CN116462704A - Strong-effect cleaning facial cleanser and preparation method thereof - Google Patents

Strong-effect cleaning facial cleanser and preparation method thereof Download PDF

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CN116462704A
CN116462704A CN202310444463.6A CN202310444463A CN116462704A CN 116462704 A CN116462704 A CN 116462704A CN 202310444463 A CN202310444463 A CN 202310444463A CN 116462704 A CN116462704 A CN 116462704A
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facial cleanser
gemini emulsifier
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gemini
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CN116462704B (en
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郑亚桐
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Guangzhou Lingkang Cosmetics Co ltd
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Guangzhou Xiagang Technology 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
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/55Phosphorus compounds
    • A61K8/553Phospholipids, e.g. lecithin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/005Antimicrobial preparations
    • 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
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/10Washing or bathing preparations
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00Compounds containing elements of Groups 5 or 15 of the Periodic Table
    • C07F9/02Phosphorus compounds
    • C07F9/06Phosphorus compounds without P—C bonds
    • C07F9/08Esters of oxyacids of phosphorus
    • C07F9/09Esters of phosphoric acids
    • C07F9/091Esters of phosphoric acids with hydroxyalkyl compounds with further substituents on alkyl
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K23/00Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
    • C09K23/14Derivatives of phosphoric acid
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
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  • Dermatology (AREA)
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Abstract

The invention provides a powerful cleaning facial cleanser and a preparation method thereof, and belongs to the technical field of facial cleansers. The preparation method comprises the following raw materials in parts by weight: the Gemini emulsifier of claim 1, wherein the Gemini emulsifier comprises 8-10 parts of a vitamin C1-2 parts of a hyaluronic acid 3-5 parts of a hyaluronic acid, 0.5-1 part of a xanthan gum, 3-5 parts of diatomite, 0.1-0.5 part of sodium citrate, 3-5 parts of glycerin, 1-2 parts of butylene glycol, 0.5-1 part of carbomer, 3-5 parts of jojoba oil, 0.5-1 part of arbutin and 70-90 parts of deionized water. The strong cleaning face washing prepared by the invention has better cleaning strength, moisture retention and air permeability; the product can deeply clean pores, effectively remove grease, dust, solid particles and the like on the surface of the skin, form an effective protective barrier on the surface of the skin, has the effects of whitening and moisturizing, and has stronger cleaning force.

Description

Strong-effect cleaning facial cleanser and preparation method thereof
Technical Field
The invention relates to the technical field of facial cleanser, in particular to a strong-efficiency cleaning facial cleanser and a preparation method thereof.
Background
With the improvement of living and cultural level of people, skin care is more and more paid attention to, and skin cleaning is the most important step of skin care. If the skin is not thoroughly cleaned, dirt remaining on the skin can clog hair follicles, making the skin look rough, shinless, and may cause acne, facial blisters, or other skin-related problems.
The facial cleanser belongs to a skin-cleaning cosmetic, and has the functions of removing dirt on skin, refreshing the skin and being beneficial to maintaining the normal physiological state of the skin. At present, facial cleaning products on the market are various, part of the products use soap base as a main cleaning agent, the foam is rich, the detergency is strong, the degreasing property is strong, the user feels tight after using the facial cleaning products, the property of the part of the emulsified products is mild, the decontamination effect is poor, the user can hardly make rich foam, and the user feels greasy after washing. Although the environmental protection consciousness of people is enhanced at present, dust pollution sometimes happens, if dust suspended particles are not cleaned, skin conditions such as large pores and excessive secretion of grease can be caused, so that the skin has the problems of fine lines, wrinkling, sagging and dryness, acne, vaccinia acne and the like. In addition, the solid particles have a smaller particle size and are more likely to deposit deep in pores, and thorough cleaning is therefore necessary.
Disclosure of Invention
The invention aims to provide a powerful cleaning facial cleanser and a preparation method thereof, which have better cleaning strength, moisture retention and air permeability; the product can deeply clean pores, effectively remove grease, dust, solid particles and the like on the surface of the skin, form an effective protective barrier on the surface of the skin, has the effects of whitening and moisturizing, and has stronger cleaning force.
The technical scheme of the invention is realized as follows:
the invention provides a Gemini emulsifier which has a structure shown in the following formula I:
wherein r=c n H 2n+1 ,n=12-18。
The invention further provides a preparation method of the Gemini emulsifier, which comprises the following steps:
s1, reacting long carbon chain fatty alcohol and phosphorus oxychloride to prepare an intermediate A, wherein the structure is as follows:wherein, the structural formula of the long carbon chain fatty alcohol is as follows: ROH, r=c n H 2n+1 ,n=12-18;
S2, reacting the intermediate A with ethylene glycol to prepare an intermediate B, wherein the structure is as follows:
s3, reacting N, N, N ', N' -tetramethyl ethylenediamine with the intermediate B to obtain the Gemini emulsifier.
As a further improvement of the invention, the ratio of the amounts of the long carbon chain fatty alcohol and phosphorus oxychloride in the step S1 is 1:1-1.2.
As a further improvement of the present invention, the ratio of the amounts of the intermediate A and ethylene glycol in step S2 is 1:1 to 1.1.
As a further improvement of the invention, the mass ratio of the N, N, N ', N' -tetramethyl ethylenediamine to the intermediate B in the step S3 is 1-1.1:2.
As a further improvement of the invention, the method specifically comprises the following steps:
s1, adding 1 molar equivalent of long carbon chain fatty alcohol and 1-1.2 molar equivalents of phosphorus oxychloride into dichloromethane, adding 3-5 molar equivalents of NaOH, carrying out reflux reaction for 1-2h, carrying out reduced pressure distillation, washing with diethyl ether, and drying to obtain an intermediate A;
s2, adding 1 molar equivalent of the intermediate A and 1-1.1 molar equivalent of ethylene glycol into dichloromethane, carrying out reflux reaction for 2-4h, carrying out reduced pressure distillation, washing with diethyl ether, and drying to obtain an intermediate B;
s3, adding 1-1.1 molar equivalent of N, N, N ', N' -tetramethyl ethylenediamine and 2 molar equivalents of intermediate B into acetonitrile, carrying out reflux reaction for 3-5h, filtering, washing, and drying with ethanol to obtain the Gemini emulsifier.
The invention further protects a strong cleaning facial cleanser, which contains the Gemini emulsifier.
As a further improvement of the invention, the content of the Gemini emulsifier is 7-12wt%.
As a further improvement of the invention, the invention is prepared from the following raw materials in parts by weight: 8-10 parts of the Gemini emulsifier, 1-2 parts of vitamin C, 3-5 parts of hyaluronic acid, 0.5-1 part of xanthan gum, 3-5 parts of diatomite, 0.1-0.5 part of sodium citrate, 3-5 parts of glycerin, 1-2 parts of butanediol, 0.5-1 part of carbomer, 3-5 parts of jojoba oil, 0.5-1 part of arbutin and 70-90 parts of deionized water.
The invention further provides a preparation method of the powerful cleaning facial cleanser, which comprises the following steps of:
(1) Dissolving a Gemini emulsifier, carbomer, vitamin C, hyaluronic acid and xanthan gum in deionized water to obtain a material 1;
(2) Mixing glycerol, butanediol, jojoba oil and arbutin under stirring for 10-15min to obtain material 2;
(3) Mixing the material 1 and the material 2, adding sodium citrate and diatomite, stirring and mixing for 10-20min, emulsifying for 3-5min with 12000-15000r/min, and discharging to obtain the strong cleaning facial cleanser.
The invention has the following beneficial effects: the Gemini emulsifier is synthesized by the method, and has the advantages of simple preparation process, mild reaction conditions and high yield, and two (or more) hydrophilic groups are connected by chemical bonds through the connecting groups, so that two (or more) surfactant monomers are combined very tightly. The structure enhances the hydrophobic effect of hydrocarbon chains on one hand, increases the escape trend of hydrophobic groups from aqueous solution, has better foamability, emulsifying agent, dispersion performance and the like, and meanwhile, the quaternary ammonium salt structure has good antibacterial and bacteriostatic properties and obviously enhances the cleaning capability.
Compared with the common facial cleanser, the strong cleaning facial cleanser has better cleaning strength, moisture retention and air permeability; the product can deeply clean pores, effectively remove grease, dust, solid particles and the like on the surface of the skin, form an effective protective barrier on the surface of the skin, has the effects of whitening and moisturizing, and has stronger cleaning force.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is a synthetic route diagram of Gemini emulsifier in example 1 of the present invention.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a Gemini emulsifier, as shown in fig. 1, specifically comprising the following steps:
s1, 1mol of long carbon chain fatty alcohol (the structural formula of the long carbon chain fatty alcohol is as follows: ROH, R=C 12 H 25 Adding 1mol of phosphorus oxychloride into dichloromethane, adding 3mol of NaOH, carrying out reflux reaction for 1h, carrying out reduced pressure distillation, washing with diethyl ether, and drying to obtain an intermediate A;
s2, adding 1mol of the intermediate A and 1mol of ethylene glycol into dichloromethane, carrying out reflux reaction for 2 hours, carrying out reduced pressure distillation, washing with diethyl ether, and drying to obtain an intermediate B;
s3, adding 1mol of N, N' -tetramethyl ethylenediamine and 2mol of intermediate B into acetonitrile, carrying out reflux reaction for 3h, filtering, washing, and drying with ethanol to obtain the Gemini emulsifier with the total yield of 90%.
Example 2
The embodiment provides a Gemini emulsifier, as shown in fig. 1, specifically comprising the following steps:
s1, 1mol of long carbon chain fatty alcohol (the structural formula of the long carbon chain fatty alcohol is as follows: ROH, R=C 18 H 37 ) Adding 1.2mol of phosphorus oxychloride into dichloromethane, adding 5mol of NaOH, carrying out reflux reaction for 2 hours, carrying out reduced pressure distillation, washing with diethyl ether, and drying to obtain the intermediateA;
S2, adding 1mol of the intermediate A and 1.1mol of ethylene glycol into dichloromethane, carrying out reflux reaction for 4 hours, carrying out reduced pressure distillation, washing with diethyl ether, and drying to obtain an intermediate B;
s3, adding 1.1mol of N, N' -tetramethyl ethylenediamine and 2mol of intermediate B into acetonitrile, carrying out reflux reaction for 5 hours, filtering, washing, drying by ethanol, and thus obtaining the Gemini emulsifier with the total yield of 87%.
Example 3
The embodiment provides a Gemini emulsifier, as shown in fig. 1, specifically comprising the following steps:
s1, 1mol of long carbon chain fatty alcohol (the structural formula of the long carbon chain fatty alcohol is as follows: ROH, R=C 14 H 29 Adding 1.1mol of phosphorus oxychloride into dichloromethane, adding 4mol of NaOH, carrying out reflux reaction for 1.5h, carrying out reduced pressure distillation, washing with diethyl ether, and drying to obtain an intermediate A;
s2, adding 1mol of the intermediate A and 1.05mol of ethylene glycol into dichloromethane, carrying out reflux reaction for 3 hours, carrying out reduced pressure distillation, washing with diethyl ether, and drying to obtain an intermediate B;
s3, adding 1.05mol of N, N' -tetramethyl ethylenediamine and 2mol of intermediate B into acetonitrile, carrying out reflux reaction for 4 hours, filtering, washing, drying by ethanol, and obtaining the Gemini emulsifier with the total yield of 90%.
Example 4
The embodiment provides a strong cleaning facial cleanser.
The raw materials comprise the following components in parts by weight: 8 parts of Gemini emulsifier, 1 part of vitamin C, 3 parts of hyaluronic acid, 0.5 part of xanthan gum, 3 parts of diatomite, 0.1 part of sodium citrate, 3 parts of glycerin, 1 part of butanediol, 0.5 part of carbomer, 3 parts of jojoba oil, 0.5 part of arbutin and 70 parts of deionized water.
The method comprises the following steps:
(1) Dissolving a Gemini emulsifier, carbomer, vitamin C, hyaluronic acid and xanthan gum in deionized water to obtain a material 1;
(2) Mixing glycerol, butanediol, jojoba oil and arbutin for 10min to obtain material 2;
(3) Mixing the material 1 and the material 2, adding sodium citrate and diatomite, stirring and mixing for 10min, emulsifying for 3min at 12000r/min, and discharging to obtain the strong cleaning facial cleanser.
Example 5
The embodiment provides a strong cleaning facial cleanser.
The raw materials comprise the following components in parts by weight: 10 parts of Gemini emulsifier, 2 parts of vitamin C, 5 parts of hyaluronic acid, 1 part of xanthan gum, 5 parts of diatomite, 0.5 part of sodium citrate, 5 parts of glycerin, 2 parts of butanediol, 1 part of carbomer, 5 parts of jojoba oil, 1 part of arbutin and 90 parts of deionized water.
The method comprises the following steps:
(1) Dissolving a Gemini emulsifier, carbomer, vitamin C, hyaluronic acid and xanthan gum in deionized water to obtain a material 1;
(2) Mixing glycerol, butanediol, jojoba oil and arbutin for 15min to obtain material 2;
(3) Mixing the material 1 and the material 2, adding sodium citrate and diatomite, stirring and mixing for 20min, emulsifying for 5min at 15000r/min, and discharging to obtain the strong cleaning facial cleanser.
Example 6
The embodiment provides a strong cleaning facial cleanser.
The raw materials comprise the following components in parts by weight: 9 parts of Gemini emulsifier, 1.5 parts of vitamin C, 4 parts of hyaluronic acid, 0.7 part of xanthan gum, 4 parts of kieselguhr, 0.3 part of sodium citrate, 4 parts of glycerin, 1.5 parts of butanediol, 0.7 part of carbomer, 4 parts of jojoba oil, 0.7 part of arbutin and 80 parts of deionized water.
The method comprises the following steps:
(1) Dissolving a Gemini emulsifier, carbomer, vitamin C, hyaluronic acid and xanthan gum in deionized water to obtain a material 1;
(2) Mixing glycerol, butanediol, jojoba oil and arbutin for 12min to obtain material 2;
(3) Mixing the material 1 and the material 2, adding sodium citrate and diatomite, stirring and mixing for 15min, emulsifying for 4min at 13500r/min, and discharging to obtain the strong cleaning facial cleanser.
Comparative example 1
The difference compared with example 6 is that the Gemini emulsifier prepared in example 3 is not added.
Test example 1 cleaning force test
50 subjects 18-32 years old were randomly equally divided into 5 groups of 10 persons each, and the effect test was performed on the powerful cleansing facial cleanser prepared in examples 4-6 and comparative example 1, and the like on the commercial products:
(1) Deoiling effect: testing the skin grease content of the inner side of the forearm of a subject before and after the facial cleanser is used, calculating the skin grease content reduction rate of each subject, and taking an average value of each group;
(2) Exfoliating effect: skin roughness on the inner side of the forearm of each subject was tested before use of the facial cleanser; after 10 days of facial cleanser application (usage cycle was once per day), the skin roughness of the front inner side of each subject was again examined, and the reduction rate was calculated, and the average value was taken for each group.
The results are shown in Table 1.
TABLE 1
Group of Grease reduction Rate (%) Roughness reduction ratio (%)
Example 4 92.2 27.2
Example 5 93.1 27.9
Example 6 94.7 28.0
Comparative example 1 77.2 18.2
Commercially available 72.5 15.3
As shown in the table above, the powerful cleansing facial cleanser prepared in examples 4 to 6 of the present invention has a better grease cleaning effect and also has a certain removal effect on the cutin of the skin.
Test example 2 human skin patch test
1. Test article: the powerful cleansing facial cleanser prepared in example 4
2. Negative control: deionized water
3. The subject: 30 people, 0 man and 30 woman, are aged 20-25 years, and meet the volunteer selection standard of the subjects.
4. The patch method comprises the following steps: selecting a qualified patch tester, adding about 0.5mL of a test object and a negative control into the patch tester by a closed patch test method, applying a special adhesive tape for external use on the back of a subject, removing the test object after 24 hours, observing skin reactions after 0.5, 24 and 48 hours respectively, and recording the results according to skin reaction grading standards in cosmetic health Specification (2007 edition). The test results are shown in Table 1:
TABLE 1 human skin patch test results
The test results of the human skin patch show that: skin adverse reactions occurred in 0 out of 30 people; the same test was used for the powerful cleansing facial cleanser prepared in examples 5 to 6, and the results were the same as those of this time. The strong cleaning facial cleanser is safe to use.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.

Claims (10)

1. The Gemini emulsifier is characterized by having a structure shown in the following formula I:
wherein r=c n H 2n+1 ,n=12-18。
2. A method for preparing the Gemini emulsifier according to claim 1, comprising the following steps:
s1, reacting long carbon chain fatty alcohol and phosphorus oxychloride to prepare an intermediate A, wherein the structure is as follows:wherein, the structural formula of the long carbon chain fatty alcohol is as follows: ROH, r=c n H 2n+1 ,n=12-18;
S2, reacting the intermediate A with ethylene glycol to prepare an intermediate B, wherein the structure is as follows:
s3, reacting N, N, N ', N' -tetramethyl ethylenediamine with the intermediate B to obtain the Gemini emulsifier.
3. The preparation method according to claim 2, wherein the ratio of the amounts of the long carbon chain fatty alcohol and phosphorus oxychloride in the step S1 is 1:1-1.2.
4. The process according to claim 2, wherein the ratio of the amounts of the intermediate a and ethylene glycol in step S2 is 1:1 to 1.1.
5. The process according to claim 2, wherein the mass ratio of N, N' -tetramethyl ethylenediamine to intermediate B in step S3 is 1-1.1:2.
6. The preparation method according to claim 2, characterized by comprising the following steps:
s1, adding 1 molar equivalent of long carbon chain fatty alcohol and 1-1.2 molar equivalents of phosphorus oxychloride into dichloromethane, adding 3-5 molar equivalents of NaOH, carrying out reflux reaction for 1-2h, carrying out reduced pressure distillation, washing with diethyl ether, and drying to obtain an intermediate A;
s2, adding 1 molar equivalent of the intermediate A and 1-1.1 molar equivalent of ethylene glycol into dichloromethane, carrying out reflux reaction for 2-4h, carrying out reduced pressure distillation, washing with diethyl ether, and drying to obtain an intermediate B;
s3, adding 1-1.1 molar equivalent of N, N, N ', N' -tetramethyl ethylenediamine and 2 molar equivalents of intermediate B into acetonitrile, carrying out reflux reaction for 3-5h, filtering, washing, and drying with ethanol to obtain the Gemini emulsifier.
7. A high-efficiency cleansing facial cleanser comprising the Gemini emulsifier of claim 1.
8. The high-efficiency cleansing facial cleanser of claim 7, wherein the Gemini emulsifier is present in an amount of 7-12wt%.
9. The powerful cleaning facial cleanser according to claim 7, which is prepared from the following raw materials in parts by weight: the Gemini emulsifier of claim 1, wherein the Gemini emulsifier comprises 8-10 parts of a vitamin C1-2 parts of a hyaluronic acid 3-5 parts of a hyaluronic acid, 0.5-1 part of a xanthan gum, 3-5 parts of diatomite, 0.1-0.5 part of sodium citrate, 3-5 parts of glycerin, 1-2 parts of butylene glycol, 0.5-1 part of carbomer, 3-5 parts of jojoba oil, 0.5-1 part of arbutin and 70-90 parts of deionized water.
10. A method of preparing a high performance cleansing facial cleanser according to claim 9 comprising the steps of:
(1) Dissolving a Gemini emulsifier, carbomer, vitamin C, hyaluronic acid and xanthan gum in deionized water to obtain a material 1;
(2) Mixing glycerol, butanediol, jojoba oil and arbutin under stirring for 10-15min to obtain material 2;
(3) Mixing the material 1 and the material 2, adding sodium citrate and diatomite, stirring and mixing for 10-20min, emulsifying for 3-5min with 12000-15000r/min, and discharging to obtain the strong cleaning facial cleanser.
CN202310444463.6A 2023-04-23 2023-04-23 Strong-effect cleaning facial cleanser and preparation method thereof Active CN116462704B (en)

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