keeping the vacuum degree at 0.09MPa and the temperature at 85 ℃, and removing unreacted substances to obtain the caprolactam-based silicone oil.
The preparation method of the nymphaea hybrid extract comprises the following steps:
taking 100g of nymphaea hybrid petals, washing off impurities, drying, crushing, and sieving with a 60-mesh sieve to obtain powder; placing the powder in a supercritical carbon dioxide extraction device, adding 30g of absolute ethyl alcohol, controlling the flow of supercritical carbon dioxide at 15L/h, the extraction pressure at 20MPa, the extraction temperature at 40 ℃, the extraction time at 2h, and performing reduced pressure separation after extraction to obtain the nymphaea hybrid extract.
Example 2
Step one, heating and dissolving: adding 100g of deionized water, 21.3g of modified pearl powder, 7.2g of sorbitol, 0.1g of rosemary essence, 5.8g of xylitol, 1.5g of caprolactam silicon oil, 1.2g of trehalose, 0.1g of citric acid and 1.2g of nicotinamide into a reaction kettle 1 subjected to high-temperature sterilization, starting stirring at a stirring speed of 220r/min, heating to 77.8 ℃, stirring for 1.4h to obtain a clear and transparent mixed solution, then scattering 0.3g of hydroxyethyl cellulose into the mixed solution while stirring, stirring for 0.6h, cooling to normal temperature after full dissolution, filtering the solution through a sterilized filter to remove undissolved impurities into a reaction kettle 2 subjected to high-temperature sterilization to obtain a solution;
step two, dissolving at normal temperature: adding 10.8g of nymphaea hybrid extract and 0.06g of potassium sorbate into the solution, stirring at normal temperature for 37.8min, and discharging to obtain the non-irritant essence with whitening and moisturizing functions.
The preparation method of the modified pearl powder in the step one comprises the following steps:
uniformly mixing 11.8g of pearl powder ball-milled to 2.4 microns with 100g of deionized water, adding the mixture into a three-neck flask, stirring at 120r/min, carrying out ultrasonic treatment at the same time, wherein the ultrasonic power is 1.6kw, and the ultrasonic treatment time is 66.6min to obtain pearl powder slurry, then dripping 1.9g of glycerol into the slurry, controlling the dripping speed to be 33.6min, controlling the reaction temperature to be 63.2 ℃, continuing to react for 2.2h after finishing dripping, aging for 2.2h after finishing the reaction, and centrifuging, washing and drying the product to obtain the modified pearl powder.
The preparation method of the caprolactam silicon oil comprises the following steps:
adding 62g of methacryloyl ethyl sulfobetaine, 31.2g of N-vinyl caprolactam, 100g of hydrogen-containing silicone oil and 0.03g of chloroplatinic acid into a dry three-neck flask, stirring at 220r/min, controlling the reaction temperature at 81.4 ℃, introducing nitrogen for protection in the reaction process, reacting for 4.2h, taking a small amount of product to measure the conversion rate of the hydrogen-containing silicone oil, adding 6.4g of n-propanol for reacting for 38.4min when the conversion rate reaches over 95%, vacuumizing at the vacuum degree of 0.09MPa and the temperature of 88.6 ℃, and removing unreacted substances to obtain the caprolactam silicon oil.
The preparation method of the nymphaea hybrid extract comprises the following steps:
taking 100g of nymphaea hybrid petals, washing off impurities, drying, crushing, and sieving with a 65-mesh sieve to obtain powder; putting the powder into a supercritical carbon dioxide extraction device, adding 32g of absolute ethyl alcohol, controlling the flow of supercritical carbon dioxide at 16L/h, the extraction pressure at 19MPa, the extraction temperature at 41.6 ℃ and the extraction time at 2.2h, and performing reduced pressure separation after extraction to obtain the nymphaea hybrid extract.
Example 3
Step one, heating and dissolving: adding 100g of deionized water, 22.2g of modified pearl powder, 9g of 1, 2-propylene glycol, 0.2g of sandalwood essence, 6.8g of xylitol, 1.7g of caprolactam silicon oil, 1.4g of trehalose, 0.1g of citric acid and 1.3g of nicotinamide into a reaction kettle 1 subjected to high-temperature sterilization, starting stirring at the stirring speed of 240r/min, heating to 78.8 ℃, stirring for 1.6h to obtain a clear and transparent mixed solution, then scattering 0.4g of carbomer 940 into the mixed solution while stirring, stirring for 0.6h, cooling the mixed solution to normal temperature after full dissolution, filtering the solution through a sterilized filter to remove undissolved impurities into the reaction kettle 2 subjected to high-temperature sterilization to obtain a solution;
step two, dissolving at normal temperature: adding 11.4g of the nymphaea hybrid extract and 0.07g of sorbic acid into the solution, stirring at normal temperature for 43.8min, and discharging to obtain the non-irritant essence with whitening and moisturizing functions.
The preparation method of the modified pearl powder in the step one comprises the following steps:
uniformly mixing 13.6g of pearl powder ball-milled to 4.2 microns with 100g of deionized water, adding the mixture into a three-neck flask, stirring at 140r/min, carrying out ultrasonic treatment at the same time, wherein the ultrasonic power is 1.7kw, and the ultrasonic treatment time is 69.6min to obtain pearl powder slurry, then dripping 2.7g of glycerol into the slurry, controlling the dripping speed to be 37.8min, controlling the reaction temperature to be 68 ℃, continuing to react for 2.4h after finishing dripping, aging for 2.4h after finishing the reaction, and centrifuging, washing and drying the product to obtain the modified pearl powder.
The preparation method of the caprolactam silicon oil comprises the following steps:
adding 63g of methacryloyl ethyl sulfobetaine, 33.8g of N-vinyl caprolactam, 100g of hydrogen-containing silicone oil and 0.04g of chloroplatinic acid into a dry three-neck flask, stirring at 240r/min, controlling the reaction temperature at 82.1 ℃, introducing nitrogen for protection in the reaction process, reacting for 4.4h, taking a small amount of product to measure the conversion rate of the hydrogen-containing silicone oil, adding 7.6g of n-propanol for reacting for 44.4min when the conversion rate reaches over 95%, vacuumizing, controlling the vacuum degree to be 0.09MPa and the temperature to be 91 ℃, and removing unreacted reactants to obtain caprolactam silicone oil.
The preparation method of the nymphaea hybrid extract comprises the following steps:
taking 100g of nymphaea hybrid petals, washing off impurities, drying, crushing, and sieving with a 65-mesh sieve to obtain powder; putting the powder into a supercritical carbon dioxide extraction device, adding 33.4g of absolute ethyl alcohol, controlling the flow of supercritical carbon dioxide at 17L/h, the extraction pressure at 18MPa, the extraction temperature at 43.8 ℃, the extraction time at 2.4h, and performing reduced pressure separation after extraction to obtain the nymphaea hybrid extract.
Example 4
Step one, heating and dissolving: adding 100g of deionized water, 23.2g of modified pearl powder, 10g of butanediol, 0.3g of green tea essence, 7.7g of xylitol, 2g of caprolactam silicon oil, 1.5g of trehalose, 0.1g of citric acid and 1.4g of nicotinamide into a reaction kettle 1 subjected to high-temperature sterilization, starting stirring at the stirring speed of 260r/min, heating to 81.2 ℃, stirring for 2 hours to obtain a clear and transparent mixed solution, scattering 0.6g of xanthan gum into the mixed solution while stirring, stirring for 0.6 hour, cooling the mixed solution to normal temperature after full dissolution, filtering the solution through a sterilized filter to remove undissolved impurities to the reaction kettle 2 subjected to high-temperature sterilization to obtain a solution;
step two, dissolving at normal temperature: adding 12.5g of nymphaea hybrid extract and 0.08g of sodium benzoate into the solution, stirring at normal temperature for 49.8min, and discharging to obtain the non-irritant essence with whitening and moisturizing functions.
The preparation method of the modified pearl powder in the step one comprises the following steps:
uniformly mixing 15g of pearl powder ball-milled to 5.1 microns with 100g of deionized water, adding the mixture into a three-neck flask, stirring at 160r/min, carrying out ultrasonic treatment at the ultrasonic power of 1.8kw for 73.2min to obtain pearl powder slurry, then dripping 3.4g of glycerol into the slurry, controlling the dripping speed to be 40.8min, controlling the reaction temperature to be 70.8 ℃, continuing to react for 2.6h after finishing dripping, aging for 2.5h after the reaction is finished, and centrifuging, washing and drying the product to obtain the modified pearl powder.
The preparation method of the caprolactam silicon oil comprises the following steps:
adding 64.6g of methacryloyl ethyl sulfobetaine, 35g of N-vinyl caprolactam, 100g of hydrogen-containing silicone oil and 0.04g of chloroplatinic acid into a dry three-neck flask, stirring at 260r/min, controlling the reaction temperature to be 82.8 ℃, introducing nitrogen for protection in the reaction process, reacting for 4.6h, taking a small amount of product to measure the conversion rate of the hydrogen-containing silicone oil, adding 8.4g of n-propanol for reacting for 48.6min when the conversion rate reaches over 95%, vacuumizing at the vacuum degree of 0.09MPa and the temperature of 95.2 ℃, and removing unreacted substances to obtain the caprolactam silicon oil.
The preparation method of the nymphaea hybrid extract comprises the following steps:
taking 100g of nymphaea hybrid petals, washing off impurities, drying, crushing, and sieving with a 70-mesh sieve to obtain powder; putting the powder into a supercritical carbon dioxide extraction device, adding 35.6g of absolute ethyl alcohol, controlling the flow of supercritical carbon dioxide at 18L/h, the extraction pressure at 17MPa, the extraction temperature at 44.8 ℃, the extraction time at 2.5h, and performing reduced pressure separation after extraction to obtain the nymphaea hybrid extract.
Example 5
Step one, heating and dissolving: adding 100g of deionized water, 23.8g of modified pearl powder, 11.6g of hyaluronic acid, 0.3g of orchid essence, 8.9g of xylitol, 2.4g of caprolactam silicone oil, 1.6g of trehalose, 0.1g of citric acid and 1.6g of nicotinamide into a reaction kettle 1 subjected to high-temperature sterilization, starting stirring at a stirring speed of 280r/min, heating to 84 ℃, stirring for 2.2 hours to obtain a clear and transparent mixed solution, scattering 0.8g of xanthan gum into the mixed solution while stirring, stirring for 0.6 hour, cooling the mixed solution to normal temperature after full dissolution, filtering the solution through a sterilized filter to remove undissolved impurities into a reaction kettle 2 subjected to high-temperature sterilization to obtain a solution;
step two, dissolving at normal temperature: adding 13.4g of nymphaea hybrid extract and 0.09g of benzoic acid into the solution, stirring at normal temperature for 55.2min, and discharging to obtain the non-irritant essence with whitening and moisturizing functions.
The preparation method of the modified pearl powder in the step one comprises the following steps:
uniformly mixing 17g of pearl powder ball-milled to 6.1 microns with 100g of deionized water, adding the mixture into a three-neck flask, stirring at 180r/min, carrying out ultrasonic treatment at the ultrasonic power of 1.8kw for 79.8min to obtain pearl powder slurry, then dripping 4.2g of glycerol into the slurry, controlling the dripping speed to be 45min, controlling the reaction temperature to be 72.8 ℃, continuing to react for 2.8h after finishing the dripping, aging for 2.6h after the reaction is finished, and centrifuging, washing and drying the product to obtain the modified pearl powder.
The preparation method of the caprolactam silicon oil comprises the following steps:
adding 65.8g of methacryloyl ethyl sulfobetaine, 37.6g of N-vinyl caprolactam, 100g of hydrogen-containing silicone oil and 0.05g of chloroplatinic acid into a dry three-neck flask, stirring at 280r/min, controlling the reaction temperature at 83.8 ℃, introducing nitrogen for protection in the reaction process, reacting for 4.8h, taking a small amount of product to measure the conversion rate of the hydrogen-containing silicone oil, adding 9.6g of n-propanol for reacting for 54.6min when the conversion rate reaches over 95%, vacuumizing at the vacuum degree of 0.09MPa and the temperature of 97.6 ℃, and removing unreacted substances to obtain the caprolactam-based silicone oil.
The preparation method of the nymphaea hybrid extract comprises the following steps:
taking 100g of nymphaea hybrid petals, washing off impurities, drying, crushing, and sieving with a 75-mesh sieve to obtain powder; putting the powder into a supercritical carbon dioxide extraction device, adding 37.4g of absolute ethyl alcohol, controlling the flow of supercritical carbon dioxide at 19L/h, the extraction pressure at 16MPa, the extraction temperature at 47 ℃, the extraction time at 2.7h, and performing reduced pressure separation after extraction to obtain the nymphaea hybrid extract.
Example 6
Step one, heating and dissolving: adding 100g of deionized water, 25g of modified pearl powder, 15g of glycerol, 0.5g of rosemary essence, 10g of xylitol, 3g of caprolactam silicon oil, 2g of trehalose, 0.2g of citric acid and 2g of nicotinamide into a reaction kettle 1 subjected to high-temperature sterilization, starting stirring at the stirring speed of 300r/min, heating to 85 ℃, stirring for 3 hours to obtain a clear and transparent mixed solution, then scattering 1g of hydroxyethyl cellulose into the mixed solution while stirring, stirring for 1 hour, cooling the mixed solution to normal temperature after full dissolution, filtering the solution through a sterilized filter to remove undissolved impurities into the reaction kettle 2 subjected to high-temperature sterilization to obtain a solution;
step two, dissolving at normal temperature: adding 15g of nymphaea hybrid extract and 0.1g of salicylic acid into the solution, stirring for 60min at normal temperature, and discharging to obtain the non-irritant essence with whitening and moisturizing functions.
The preparation method of the modified pearl powder in the step one comprises the following steps:
uniformly mixing 20g of pearl powder ball-milled to 10 micrometers and 100g of deionized water, adding the mixture into a three-neck flask, stirring at 200r/min, carrying out ultrasonic treatment at the same time, wherein the ultrasonic power is 2kw, and the ultrasonic treatment time is 90min to obtain pearl powder slurry, then dripping 5g of glycerol into the slurry, controlling the dripping speed to be 60min, controlling the reaction temperature to be 80 ℃, continuing to react for 3h after finishing dripping, aging for 3h after the reaction is finished, and centrifuging, washing and drying the product to obtain the modified pearl powder.
The preparation method of the caprolactam silicon oil comprises the following steps:
adding 70g of methacryloyl ethyl sulfobetaine, 40g of N-vinyl caprolactam, 100g of hydrogen-containing silicone oil and 0.06g of chloroplatinic acid into a dry three-neck flask, stirring at 300r/min, controlling the reaction temperature at 85 ℃, introducing nitrogen for protection in the reaction process, reacting for 5h, taking a small amount of product to measure the conversion rate of the hydrogen-containing silicone oil, adding 10g of n-propanol for reacting for 60min when the conversion rate reaches over 95%, vacuumizing, keeping the vacuum degree at 0.09MPa and the temperature at 100 ℃, and removing unreacted substances to obtain the caprolactam-based silicone oil.
The preparation method of the nymphaea hybrid extract comprises the following steps:
taking 100g of nymphaea hybrid petals, washing off impurities, drying, crushing, and sieving with a 80-mesh sieve to obtain powder; putting the powder into a supercritical carbon dioxide extraction device, adding 40g of absolute ethyl alcohol, controlling the flow of supercritical carbon dioxide at 20L/h, the extraction pressure at 15MPa, the extraction temperature at 50 ℃ and the extraction time at 3h, and performing reduced pressure separation after extraction to obtain the nymphaea hybrid extract.
Comparative example 1
The amount of the pearl powder added in the first step was 0g with respect to example 1, and the rest was the same as in example 1.
Comparative example 2
The silicone oil added was not hydrophilically modified with respect to example 1, and the rest was the same as example 1.
Comparative example 3
The amount of lotus extract added was 0g with respect to example 1, and the rest was the same as example 1.
The experimental results of the comparative examples and examples are shown in the following table.
Figure GDA0003070020360000091
Figure GDA0003070020360000101
Figure GDA0003070020360000102
Figure GDA0003070020360000111

Claims (5)

1. A preparation method of non-irritant essence with whitening and moisturizing functions is characterized by comprising the following steps:
step one, heating and dissolving: adding 100 parts by mass of deionized water, 1-3 parts by mass of modified pearl powder, 5-15 parts by mass of humectant, 0.1-0.5 part by mass of essence, 5-10 parts by mass of xylitol, 1-3 parts by mass of caprolactam silicon oil, 1-2 parts by mass of trehalose, 0.1-0.2 part by mass of citric acid and 1-2 parts by mass of nicotinamide into a reaction kettle 1 subjected to high-temperature sterilization, starting stirring at a stirring speed of 200-300r/min, heating to 75-85 ℃, stirring for 1-3 hours to obtain a clear and transparent mixed solution, then scattering 0.1-1.0 part by mass of thickener into the mixed solution while stirring, stirring for 0.5-1 hour, cooling the mixed solution to normal temperature after full dissolution, filtering the solution through a sterilized filter to remove undissolved impurities into a reaction kettle 2 subjected to high-temperature sterilization, obtaining a solution;
step two, dissolving at normal temperature: adding 10-15 parts of nymphaea hybrid extract and 0.05-0.10 part of preservative into the solution, stirring for 30-60min at normal temperature, and discharging to obtain non-irritant essence with whitening and moisturizing functions;
the preparation method of the caprolactam silicon oil comprises the following steps:
adding 60-70 parts of methacryloyl ethyl sulfobetaine, 30-40 parts of N-vinyl caprolactam, 100 parts of hydrogen-containing silicone oil and 0.03-0.06 part of chloroplatinic acid into a dry three-neck flask according to the mass parts, stirring at 200-300r/min, controlling the reaction temperature at 80-85 ℃, introducing nitrogen for protection in the reaction process, reacting for 4-5h, taking a small amount of product to measure the conversion rate of the hydrogen-containing silicone oil, adding 5-10 parts of N-propanol for reacting for 30-60min when the conversion rate reaches over 95 percent, vacuumizing at the vacuum degree of 0.09MPa and the temperature of 85-100 ℃, and removing unreacted substances to obtain caprolactam silicon oil;
the preparation method of the modified pearl powder in the step one comprises the following steps:
uniformly mixing 10-20 parts of pearl powder which is ball-milled to 1-10 microns and 100 parts of deionized water according to the mass parts, adding the mixture into a three-neck flask, stirring at 200r/min with ultrasonic power of 1.5-2.0kw for 60-90min to obtain pearl powder slurry, then dripping 1-5 parts of glycerol into the slurry, controlling the dripping speed to be 30-60min, controlling the reaction temperature to be 60-80 ℃, continuing to react for 2-3h after the dripping is finished, aging for 2-3h after the reaction is finished, and centrifuging, washing and drying the product to obtain modified pearl powder;
the preparation method of the nymphaea hybrid extract comprises the following steps:
taking 100 parts of nymphaea hybrid petals according to the parts by mass, washing off impurities, drying, crushing, and sieving by a 60-80-mesh sieve to obtain powder; placing the powder in a supercritical carbon dioxide extraction device, adding 30-40 parts of absolute ethyl alcohol, controlling the flow of supercritical carbon dioxide at 15-20L/h, the extraction pressure at 15-20MPa, the extraction temperature at 40-50 ℃, the extraction time at 2-3h, and performing reduced pressure separation after extraction to obtain the nymphaea hybrid extract.
2. The method for preparing the non-irritating essence with whitening and moisturizing functions as claimed in claim 1, wherein the moisturizing agent in the step one is a composition of one or more of glycerin, sorbitol, 1, 2-propylene glycol, butylene glycol and hyaluronic acid.
3. The method for preparing the non-irritating essence with whitening and moisturizing functions as claimed in claim 1, wherein the essence in the first step is one or a combination of orchid essence, rosemary essence, sandalwood essence and green tea essence.
4. The method for preparing the non-irritating essence with whitening and moisturizing functions according to claim 1, wherein the thickening agent in the first step is one or a combination of polyethylene glycol, hydroxyethyl cellulose, carbomer 940 and xanthan gum.
5. The method for preparing the non-irritating essence with whitening and moisturizing functions according to claim 1, wherein the preservative in the second step is one or a combination of potassium sorbate, sorbic acid, sodium benzoate, benzoic acid and salicylic acid.
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