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:
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:
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.
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.