CN106753888A - A kind of skin-care detergent and preparation method thereof - Google Patents
A kind of skin-care detergent and preparation method thereof Download PDFInfo
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- CN106753888A CN106753888A CN201610948482.2A CN201610948482A CN106753888A CN 106753888 A CN106753888 A CN 106753888A CN 201610948482 A CN201610948482 A CN 201610948482A CN 106753888 A CN106753888 A CN 106753888A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/88—Ampholytes; Electroneutral compounds
- C11D1/94—Mixtures with anionic, cationic or non-ionic compounds
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/382—Vegetable products, e.g. soya meal, wood flour, sawdust
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/384—Animal products
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/48—Medical, disinfecting agents, disinfecting, antibacterial, germicidal or antimicrobial compositions
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/008—Polymeric surface-active agents
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/88—Ampholytes; Electroneutral compounds
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Abstract
The present invention provides a kind of skin-care detergent and preparation method thereof, and liquid detergent of the invention is free of preservative, and skin care, formula is neutral, strong detergency, can be sterilized safely, while human body skin can be protected.Krill shell enzymolysis product in the present invention,, by synergistic function, the permeability to skin is strong, can pass through cuticula and is combined with skin epithelial cell for bioactive ingredients in vinegar unstrained spirits aqueous extract, the metabolism of Skin Cell is participated in and improved, strengthens the collagen activity in skin.It can keep the integrality of cuticula moisture and fibre structure, improve Skin Cell living environment and promote the metabolism of skin histology, strengthen blood circulation, reach the purpose of skin care.Rosemary Oil is added simultaneously, and rich in natural plant composition, smell is pure and fresh, and can effectively go out peculiar smell.Inventive formulation safety non-toxic, it is easy to biodegradable, it is safer to human body and environment.
Description
Technical field
The invention belongs to articles for washing technical field, and in particular to a kind of skin-care detergent and preparation method thereof.
Background technology
With the improvement of people ' s living standards, liquid detergent has turned into essential material in daily life.It is known to wash
Clean essence, typically by the composition group such as cocoanut fatty acid diethanolamide, sodium sulfate of polyethenoxy ether of fatty alcohol, alkyl benzene sulphonate
With forming, the liquid detergent combined by these compositions has a preferable dirt-removing power, but its most product can stimulate when using
Skin, commonly using skin can be made to come to harm, makes dry and astringent, coarse skin, cracking, decortication etc..
Current people often after liquid detergent has been used, hand are rinsed well and skin care is coated immediately to protect the both hands of itself
Frost, to make up the loss of skin surface grease, anti-skin peeling, corrugation and premature aging in time.Or it is straight by band left-hand seat
Set, prevents liquid detergent from directly being contacted with skin.
But it is clear that the way of the above fails fundamentally to solve the problems, such as presently, there are, because, even if in time in both hands
Coating face cream can prevent skin peeling, corrugation and premature aging, can not ensure that skin is not subject to when using next time
Injury, in other words, when this kind of liquid detergent is used next time, liquid detergent can directly wash away the face cream of both hands, and again
It is secondary that skin is damaged.Therefore, necessary improvement can only be done from the chemical composition of liquid detergent, could effectively solves to wash clean at present
The problem that essence is present.
The content of the invention
In view of this, the present invention provides a kind of skin-care detergent and preparation method thereof, and liquid detergent of the invention is free of anti-corrosion
Agent, formula is neutral, and dirt-removing power is strong, can be sterilized safely, while human body skin can be protected.
The technical scheme is that：A kind of skin-care detergent, by following parts by weight into being grouped into：Shitosan both sexes
High molecular surfactant 44-62 parts, 33-47 parts of soluble polyurethane type surfactant, deionized water 12-23 parts, fan
Repeatedly essential oil 2-5 parts, 3-7 parts of krill shell enzymolysis product, 14-27 parts of vinegar unstrained spirits aqueous extract.
Further, described skin-care detergent, by following parts by weight into being grouped into：Shitosan Amphiphatic high polymer table
51-58 parts of face activating agent, 37-43 parts of soluble polyurethane type surfactant, deionized water 17-21 parts, Rosemary Oil
3-4 parts, 4-5 parts of krill shell enzymolysis product, 18-25 parts of vinegar unstrained spirits aqueous extract.
Further, the molecular formula of the shitosan amphoteric polymeric surfactant is,
Wherein n=6-18.
Further, the preparation method of the soluble polyurethane type surfactant is：S1, weighs two isocyanides of equivalent
Acid esters, maleic anhydride and polyethylene glycol, its mass ratio are 3：8：5；S2, takes polyethylene glycol that S1 weighs and suitable in flask
The dibutyl tin laurate of amount, stirs；S3, maleic anhydride is added in proper amount of acetone solution, is stirred；S4,
The solution for adding the 3rd step to be formed in the solid formed to second step under the stirring, after flask is placed on 65 DEG C of condition
Lower reaction；S5, after four hours, stirs and adds diisocyanate solution to react simultaneously under conditions of having nitrogen to protect；S6,
Again after four hours, appropriate trimethylolpropane is added in flask, close beaker bottleneck；S7, then by after four hours,
Sealed up for safekeeping to suitable quantity of water is added in flask；S8, taking precipitate is clean in 45 DEG C of acetone soln after two weeks, is drying to obtain water
Soluble polyurethane surfactant.
Further, the preparation method of the krill shell enzymolysis product is：Krill shell is size-reduced, sieve and go
After the pretreatment such as miscellaneous, with solid-liquid ratio 1: 5（m/V）Add water, soaked overnight, using trypsase and papain mixed enzymolysis
Mode, enzymatic hydrolysis condition is：45 DEG C of temperature, pH 7.5, the .5h of hydrolysis time 2, trypsase and papain it is enzyme-added
Amount is respectively 1500 U/g and 1300U/g；The enzyme that gone out after terminating is digested, 5000r/min is centrifuged 10min at 4 DEG C by enzymolysis liquid, takes
Supernatant, then obtain krill shell enzymolysis product by micro-filtration.
Further, the preparation method of the vinegar unstrained spirits aqueous extract is：The vinegar unstrained spirits after acetic fermentation is taken, by 1:6 material
Liquor ratio（g:mL）Distilled water is added, is filtered to get filtrate after the h of mechanical shaking extraction 3 at room temperature, filtrate is aseptic by 0.22 μm again
Membrane filtration is degerming, obtains vinegar unstrained spirits aqueous extract.
A kind of preparation method of skin-care detergent, including step in detail below：By in deionized water addition reactor, heat
To 70 DEG C, soluble polyurethane type surfactant, shitosan amphoteric polymeric surfactant are sequentially added by weight
After stirring, temperature is down to 40 DEG C, and the PH values of solution are adjusted into 7.1, adds Rosemary Oil, krill shell enzymolysis to produce
Thing, vinegar unstrained spirits aqueous extract is stirred until homogeneous, and the feed liquid that will be stirred is de-gassed, using vacuum outgas, vacuum cavitations in 5Mpa,
Mixed liquor is dispensed, you can obtain skin-care detergent.
The present invention is using shitosan amphoteric polymeric surfactant and soluble polyurethane type surfactant compound
Into liquid detergent, with good hydrophily and lipophile, the viscosity of soluble polyurethane type surfactant is not because of rotating speed
Change and change, but can increase with the increase of concentration, be typical newtonian liquid, with good decontamination, emulsification,
Wetting and foam performance, small to skin and eye irritation, stabilization, enhances the mildness of formula system in hard water.Shell gathers
Sugared amphoteric polymeric surfactant with shitosan as primary raw material, with good wetting, emulsifiability and stronger decontamination
Ability, to acid, alkali and hard water stabilization.
The present invention provide skin-care detergent with the market the overwhelming majority liquid detergent differences be, no added preservative, with
Rosemary Oil, krill shell enzymolysis product, vinegar unstrained spirits aqueous extract as main sterilization component, by the collaboration of each component
Synergistic effect, mainly acts on pathogenic bacteria in terms of two：1. act on the cell membrane and cell film system of pathogenic bacteria, directly and
It is saturating that the selectivity to material for depending on the energetic supersession of membrane structure integrality and cell and organelle to depend on for existence is destroyed rapidly
Property, nutriment and metabolite microorganism cannot be made to lose nutrition and its growth retardation is caused normally through cell membrane, reach
To the purpose of restraining and sterilizing bacteria；2. after cell membrane is destroyed, the active material of small molecule enter into cell membrane with it is intracellular
Polar substances are combined, and protein is synthesized, and DNA cannot be replicated, so as to change inhereditary material or genic synthesis
The activity of enzyme or functional protein in influence microbial body, suppresses its growth.3., by suppressing the respiration of pathogenic bacteria, make
Metabolic activity is obstructed, it is impossible to maintains normal dynamic membrane structure, causes the self-dissolving of cell.By containing in the active component in invention
The groups such as the abundant hydroxyl having, easily form hydrogen bond with active site in alcohol, and then cause metabolic system disorderly, and then reach
Sterilized effect.
Krill shell enzymolysis product in the present invention, the bioactive ingredients in vinegar unstrained spirits aqueous extract are made by Synergistic
With, the permeability to skin is strong, can pass through cuticula and is combined with skin epithelial cell, participates in and improve the metabolism of Skin Cell,
Strengthen the collagen activity in skin.It can keep the integrality of cuticula moisture and fibre structure, improve Skin Cell
The metabolism of living environment and promotion skin histology, strengthens blood circulation, reaches the purpose of skin care.Meanwhile, biology is living
Property composition can directly penetrate into skin bottom, and good with the compatibility of surrounding tissue, can helper cell be manufactured into collagen, promote
Skin Cell normal growth, reaches the effect moistened and repair skin.Rosemary Oil is added simultaneously, rich in natural plant composition,
Smell is pure and fresh, and can effectively go out peculiar smell.Inventive formulation safety non-toxic, it is easy to biodegradable, it is safer to human body and environment.
Specific embodiment
Technical scheme is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that retouched
The embodiment stated is only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this
The every other embodiment that field those of ordinary skill is obtained under the premise of creative work is not made, belongs to the present invention
The scope of protection.
Embodiment 1
A kind of skin-care detergent, by following parts by weight into being grouped into：54 parts of shitosan amphoteric polymeric surfactant, water
39 parts of soluble polyurethane type surfactant, 19 parts of deionized water, 3 parts of Rosemary Oil, krill shell enzymolysis product 5
Part, 21 parts of vinegar unstrained spirits aqueous extract.
Further, the molecular formula of the shitosan amphoteric polymeric surfactant is,
Wherein n=12.
Further, the shitosan amphoteric polymeric surfactant is with natural chitosan as raw material, with long-chain fat
Fat aldehyde, 3- chlorine-2-hydroxyls propane sulfonic acid are used as a kind of synthetically prepared water-soluble high score based on shitosan for obtaining of alkylating reagent
Sub- surfactant.
Further, the preparation method of the soluble polyurethane type surfactant is：S1, weighs two isocyanides of equivalent
Acid esters, maleic anhydride and polyethylene glycol, its mass ratio are 3：8：5；S2, takes polyethylene glycol that S1 weighs and suitable in flask
The dibutyl tin laurate of amount, stirs；S3, maleic anhydride is added in proper amount of acetone solution, is stirred；S4,
The solution for adding the 3rd step to be formed in the solid formed to second step under the stirring, after flask is placed on 65 DEG C of condition
Lower reaction；S5, after four hours, stirs and adds diisocyanate solution to react simultaneously under conditions of having nitrogen to protect；S6,
Again after four hours, appropriate trimethylolpropane is added in flask, close beaker bottleneck；S7, then by after four hours,
Sealed up for safekeeping to suitable quantity of water is added in flask；S8, taking precipitate is clean in 45 DEG C of acetone soln after two weeks, is drying to obtain water
Soluble polyurethane surfactant.
Further, the preparation method of the vinegar unstrained spirits aqueous extract is：It is solid-liquid ratio 1: 10 to impose a condition（m/V）, fiber
Plain enzyme Cellulase ACCF-4740 additions 2%, 55 DEG C of temperature, pH 4.5, the h of reaction time 1.3.Cellulose hydrolyzation
After end, boiling water bath is gone out enzyme 15 min, and 9000 r/min centrifugations are collected supernatant and obtain splitting kettle algae cellulose hydrolyzation liquid.Split
Kettle algae enzymolysis liquid goes out after enzyme activity, regulation pH value to 6.2-6.6, high pressure steam sterilization（121 DEG C, 20 min）, then it is inoculated with volume
The Pediococcus pentosaceus liquid of the MRS culture mediums activation of fraction 1% stands, is sent out to kettle algae enzymolysis liquid, 37 DEG C of constant incubators are split
Ferment.After fermentation ends, supernatant freeze-drying is collected in high pressure steam sterilization, 9000 r/min centrifugations, obtains the extraction of vinegar unstrained spirits water
Liquid, saves backup under the conditions of -20 DEG C.
Embodiment 2
A kind of skin-care detergent, by following parts by weight into being grouped into：53 parts of shitosan amphoteric polymeric surfactant,
38 parts of soluble polyurethane type surfactant, 18 parts of deionized water, 4 parts of Rosemary Oil, krill shell enzymolysis product 4
Part, 18 parts of vinegar unstrained spirits aqueous extract.
Further, the molecular formula of the shitosan amphoteric polymeric surfactant is,
Wherein n=10.
Further, the preparation method of the soluble polyurethane type surfactant is：S1, weighs two isocyanides of equivalent
Acid esters, maleic anhydride and polyethylene glycol, its mass ratio are 3：8：5；S2, takes polyethylene glycol that S1 weighs and suitable in flask
The dibutyl tin laurate of amount, stirs；S3, maleic anhydride is added in proper amount of acetone solution, is stirred；S4,
The solution for adding the 3rd step to be formed in the solid formed to second step under the stirring, after flask is placed on 65 DEG C of condition
Lower reaction；S5, after four hours, stirs and adds diisocyanate solution to react simultaneously under conditions of having nitrogen to protect；S6,
Again after four hours, appropriate trimethylolpropane is added in flask, close beaker bottleneck；S7, then by after four hours,
Sealed up for safekeeping to suitable quantity of water is added in flask；S8, taking precipitate is clean in 45 DEG C of acetone soln after two weeks, is drying to obtain water
Soluble polyurethane surfactant.
Further, the preparation method of the krill shell enzymolysis product is：Krill shell is size-reduced, sieve and go
After the pretreatment such as miscellaneous, with solid-liquid ratio 1: 5（m/V）Add water, soaked overnight, using trypsase and papain mixed enzymolysis
Mode, enzymatic hydrolysis condition is：45 DEG C of temperature, pH 7.5, the .5h of hydrolysis time 2, trypsase and papain it is enzyme-added
Amount is respectively 1500 U/g and 1300U/g；The enzyme that gone out after terminating is digested, 5000r/min is centrifuged 10min at 4 DEG C by enzymolysis liquid, takes
Supernatant, then obtain krill shell enzymolysis product by micro-filtration.
Further, the preparation method of the vinegar unstrained spirits aqueous extract is：The vinegar unstrained spirits after acetic fermentation is taken, by 1:6 material
Liquor ratio（g:mL）Distilled water is added, is filtered to get filtrate after the h of mechanical shaking extraction 3 at room temperature, filtrate is aseptic by 0.22 μm again
Membrane filtration is degerming, obtains vinegar unstrained spirits aqueous extract.
A kind of preparation method of skin-care detergent, including step in detail below：By in deionized water addition reactor, heat
To 70 DEG C, soluble polyurethane type surfactant, shitosan amphoteric polymeric surfactant are sequentially added by weight
After stirring, temperature is down to 40 DEG C, and the PH values of solution are adjusted into 7.1, adds Rosemary Oil, krill shell enzymolysis to produce
Thing, vinegar unstrained spirits aqueous extract is stirred until homogeneous, and the feed liquid that will be stirred is de-gassed, using vacuum outgas, vacuum cavitations in 5Mpa,
Mixed liquor is dispensed, you can obtain skin-care detergent.
Embodiment 3
A kind of skin-care detergent, by following parts by weight into being grouped into：55 parts of shitosan amphoteric polymeric surfactant,
40 parts of soluble polyurethane type surfactant, 29 parts of deionized water, 4 parts of Rosemary Oil, krill shell enzymolysis product 5
Part, 25 parts of vinegar unstrained spirits aqueous extract.
Further, the molecular formula of the shitosan amphoteric polymeric surfactant is,
Wherein n=14.
Further, the preparation method of the soluble polyurethane type surfactant is：S1, weighs two isocyanides of equivalent
Acid esters, maleic anhydride and polyethylene glycol, its mass ratio are 3：8：5；S2, takes polyethylene glycol that S1 weighs and suitable in flask
The dibutyl tin laurate of amount, stirs；S3, maleic anhydride is added in proper amount of acetone solution, is stirred；S4,
The solution for adding the 3rd step to be formed in the solid formed to second step under the stirring, after flask is placed on 65 DEG C of condition
Lower reaction；S5, after four hours, stirs and adds diisocyanate solution to react simultaneously under conditions of having nitrogen to protect；S6,
Again after four hours, appropriate trimethylolpropane is added in flask, close beaker bottleneck；S7, then by after four hours,
Sealed up for safekeeping to suitable quantity of water is added in flask；S8, taking precipitate is clean in 45 DEG C of acetone soln after two weeks, is drying to obtain water
Soluble polyurethane surfactant.
Further, the preparation method of the krill shell enzymolysis product is：Krill shell is size-reduced, sieve and go
After the pretreatment such as miscellaneous, with solid-liquid ratio 1: 5（m/V）Add water, soaked overnight, using trypsase and papain mixed enzymolysis
Mode, enzymatic hydrolysis condition is：45 DEG C of temperature, pH 7.5, the .5h of hydrolysis time 2, trypsase and papain it is enzyme-added
Amount is respectively 1500 U/g and 1300U/g；The enzyme that gone out after terminating is digested, 5000r/min is centrifuged 10min at 4 DEG C by enzymolysis liquid, takes
Supernatant, then obtain krill shell enzymolysis product by micro-filtration.
Further, the preparation method of the vinegar unstrained spirits aqueous extract is：The vinegar unstrained spirits after acetic fermentation is taken, by 1:6 material
Liquor ratio（g:mL）Distilled water is added, is filtered to get filtrate after the h of mechanical shaking extraction 3 at room temperature, filtrate is aseptic by 0.22 μm again
Membrane filtration is degerming, obtains vinegar unstrained spirits aqueous extract.
A kind of preparation method of skin-care detergent, including step in detail below：By in deionized water addition reactor, heat
To 70 DEG C, soluble polyurethane type surfactant, shitosan amphoteric polymeric surfactant are sequentially added by weight
After stirring, temperature is down to 40 DEG C, and the PH values of solution are adjusted into 7.1, adds Rosemary Oil, krill shell enzymolysis to produce
Thing, vinegar unstrained spirits aqueous extract is stirred until homogeneous, and the feed liquid that will be stirred is de-gassed, using vacuum outgas, vacuum cavitations in 5Mpa,
Mixed liquor is dispensed, you can obtain skin-care detergent.
Embodiment 4
A kind of skin-care detergent, by following parts by weight into being grouped into：51 parts of shitosan amphoteric polymeric surfactant,
37 parts of soluble polyurethane type surfactant, 17 parts of deionized water, 3 parts of Rosemary Oil, krill shell enzymolysis product 4
Part, 20 parts of vinegar unstrained spirits aqueous extract.
Further, the molecular formula of the shitosan amphoteric polymeric surfactant is,
Wherein n=8.
Further, the preparation method of the soluble polyurethane type surfactant is：S1, weighs two isocyanides of equivalent
Acid esters, maleic anhydride and polyethylene glycol, its mass ratio are 3：8：5；S2, takes polyethylene glycol that S1 weighs and suitable in flask
The dibutyl tin laurate of amount, stirs；S3, maleic anhydride is added in proper amount of acetone solution, is stirred；S4,
The solution for adding the 3rd step to be formed in the solid formed to second step under the stirring, after flask is placed on 65 DEG C of condition
Lower reaction；S5, after four hours, stirs and adds diisocyanate solution to react simultaneously under conditions of having nitrogen to protect；S6,
Again after four hours, appropriate trimethylolpropane is added in flask, close beaker bottleneck；S7, then by after four hours,
Sealed up for safekeeping to suitable quantity of water is added in flask；S8, taking precipitate is clean in 45 DEG C of acetone soln after two weeks, is drying to obtain water
Soluble polyurethane surfactant.
Further, the preparation method of the krill shell enzymolysis product is：Krill shell is size-reduced, sieve and go
After the pretreatment such as miscellaneous, with solid-liquid ratio 1: 5（m/V）Add water, soaked overnight, using trypsase and papain mixed enzymolysis
Mode, enzymatic hydrolysis condition is：45 DEG C of temperature, pH 7.5, the .5h of hydrolysis time 2, trypsase and papain it is enzyme-added
Amount is respectively 1500 U/g and 1300U/g；The enzyme that gone out after terminating is digested, 5000r/min is centrifuged 10min at 4 DEG C by enzymolysis liquid, takes
Supernatant, then obtain krill shell enzymolysis product by micro-filtration.
Further, the preparation method of the vinegar unstrained spirits aqueous extract is：The vinegar unstrained spirits after acetic fermentation is taken, by 1:6 material
Liquor ratio（g:mL）Distilled water is added, is filtered to get filtrate after the h of mechanical shaking extraction 3 at room temperature, filtrate is aseptic by 0.22 μm again
Membrane filtration is degerming, obtains vinegar unstrained spirits aqueous extract.
A kind of preparation method of skin-care detergent, including step in detail below：By in deionized water addition reactor, heat
To 70 DEG C, soluble polyurethane type surfactant, shitosan amphoteric polymeric surfactant are sequentially added by weight
After stirring, temperature is down to 40 DEG C, and the PH values of solution are adjusted into 7.1, adds Rosemary Oil, krill shell enzymolysis to produce
Thing, vinegar unstrained spirits aqueous extract is stirred until homogeneous, and the feed liquid that will be stirred is de-gassed, using vacuum outgas, vacuum cavitations in 5Mpa,
Mixed liquor is dispensed, you can obtain skin-care detergent.
Embodiment 5
A kind of skin-care detergent, by following parts by weight into being grouped into：58 parts of shitosan amphoteric polymeric surfactant, water
43 parts of soluble polyurethane type surfactant, 21 parts of deionized water, 4 parts of Rosemary Oil, 5 parts of krill shell enzymolysis product,
23 parts of vinegar unstrained spirits aqueous extract.
Further, the molecular formula of the shitosan amphoteric polymeric surfactant is,
Wherein n=16.
Further, the preparation method of the soluble polyurethane type surfactant is：S1, weighs two isocyanides of equivalent
Acid esters, maleic anhydride and polyethylene glycol, its mass ratio are 3：8：5；S2, takes polyethylene glycol that S1 weighs and suitable in flask
The dibutyl tin laurate of amount, stirs；S3, maleic anhydride is added in proper amount of acetone solution, is stirred；S4,
The solution for adding the 3rd step to be formed in the solid formed to second step under the stirring, after flask is placed on 65 DEG C of condition
Lower reaction；S5, after four hours, stirs and adds diisocyanate solution to react simultaneously under conditions of having nitrogen to protect；S6,
Again after four hours, appropriate trimethylolpropane is added in flask, close beaker bottleneck；S7, then by after four hours,
Sealed up for safekeeping to suitable quantity of water is added in flask；S8, taking precipitate is clean in 45 DEG C of acetone soln after two weeks, is drying to obtain water
Soluble polyurethane surfactant.
Further, the preparation method of the krill shell enzymolysis product is：Krill shell is size-reduced, sieve and go
After the pretreatment such as miscellaneous, with solid-liquid ratio 1: 5（m/V）Add water, soaked overnight, using trypsase and papain mixed enzymolysis
Mode, enzymatic hydrolysis condition is：45 DEG C of temperature, pH 7.5, the .5h of hydrolysis time 2, trypsase and papain it is enzyme-added
Amount is respectively 1500 U/g and 1300U/g；The enzyme that gone out after terminating is digested, 5000r/min is centrifuged 10min at 4 DEG C by enzymolysis liquid, takes
Supernatant, then obtain krill shell enzymolysis product by micro-filtration.
Further, the preparation method of the vinegar unstrained spirits aqueous extract is：The vinegar unstrained spirits after acetic fermentation is taken, by 1:6 material
Liquor ratio（g:mL）Distilled water is added, is filtered to get filtrate after the h of mechanical shaking extraction 3 at room temperature, filtrate is aseptic by 0.22 μm again
Membrane filtration is degerming, obtains vinegar unstrained spirits aqueous extract.
A kind of preparation method of skin-care detergent, including step in detail below：By in deionized water addition reactor, heat
To 70 DEG C, soluble polyurethane type surfactant, shitosan amphoteric polymeric surfactant are sequentially added by weight
After stirring, temperature is down to 40 DEG C, and the PH values of solution are adjusted into 7.1, adds Rosemary Oil, krill shell enzymolysis to produce
Thing, vinegar unstrained spirits aqueous extract is stirred until homogeneous, and the feed liquid that will be stirred is de-gassed, using vacuum outgas, vacuum cavitations in 5Mpa,
Mixed liquor is dispensed, you can obtain skin-care detergent.
Comparative example 1
A kind of skin-care detergent, by following parts by weight into being grouped into：39 parts of soluble polyurethane type surfactant, goes
19 parts of ionized water, 3 parts of Rosemary Oil, 5 parts of krill shell enzymolysis product, 21 parts of vinegar unstrained spirits aqueous extract.
Further, the preparation method of the soluble polyurethane type surfactant is：S1, weighs two isocyanides of equivalent
Acid esters, maleic anhydride and polyethylene glycol, its mass ratio are 3：8：5；S2, takes polyethylene glycol that S1 weighs and suitable in flask
The dibutyl tin laurate of amount, stirs；S3, maleic anhydride is added in proper amount of acetone solution, is stirred；S4,
The solution for adding the 3rd step to be formed in the solid formed to second step under the stirring, after flask is placed on 65 DEG C of condition
Lower reaction；S5, after four hours, stirs and adds diisocyanate solution to react simultaneously under conditions of having nitrogen to protect；S6,
Again after four hours, appropriate trimethylolpropane is added in flask, close beaker bottleneck；S7, then by after four hours,
Sealed up for safekeeping to suitable quantity of water is added in flask；S8, taking precipitate is clean in 45 DEG C of acetone soln after two weeks, is drying to obtain water
Soluble polyurethane surfactant.
Further, the preparation method of the krill shell enzymolysis product is：Krill shell is size-reduced, sieve and go
After the pretreatment such as miscellaneous, with solid-liquid ratio 1: 5（m/V）Add water, soaked overnight, using trypsase and papain mixed enzymolysis
Mode, enzymatic hydrolysis condition is：45 DEG C of temperature, pH 7.5, the .5h of hydrolysis time 2, trypsase and papain it is enzyme-added
Amount is respectively 1500 U/g and 1300U/g；The enzyme that gone out after terminating is digested, 5000r/min is centrifuged 10min at 4 DEG C by enzymolysis liquid, takes
Supernatant, then obtain krill shell enzymolysis product by micro-filtration.
Further, the preparation method of the vinegar unstrained spirits aqueous extract is：The vinegar unstrained spirits after acetic fermentation is taken, by 1:6 material
Liquor ratio（g:mL）Distilled water is added, is filtered to get filtrate after the h of mechanical shaking extraction 3 at room temperature, filtrate is aseptic by 0.22 μm again
Membrane filtration is degerming, obtains vinegar unstrained spirits aqueous extract.
A kind of preparation method of skin-care detergent, including step in detail below：By in deionized water addition reactor, heat
To 70 DEG C, after adding soluble polyurethane type surfactant to stir by weight, temperature is down to 40 DEG C, by solution
PH values are adjusted to 7.1, add Rosemary Oil, krill shell enzymolysis product, vinegar unstrained spirits aqueous extract to be stirred until homogeneous, will stir
Good feed liquid is de-gassed, and using vacuum outgas, vacuum cavitations are dispensed in 5Mpa to mixed liquor, you can obtained skin care and washed
Clean essence.
Comparative example 2
A kind of skin-care detergent, by following parts by weight into being grouped into：54 parts of shitosan amphoteric polymeric surfactant, goes
19 parts of ionized water, 3 parts of Rosemary Oil, 5 parts of krill shell enzymolysis product, 21 parts of vinegar unstrained spirits aqueous extract.
Further, the molecular formula of the shitosan amphoteric polymeric surfactant is,
Wherein n=12.
Further, the preparation method of the krill shell enzymolysis product is：Krill shell is size-reduced, sieve and go
After the pretreatment such as miscellaneous, with solid-liquid ratio 1: 5（m/V）Add water, soaked overnight, using trypsase and papain mixed enzymolysis
Mode, enzymatic hydrolysis condition is：45 DEG C of temperature, pH 7.5, the .5h of hydrolysis time 2, trypsase and papain it is enzyme-added
Amount is respectively 1500 U/g and 1300U/g；The enzyme that gone out after terminating is digested, 5000r/min is centrifuged 10min at 4 DEG C by enzymolysis liquid, takes
Supernatant, then obtain krill shell enzymolysis product by micro-filtration.
Further, the preparation method of the vinegar unstrained spirits aqueous extract is：The vinegar unstrained spirits after acetic fermentation is taken, by 1:6 material
Liquor ratio（g:mL）Distilled water is added, is filtered to get filtrate after the h of mechanical shaking extraction 3 at room temperature, filtrate is aseptic by 0.22 μm again
Membrane filtration is degerming, obtains vinegar unstrained spirits aqueous extract.
A kind of preparation method of skin-care detergent, including step in detail below：By in deionized water addition reactor, heat
To 70 DEG C, after adding shitosan amphoteric polymeric surfactant to stir by weight, temperature is down to 40 DEG C, by solution
PH values be adjusted to 7.1, add Rosemary Oil, krill shell enzymolysis product, vinegar unstrained spirits aqueous extract to be stirred until homogeneous, will stir
The feed liquid mixed is de-gassed, and using vacuum outgas, vacuum cavitations are dispensed in 5Mpa to mixed liquor, you can obtain skin care
Liquid detergent.
Comparative example 3
A kind of skin-care detergent, by following parts by weight into being grouped into：54 parts of shitosan amphoteric polymeric surfactant, water
39 parts of soluble polyurethane type surfactant, 19 parts of deionized water, 3 parts of Rosemary Oil, krill shell enzymolysis product 5
Part.
Further, the molecular formula of the shitosan amphoteric polymeric surfactant is,
Wherein n=12.
Further, the preparation method of the soluble polyurethane type surfactant is：S1, weighs two isocyanides of equivalent
Acid esters, maleic anhydride and polyethylene glycol, its mass ratio are 3：8：5；S2, takes polyethylene glycol that S1 weighs and suitable in flask
The dibutyl tin laurate of amount, stirs；S3, maleic anhydride is added in proper amount of acetone solution, is stirred；S4,
The solution for adding the 3rd step to be formed in the solid formed to second step under the stirring, after flask is placed on 65 DEG C of condition
Lower reaction；S5, after four hours, stirs and adds diisocyanate solution to react simultaneously under conditions of having nitrogen to protect；S6,
Again after four hours, appropriate trimethylolpropane is added in flask, close beaker bottleneck；S7, then by after four hours,
Sealed up for safekeeping to suitable quantity of water is added in flask；S8, taking precipitate is clean in 45 DEG C of acetone soln after two weeks, is drying to obtain water
Soluble polyurethane surfactant.
Further, the preparation method of the krill shell enzymolysis product is：Krill shell is size-reduced, sieve and go
After the pretreatment such as miscellaneous, with solid-liquid ratio 1: 5（m/V）Add water, soaked overnight, using trypsase and papain mixed enzymolysis
Mode, enzymatic hydrolysis condition is：45 DEG C of temperature, pH 7.5, the .5h of hydrolysis time 2, trypsase and papain it is enzyme-added
Amount is respectively 1500 U/g and 1300U/g；The enzyme that gone out after terminating is digested, 5000r/min is centrifuged 10min at 4 DEG C by enzymolysis liquid, takes
Supernatant, then obtain krill shell enzymolysis product by micro-filtration.
A kind of preparation method of skin-care detergent, including step in detail below：By in deionized water addition reactor, heat
To 70 DEG C, soluble polyurethane type surfactant, shitosan amphoteric polymeric surfactant are sequentially added by weight
After stirring, temperature is down to 40 DEG C, and the PH values of solution are adjusted into 7.1, adds Rosemary Oil, krill shell enzymolysis to produce
Thing is stirred until homogeneous, and the feed liquid that will be stirred is de-gassed, and using vacuum outgas, vacuum cavitations are carried out in 5Mpa to mixed liquor
Packing, you can obtain skin-care detergent.
Comparative example 4
A kind of skin-care detergent, by following parts by weight into being grouped into：54 parts of shitosan amphoteric polymeric surfactant, water
39 parts of soluble polyurethane type surfactant, 19 parts of deionized water, 3 parts of Rosemary Oil, 21 parts of vinegar unstrained spirits aqueous extract.
Further, the molecular formula of the shitosan amphoteric polymeric surfactant is,
Wherein n=12.
Further, the preparation method of the soluble polyurethane type surfactant is：S1, weighs two isocyanides of equivalent
Acid esters, maleic anhydride and polyethylene glycol, its mass ratio are 3：8：5；S2, takes polyethylene glycol that S1 weighs and suitable in flask
The dibutyl tin laurate of amount, stirs；S3, maleic anhydride is added in proper amount of acetone solution, is stirred；S4,
The solution for adding the 3rd step to be formed in the solid formed to second step under the stirring, after flask is placed on 65 DEG C of condition
Lower reaction；S5, after four hours, stirs and adds diisocyanate solution to react simultaneously under conditions of having nitrogen to protect；S6,
Again after four hours, appropriate trimethylolpropane is added in flask, close beaker bottleneck；S7, then by after four hours,
Sealed up for safekeeping to suitable quantity of water is added in flask；S8, taking precipitate is clean in 45 DEG C of acetone soln after two weeks, is drying to obtain water
Soluble polyurethane surfactant.
Further, the preparation method of the vinegar unstrained spirits aqueous extract is：The vinegar unstrained spirits after acetic fermentation is taken, by 1:6 material
Liquor ratio（g:mL）Distilled water is added, is filtered to get filtrate after the h of mechanical shaking extraction 3 at room temperature, filtrate is aseptic by 0.22 μm again
Membrane filtration is degerming, obtains vinegar unstrained spirits aqueous extract.
A kind of preparation method of skin-care detergent, including step in detail below：By in deionized water addition reactor, heat
To 70 DEG C, soluble polyurethane type surfactant, shitosan amphoteric polymeric surfactant are sequentially added by weight
After stirring, temperature is down to 40 DEG C, and the PH values of solution are adjusted into 7.1, adds Rosemary Oil, the stirring of vinegar unstrained spirits aqueous extract
To uniform, the feed liquid that will be stirred is de-gassed, and using vacuum outgas, vacuum cavitations are dispensed in 5Mpa to mixed liquor, i.e.,
Can obtain skin-care detergent.
Comparative example 5
Receive the full effect enriching liquid detergent of good Mrs's brand of Li Xinxihua Co., Ltds production from Hebei, bucket limit makes the date be
20180523, as a comparison case 5.
Comparative example 6
From the lemon aloe liquid detergent of labourer's personal style and attitude board of Guangzhou Nanshun Cleaning Products Co., Ltd.'s production, bucket limit makes the date be
20180803A, as a comparison case 6.
Experimental test
1. bactericidal effect test
Using Suspension quantitative bactericidal test, the Escherichia coli after activation, salmonella, Candida albicans are taken first and is seeded to triangle
In shaking flask, 37 DEG C, the 160 r/h of min shaken cultivations 36.Then respectively inoculation 1ml above-mentioned bacteria suspensions respectively with 9
The 2% dilution mixing of the liquid detergent of ml embodiments 1-5 and comparative example 1-6,37 DEG C, 160 r/min vibration 30min,
With dilution the method for falling ware measure detergent to Escherichia coli, salmonella, Candida albicans killing logarithm value, it is parallel in triplicate
Experiment, calculates bactericidal effect such as following table.
2. detergency experiment
Press《Manual dishwashing detergent》The method of the standards of GB 9985-2000 purchase artificial dirt, 250 ppm hard water,
Instrument needed for dirt ceramics plate and foam level method test detergency.Using foam end point method, respectively Example 1-5 with
And comparative example 1-6 liquid detergent 5mL, by 1000mL concentration for the hard water of 250ppm is poured into enamel basin, separately by 1000mL concentration
For the hard water of 250ppm is put into tubualted bottle.In room temperature（25 ℃）Under, the delivery port of tubualted bottle is opened, hard water is rushed in flowing into basin
Spume.After hard water stops flowing out（The s of process about 45）, plate is scrubbed with 102 mm pigs palm fibre paintbrush, first brush clockwise
5 times, another mistake hour hands brush 5 times, after so repeating 1 time, the dirt major part being applied on plate is washed down, finally again will not
Wash lower part to scrub off, until foam is wholly absent, record the number that washes dishes, and be finally converted into deep bid subnumber, it is as a result as follows
Shown in table.
3. irritation test
Simulation irritant experiment is carried out in laboratory, respectively Example 1-5 and comparative example 1-6 liquid detergent 1mL, will
1000mL running water is poured into enamel basin, and liquid detergent is fully dissolved in water, 25 ± 2 DEG C of water temperature, water used for it is conventional originally
Water, experimenter（Each 5 people of men and women）Washed in liquid detergent aqueous wash medium, daily washing 2 times, every time 3 hours, continuous 1 week.It is right
Averaged again after the excitant of wrist-watch skin is scored according to the standard of following table, scored higher, excitant is smaller.
Excitant test result is as shown in the table.
4. security toxicological test.
The main formula of Example 1 carries out toxicological test, foundation respectively《Foodsafety Toxicological Assessment program and side
Method》GB 15193-2003, using maximum tolerance metering experiment method, dosage is set to 10000 mg/kg BW, from 20
Kunming mice, male and female half and half.The h of animal fasting 16, drinking-water is not limited before experiment.The mg/mL of animal 500 is given using administration by gavage
The sample solution of concentration, gavage amount is 0.4 mL/20 g body weight.The poisoning manifestations and death condition of animal are observed after gavage,
Weigh weekly 1 time, observe 14 d, it is as a result as shown in the table.
| Sample ID | Shitosan amphoteric polymeric surfactant | Soluble polyurethane type surfactant | Vinegar unstrained spirits aqueous extract | Krill shell enzymolysis product |
| LD50（mg/kg·BW） | 20000 | 15000 | 50000 | 35000 |
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and do not carrying on the back
In the case of spirit or essential attributes of the invention, the present invention can be in other specific forms realized.Therefore, no matter from which
From the point of view of a bit, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention will by appended right
Ask and limited rather than described above, it is intended that all changes that will fall in the implication and scope of the equivalency of claim
Include in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each implementation method is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that for clarity, those skilled in the art should
Specification an as entirety, the technical scheme in each embodiment can also be formed into those skilled in the art through appropriately combined
May be appreciated other embodiment.The ins and outs not described in detail in the present invention, can be by any in this area
Prior art is realized.Particularly, all technical characterstics not described in detail can be realized by any prior art in the present invention.
Claims (7)
1. a kind of skin-care detergent, it is characterised in that by following parts by weight into being grouped into：Shitosan Amphiphatic high polymer surface
Activating agent 44-62 parts, 33-47 parts of soluble polyurethane type surfactant, deionized water 12-23 parts, Rosemary Oil
2-5 parts, 3-7 parts of krill shell enzymolysis product, 14-27 parts of vinegar unstrained spirits aqueous extract.
2. skin-care detergent according to claim 1, it is characterised in that by following parts by weight into being grouped into：Shell gathers
Sugared amphoteric polymeric surfactant 51-58 parts, 37-43 parts of soluble polyurethane type surfactant, deionized water 17-
21 parts, Rosemary Oil 3-4 parts, 4-5 parts of krill shell enzymolysis product, 18-25 parts of vinegar unstrained spirits aqueous extract.
3. skin-care detergent according to claim 1, it is characterised in that the shitosan amphoteric polymeric surfactant
Molecular formula be, wherein n=6-18.
4. skin-care detergent according to claim 1, it is characterised in that the soluble polyurethane type surfactant
Preparation method is：S1, weighs diisocyanate, maleic anhydride and the polyethylene glycol of equivalent, and its mass ratio is 3：8：5；S2,
Polyethylene glycol and appropriate dibutyl tin laurate that S1 is weighed are taken in flask, is stirred；S3, it is molten in proper amount of acetone
Maleic anhydride is added in liquid, is stirred；S4, adds the 3rd step to be formed in the solid formed to second step under stirring
Solution, after flask is placed on 65 DEG C under conditions of react；S5, after four hours, under conditions of thering is nitrogen to protect simultaneously
Stirring adds diisocyanate solution reaction；After S6, then four hours, appropriate trimethylolpropane is added in flask, sealed
Close beaker bottleneck；S7, then by after four hours, being sealed up for safekeeping to suitable quantity of water is added in flask；S8, taking precipitate after two weeks
It is clean in 45 DEG C of acetone soln, it is drying to obtain soluble polyurethane surfactant.
5. skin-care detergent according to claim 1, it is characterised in that the preparation of the krill shell enzymolysis product
Method is：After the pretreatments such as krill shell is size-reduced, sieving and impurity elimination, with solid-liquid ratio 1: 5（m/V）Add water, soaked overnight,
By the way of trypsase and papain mixed enzymolysis, enzymatic hydrolysis condition is：45 DEG C of temperature, pH 7.5, hydrolysis time
The enzyme concentration of 2 .5h, trypsase and papain is respectively 1500 U/g and 1300U/g；The enzyme that gone out after terminating is digested, by enzyme
Solution liquid 5000r/min centrifugations 10min at 4 DEG C, takes supernatant, then obtain krill shell enzymolysis product by micro-filtration.
6. skin-care detergent according to claim 1, it is characterised in that the preparation method of the vinegar unstrained spirits aqueous extract is：
The vinegar unstrained spirits after acetic fermentation is taken, by 1:6 solid-liquid ratio（g:mL）Distilled water is added, is filtered after the h of mechanical shaking extraction 3 at room temperature
Filtrate is obtained, by filtrate again by 0.22 μm of sterilised membrane filter filtration sterilization, vinegar unstrained spirits aqueous extract is obtained.
7. the preparation method of a kind of skin-care detergent as described in any one of claim 1- 6, it is characterised in that including following
Specific steps：By in deionized water addition reactor, 70 DEG C are heated to, soluble polyurethane type table is sequentially added by weight
Face activating agent, after shitosan amphoteric polymeric surfactant stirs, temperature is down to 40 DEG C, and the PH values of solution are adjusted to
7.1, add Rosemary Oil, krill shell enzymolysis product, vinegar unstrained spirits aqueous extract to be stirred until homogeneous, the feed liquid that will be stirred is entered
Row degassing, using vacuum outgas, vacuum cavitations are dispensed in 5Mpa to mixed liquor, you can obtain skin-care detergent.
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