CN106726698B - Amino acid type facial cleanser and preparation method thereof - Google Patents

Amino acid type facial cleanser and preparation method thereof Download PDF

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CN106726698B
CN106726698B CN201611026663.6A CN201611026663A CN106726698B CN 106726698 B CN106726698 B CN 106726698B CN 201611026663 A CN201611026663 A CN 201611026663A CN 106726698 B CN106726698 B CN 106726698B
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amino acid
facial cleanser
acid type
type facial
surfactant
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CN106726698A (en
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张云岭
李洪海
倪向梅
洪奇
吕智
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Shanghai Inoherb Cosmetic 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
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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Abstract

The invention provides amino acid type facial cleanser, which comprises the following raw materials: 10-30 wt% of amino acid surfactant, 0.5-2 wt% of thickening agent, 0.2-2.5 wt% of neutralizing agent, 0.1-1 wt% of conditioning agent and deionized water. The invention also provides a preparation method of the amino acid type facial cleanser, which comprises the steps of firstly diluting the thickening agent, then adding the amino acid surfactant into the thickening agent, stirring and dissolving the amino acid surfactant, then adding the conditioner and the like, and standing overnight to obtain the amino acid type facial cleanser. The amino acid type facial cleanser provided by the invention is neutral, mild and skin-friendly, safe and non-irritant, does not increase skin burden, can deeply clean skin, quickly restores oil-water balance and acid-base balance after skin cleaning, is suitable for any skin type, and can be used for a long time. The product is emulsion appearance texture, has excellent look and feel and moisture retention, has excellent high and low temperature stability and certain thickness, and can meet good user experience.

Description

Amino acid type facial cleanser and preparation method thereof
Technical Field
The invention belongs to the technical field of daily cosmetics, relates to an amino acid type facial cleanser and a preparation method thereof, and particularly relates to a facial cleanser containing at least two amino acid surfactants and having high and low temperature stability and a preparation method thereof.
Background
Cleansing is an extremely important step for the maintenance of facial skin. If the skin care product is not cleaned, microorganisms are easy to breed in the retained grease and dirt to damage the skin, and a closed barrier is formed on the surface of the skin to influence the permeation and absorption of the subsequent skin care product.
The traditional soap-based facial cleansing cream takes fatty acid soap saponified by strong alkali as a main cleansing component, has strong degreasing force, can cause excessive loss of facial sebum and damage cuticle after long-term use, and causes excessive loss of skin and dryness and tightness; in addition, the pH value of the skin care product is high, so that the acid-base environment of the skin is greatly influenced, and the skin can be greatly irritated.
The amino acid facial cleanser takes the skin-friendly amino acid surfactant as a main cleaning component, and has moderate cleaning power and higher safety. The amino acid cleansing cream is weakly acidic or neutral, has less residue, and can really protect the health of skin and lead the trend of cleansing products due to the fact that the amino acid cleansing cream is close to the pH value of the surface of the skin. However, the following challenges are encountered in the development of the technology for cleansing products based on amino acid surfactants: 1) is difficult to thicken and keep stable for a long time, the appearance of the product is not smooth and fine, and the phenomenon of water separation can occur in the shelf life. 2) The stability at high and low temperature is not enough, the product can be thinned at high temperature, and the layered surface becomes rough under the low-temperature environment. These results in a lack of product quality and therefore a poor user experience.
The invention has application number 201410332325, and the inventive name is: the patent application of the amino acid facial cleanser containing sodium lauroyl glutamate surfactant provides an amino acid facial cleanser containing sodium lauroyl glutamate surfactant, but does not disclose the stability of the amino acid facial cleanser and does not detect the high-temperature and low-temperature performance of the facial cleanser.
The invention has application number 201010523235, and the inventive name is: chinese patent of an amino acid facial cleanser and a preparation method thereof discloses an amino acid facial cleanser with the content of sodium lauroyl glutamate surfactant being more than 25 percent and a preparation method thereof. The obtained product has good high-low temperature stability, but the surfactant is limited to sodium lauroyl glutamate, and the large-scale production of the product is limited due to the high price of the surfactant.
Disclosure of Invention
Aiming at the defects of the prior amino acid facial cleanser or facial cream technology, the invention provides the amino acid facial cleanser containing various amino acid surfactants and specific thickening agents and a preparation method thereof.
The first aspect of the invention provides an amino acid type facial cleanser, which comprises the following raw materials:
Figure BDA0001157952140000021
preferably, the amino acid type facial cleanser comprises the following raw materials:
Figure BDA0001157952140000022
in a preferred embodiment, the amino acid surfactant is a fatty acyl glycinate salt, preferably a mixture of potassium and sodium fatty acyl glycinates, more preferably a combination of any two or more of sodium cocoyl glycinate, potassium cocoyl glycinate, disodium cocoyl glutamate, sodium lauroyl glutamate, TEA cocoyl glutamate, and the like.
In a preferred embodiment, the mass ratio of the fatty acyl sodium glycinate to the fatty acyl potassium glycinate is 1: 0.1-1: 10, preferably 1: 0.3-1: 5, more preferably 1: 0.5-1: 3.
in a preferred embodiment, the thickening agent is any one or combination of polyvinylpyrrolidone, carbomer, acrylic acid and/or acrylic acid ester/C10-30 alkanol acrylate cross-linked polymer, polyvinyl methyl ether/methyl acrylate and decadiene cross-linked polymer, soybean protein gel and silica gel.
In a preferred embodiment, the amino acid type facial cleanser further comprises any one or more of non-amino acid surfactants, humectants, plant extract, pigments, pearling agents and inorganic salts.
Wherein, the non-amino acid surfactant comprises one or more of laurate, myristate, sodium dodecyl sulfate, laureth sulfate, cocamidopropyl betaine, cocoyl betaine, lauramidopropyl betaine, lauryl betaine, cocoamphoacetate and the like.
Preferably, the non-amino acid surfactant is present in an amount of 1-15 wt%, preferably 4-10 wt%, such as 5 wt%, 8 wt%, etc.
Preferably, the inorganic salt is any one or combination of sodium chloride and potassium chloride, and is preferably sodium chloride, the sodium chloride being present in an amount of 0.2 to 6 wt%, and preferably 2 to 5 wt%, such as 3 wt%, 4 wt%, etc.
Preferably, the humectant is one or a combination of more of polyalcohol and polysaccharide. More preferably, the humectant is one or a combination of glycerol, trehalose, sodium hyaluronate and natural moisturizing factor NMF.
Further, the content of the humectant is 5 to 30 wt%, and most preferably, the content of the humectant is 8 to 15 wt%, such as 10 wt%, 12 wt%, and the like.
In a preferred embodiment, the neutralizing agent is any one or combination of triethanolamine, tetrahydroxypropyl ethylenediamine, aminomethyl propanol, aminomethyl propanediol, tromethamine and arginine, and the pH value of the amino acid facial cleanser is adjusted to be 4.0-10.0.
In a preferred embodiment, the conditioning agent is preferably a cationic conditioning agent selected from one or more of polyquaternium-7, polyquaternium-39, polyquaternium-44, hexadecyltrimethylammonium chloride and dioctadecyldimethylammonium chloride.
In a preferred embodiment, the plant extract is any one or a combination of several of soapberry extract, rhodiola crenulata extract, camellia extract and witch hazel extract, and the content of the plant extract is 0.1-1 wt%, preferably 0.2-0.5 wt%.
In a preferred embodiment, the pigment is titanium dioxide powder and the content of the pigment is 0.1 to 2 wt%, preferably 0.4 to 1 wt%.
In a preferred embodiment, the pearlescent agent comprises ethylene glycol distearate and/or ethylene glycol stearate, more preferably, the pearlescent agent is present in an amount of 0.1 to 2 wt%, such as 0.5 wt%, 1.8 wt%, etc., most preferably 0.8 to 1.5 wt%, such as 1.0 wt%, 1.3 wt%.
In addition, the amino acid type facial cleanser provided by the invention can be added with any one or a combination of a plurality of essences, preservatives, pigments for cosmetics, nutritional additives and the like in a proper amount according to needs.
Another aspect of the present invention provides a method for preparing an amino acid type facial cleanser, comprising the steps of:
step 1, adding 0.5-2 wt% of thickening agent into a proper amount of deionized water, and uniformly stirring to obtain a diluted thickening agent;
step 2, adding 10-30 wt% of amino acid surfactant into the diluted thickening agent obtained in the step 1, heating to 80-90 ℃, stirring to dissolve for 30-60min, standing, and then adding 0.2-2.5 wt% of neutralizer into the mixture; cooling to 45-55 deg.C to obtain intermediate product;
and 3, adding 0.1-1 wt% of conditioner into the intermediate product obtained in the step 2, continuing stirring for 30-60min, and standing overnight to obtain the amino acid type facial cleanser.
In a preferred embodiment, before adding 0.1-1 wt% of the conditioning agent to the intermediate product obtained in step 2, a neutralizing agent is also added to the intermediate product to adjust the pH to 4.0-10.0, preferably to 6.0-8.0.
In a preferred embodiment, the step 3, when adding the conditioning agent, further comprises adding 0.1-2 wt% of whitening agent.
The invention has the following beneficial effects:
(1) the amino acid type facial cleanser provided by the invention is neutral, has the pH value of 4.0-10.0, is mild, is skin-friendly, safe and non-irritant, does not increase skin burden, can deeply clean skin, quickly restores oil-water balance and acid-base balance after skin cleaning, is suitable for any skin type, and can be used for a long time.
(2) The product has good appearance and texture, and has good appearance and moisture retention.
(3) The product has excellent high and low temperature stability and certain consistency, and meets good user experience.
Drawings
FIG. 1 is a graph showing the effect of inorganic salt content on the viscosity of the amino acid type facial cleanser provided by the present invention.
Detailed Description
The following will explain the performance of the amino acid type facial cleanser provided by the invention and the preparation method thereof by combining specific examples.
Examples one to eight
Adding U20 (acrylic acid or acrylic ester/C10-30 alkanol acrylate cross-linked polymer) and deionized water into an emulsifying pot, stirring to uniformly disperse the mixture, adding sodium cocoyl glycinate and potassium cocoyl glycinate into the emulsifying pot, heating to 80-85 ℃, stirring to dissolve for 45min, and slightly standing for 30-60min to eliminate surface bubbles; cooling to 45-55 deg.C, adding triethanolamine for neutralization; and (3) continuously cooling to 45-50 ℃, adding other components according to the mass ratio, continuously stirring for 30min, keeping the temperature to 45-50 ℃, completely and uniformly dispersing the components, discharging, and standing for 12h to obtain the amino acid type facial cleanser, wherein the amino acid type facial cleanser is an emulsion product, the mass percentage of each component is shown in table 1, and the evaluation data of the amino acid type facial cleansers prepared in the embodiments are shown in fig. 1 and table 2.
TABLE 1 Effect of sodium chloride content on product Properties
Figure BDA0001157952140000051
Wherein U20 is acrylic acid or acrylic ester/C10-30 alkanol acrylate cross-linked polymer(s) ((
Figure BDA0001157952140000052
Ultrez 20Polymer, Lu Bo run management (Shanghai) Co., Ltd.);
table 2, performance testing of products prepared in examples one to eight
Figure BDA0001157952140000053
Figure BDA0001157952140000061
Wherein the pH value is measured by a direct measurement method, namely the pH value measured by putting a pH meter electrode into an undiluted sample at the temperature of 25 ℃.
The viscosity is measured by the detection method described in GB/T15357-2014, and the rotating speed is 20 rpm.
15 ℃/25 ℃ (3 cycles) test: the sample was placed in a freezing chamber at-15 ℃ for 24 hours, taken out, and then kept at 25 ℃ for 25 hours, as one cycle, and the cycle was repeated 3 times for observation and testing. The following tests, using the same test method.
O: the representative stability is good; x: indicating delamination and/or a roughened appearance of the sample.
As can be seen from fig. 1 and table 2, in the same formulation system, when U20 is used as a thickener and the content of U20 is 1 wt%, the addition amount of sodium chloride is in the range of 0.5 to 4 wt%, and the viscosity of the amino acid type facial cleanser rapidly increases as the salt content increases. In the first to third examples, the content of sodium chloride is less than 2 wt%, and the prepared amino acid type facial cleanser has a product viscosity of less than 3000MPas and is easy to be in an unstable state of high-temperature demixing and low-temperature thickening. Since sodium chloride reduces the foam content of the product, it is preferred that the sodium chloride content is less than 5 wt%.
Example nine to example fourteen
Adding U20 (acrylic acid or acrylic ester/C10-30 alkanol acrylate cross-linked polymer) and deionized water into an emulsifying pot, stirring to uniformly disperse the mixture, adding sodium cocoyl glycinate and/or potassium cocoyl glycinate into the emulsifying pot, heating to 80-85 ℃, stirring to dissolve for 45min, and slightly standing for 30-60min to eliminate surface bubbles; cooling to 45-55 deg.C, adding triethanolamine for neutralization; and (3) continuously cooling to 45-50 ℃, adding other components according to the mass ratio, continuously stirring for 30min, keeping the temperature to 45-50 ℃, completely and uniformly dispersing the components, discharging, standing for 12h to obtain the amino acid type facial cleanser, wherein the amino acid type facial cleanser is an emulsion product, the mass percentage of each component is shown in table 3, the performances of the amino acid type facial cleansers prepared in different embodiments are examined, and the results are shown in table 4.
TABLE 3 influence of amino acid surfactant type and ratio on product Performance
Figure BDA0001157952140000071
Table 4, performance testing of products prepared in examples nine to fourteen
Figure BDA0001157952140000072
Wherein the meanings of the symbols and the test methods of the properties are the same as those in Table 2.
From the above data analysis we can conclude that:
EXAMPLES nine to eleventh examples to examine the influence of the amino acid pair on the product performance, the type and content of the salt (sodium chloride, 0.8 wt% in each case) and the type and content of the thickener (U20, 0.8 wt% in each case) were kept unchanged. Example nine using sodium cocoyl glycinate alone, a higher viscosity of 8280MPas, which is easily achieved with the amino acid type facial cleanser, but which is easily thickened at low temperature to cause system instability, was easily achieved. In the tenth example, the single potassium cocoyl glycinate is used, and the viscosity of the amino acid type facial cleanser is low and is 1900MPas, so that the product is easy to generate high-temperature stratification.
In the eleventh embodiment, the ratio of sodium cocoyl glycinate to potassium cocoyl glycinate is adjusted without changing the total amount, so that the viscosity of the obtained amino acid type facial cleanser is 5100MPas, and the high-temperature and low-temperature stability of the product is excellent.
In example twelve, without changing the total amount of sodium cocoyl glycinate and potassium cocoyl glycinate, the relative content of sodium cocoyl glycinate was increased from 7 to 9 wt% compared to example eleven, resulting in a product with a viscosity increasing from 5100 to 6000MPas, and therefore it can be concluded that: sodium salts promote an increase in product viscosity more readily than potassium salts.
Because the influence of the potassium salt on the viscosity of the product is small, the content of the potassium cocoyl glycinate is reduced, the viscosity of the product cannot be greatly reduced, in the thirteenth embodiment, the content of the potassium cocoyl glycinate is reduced, the content of the sodium chloride is greatly increased, and compared with the viscosity of the twelfth embodiment, the obtained product is not increased but reduced, which shows that the salt and the amino acid have a synergistic effect in the process of preparing the product. In the thirteen embodiment and the fourteenth embodiment, the viscosity of the product can be controlled within a certain range by adjusting the relative content of the amino acid and the sodium chloride, and the obtained product can keep stable in the high and low temperature stability test.
Example fifteen to example eighteen:
adding thickener and deionized water into emulsifying pot, stirring to disperse uniformly, adding potassium myristoyl glycinate and sodium myristoyl glycinate at different ratios into emulsifying pot, heating to 80-85 deg.C, stirring for dissolving for 45min, and standing for 30-60min to eliminate liquid surface bubble; cooling to 45-55 deg.C, adding corresponding neutralizer to adjust pH value of the system; and (3) continuously cooling to 45-50 ℃, adding other components according to the mass ratio, continuously stirring for 30min, keeping the temperature to 45-50 ℃, completely and uniformly dispersing the components, discharging, standing for 12h to obtain the amino acid type facial cleanser, wherein the amino acid type facial cleanser is an emulsion product, the mass percentage of each component is shown in table 5, and the performance of the amino acid type facial cleansers prepared in different embodiments is examined, and the result is shown in table 6.
TABLE 5 Effect of thickener type on product Properties
Figure BDA0001157952140000091
Wherein U20 is acrylic acid or acrylic ester/C10-30 alkanol acrylate cross-linked polymer(s) ((
Figure BDA0001157952140000092
Ultrez 20Polymer, Lu Bo run management (Shanghai) Co., Ltd.);
SC200 is acrylic acid or acrylic ester/C10-30 alkanol acrylate crosspolymer (
Figure BDA0001157952140000093
SC-200Polymer, Lo Borun management (Shanghai) Co., Ltd.);
SF-1 is acrylic acid or acrylate copolymer (Carbopol Aqua SF-1, Loborun management (Shanghai) Co., Ltd.);
STRUCTUREXL (hydroxypropyl starch phosphate, Acksonobel, Inc.).
Table 6, performance testing of products prepared in examples fifteen to eighteen
Figure BDA0001157952140000101
Wherein the meanings of the symbols and the test methods of the properties in Table 6 are the same as those in Table 2.
As can be seen from table 6, the amino acid facial cleansers prepared in the fifteen to seventeenth examples have stable high and low temperature performance, and the viscosity of the product is above 3000MPas, while the amino acid facial cleansers prepared in the eighteen examples have unstable high and low temperature performance, and the product is delaminated at high temperature, but the product becomes rougher at low temperature, and the stability requirements cannot be met at high and low temperature. Example eighteen the viscosity of the amino acid facial cleanser prepared according to the present invention is 1200MPas, therefore, it is presumed that since titanium dioxide is added to the amino acid facial cleanser prepared according to the present invention, in order to maintain the stability of titanium dioxide in the product, a thickener is required to provide a certain suspending power while thickening, and as can be seen from table 4, when the viscosity is above 3000MPas, the product has excellent stability, and acrylic acid or acrylic ester/C10-30 alkanol acrylic ester cross-linked polymer, typically representing the trade name of raw materials:
Figure BDA0001157952140000102
ultrez 20Polymer and
Figure BDA0001157952140000103
SC-200Polymer, acrylic or acrylate copolymer, typically under the trade name of the raw materials: carbopol Aqua SF-1. The thickening agent has the characteristics of thickeningCertain suspended particle function. Hydroxypropyl starch phosphate (starch XL) has a thickening effect, but has a relatively weak suspending ability, resulting in insufficient product stability.
Example nineteenth to example twenty
(ii) SC200 is acrylic acid or acrylic ester/C10-30 alkanol acrylate crosspolymer: (
Figure BDA0001157952140000104
SC-200Polymer, Lubomoisten additive (Zhuhai) Co., Ltd.) and deionized water are added into an emulsifying pot, stirred to be uniformly dispersed, then sodium cocoyl glycinate and potassium cocoyl glycinate are added into the emulsifying pot, heated to 80-85 ℃, stirred to be dissolved for 45min, and slightly kept stand for 30-60min to eliminate liquid surface vapor bubbles; cooling to 45-55 deg.C, adding triethanolamine for neutralization; and (3) continuously cooling to 45-50 ℃, adding other components according to the mass ratio, continuously stirring for 30min, keeping the temperature to 45-50 ℃, completely and uniformly dispersing the components, discharging, standing for 12h to obtain the amino acid type facial cleanser, wherein the amino acid type facial cleanser is an emulsion product, the mass percentage of each component is shown in table 7, and the performance of the amino acid type facial cleansers prepared in different embodiments is examined, and the result is shown in table 8.
TABLE 7 Effect of thickener type on product Properties
Figure BDA0001157952140000111
Table 8, nineteen examples and twenty examples the performance tests of the products prepared
Figure BDA0001157952140000112
Figure BDA0001157952140000121
In table 8, the meanings of the symbols and the test methods for the properties are the same as those in table 2.
Example twenty compared to example nineteen, only the sodium chloride and triethanolamine content was increased. From the first to eighth examples, it is understood that the addition amount of sodium chloride is in the range of 0.5 to 4 wt%, and the viscosity of the amino acid type facial cleanser rapidly increases as the sodium chloride content increases. In the twenty embodiment, compared with the nineteen embodiment, the viscosity of the amino acid facial cleanser is not increased but decreased, which shows that the viscosity of the amino acid facial cleanser provided by the invention is decreased along with the increase of the pH value, because the solubility of the cocoyl glycinate is higher than that of the cocoyl glycine, the lower the pH value, the more insoluble substances are, the higher the viscosity is, but the lower the pH value is, the coarser the material body is, and the optimal pH value of the formula is set to be 6.0-8.0.

Claims (10)

1. An amino acid type facial cleanser comprising:
Figure FDA0002325728570000011
the method is characterized in that:
the amino acid surfactant is a mixture of fatty acyl sodium glycinate and fatty acyl potassium glycinate, and the mass ratio of the fatty acyl sodium glycinate to the fatty acyl potassium glycinate is 1: 0.1-1: 10;
the inorganic salt is any one or combination of sodium chloride and potassium chloride, and the thickening agent is selected from carbomer, acrylic acid or acrylic ester/C10-30 alkanol acrylate cross-linked polymer, polyvinyl methyl ether/methyl acrylate and decadiene cross-linked polymer, and acrylic acid or acrylic ester copolymer;
the viscosity of the amino acid type facial cleanser is more than 3000 mPa.s.
2. The amino acid type facial cleanser according to claim 1, comprising:
Figure FDA0002325728570000012
3. the amino acid type facial cleanser according to claim 1, wherein the mass ratio of fatty acyl sodium glycinate to fatty acyl potassium glycinate is 1: 0.3-1: 5.
4. the amino acid type facial cleanser according to claim 1, wherein said thickener is selected from the group consisting of acrylic acid or acrylic ester/C10-30 alkanol acrylate crosspolymer, and acrylic acid or acrylic ester copolymer.
5. The amino acid facial cleanser of claim 1, further comprising one or more of a non-amino acid surfactant, a moisturizer, a plant extract, a pigment and a pearlizing agent.
6. The amino acid type facial cleanser according to claim 1, wherein the content of said inorganic salt is 2 to 5% by weight.
7. The amino acid type facial cleanser according to claim 5, wherein the non-amino acid type surfactant is any one or a combination of lauric acid salt, myristic acid salt, sodium lauryl sulfate, laureth sulfate, cocamidopropyl betaine, cocoyl betaine, lauramidopropyl betaine, lauryl betaine, cocoamphoacetate and the like, and the content of the non-amino acid type surfactant is 1-15 wt%.
8. The amino acid facial cleanser of claim 1, wherein the neutralizing agent is any one or a combination of triethanolamine, tetrahydroxypropylethylenediamine, aminomethyl propanol, aminomethyl propylene glycol, tromethamine and arginine, and the pH value of the amino acid facial cleanser is adjusted to 6.0-8.0.
9. A method for producing the amino acid type face cleansing cream of claim 1, comprising the steps of:
step 1, adding 0.5-2 wt% of thickening agent into a proper amount of deionized water, and uniformly stirring to obtain a diluted thickening agent;
step 2, adding 10-30 wt% of amino acid surfactant into the diluted thickening agent obtained in the step 1, heating to 80-90 ℃, stirring to dissolve for 30-60min, standing, and then adding 0.2-2.5 wt% of neutralizer into the mixture; cooling to 45-55 deg.C to obtain intermediate product;
and 3, adding 0.1-1 wt% of conditioner into the intermediate product obtained in the step 2, continuing stirring for 30-60min, and standing overnight to obtain the amino acid type facial cleanser.
10. The method for preparing an amino acid type facial cleanser according to claim 9, wherein a neutralizing agent is further added to said intermediate product obtained in step 2 to adjust the pH to 6.0 to 8.0 before 0.1 to 1 wt% of a conditioning agent is added to said intermediate product.
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