WO2021196628A1 - 一种天然化可食性洗发剂及其制备方法 - Google Patents

一种天然化可食性洗发剂及其制备方法 Download PDF

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WO2021196628A1
WO2021196628A1 PCT/CN2020/128681 CN2020128681W WO2021196628A1 WO 2021196628 A1 WO2021196628 A1 WO 2021196628A1 CN 2020128681 W CN2020128681 W CN 2020128681W WO 2021196628 A1 WO2021196628 A1 WO 2021196628A1
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Prior art keywords
shampoo
hair
edible
grade
food
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PCT/CN2020/128681
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English (en)
French (fr)
Inventor
贾福怀
马云龙
郑宇强
涂宏建
王彩霞
熊菲菲
王鹏泽
李�杰
陈李红
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宁波御坊堂生物科技有限公司
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Priority to US17/758,232 priority Critical patent/US20230026434A1/en
Publication of WO2021196628A1 publication Critical patent/WO2021196628A1/zh

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34—Alcohols
    • A61K8/345—Alcohols containing more than one hydroxy group
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36—Carboxylic acids; Salts or anhydrides thereof
    • A61K8/365—Hydroxycarboxylic acids; Ketocarboxylic acids
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37—Esters of carboxylic acids
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37—Esters of carboxylic acids
    • A61K8/375—Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/39—Derivatives containing from 2 to 10 oxyalkylene groups
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/55—Phosphorus compounds
    • A61K8/553—Phospholipids, e.g. lecithin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60—Sugars; Derivatives thereof
    • A61K8/602—Glycosides, e.g. rutin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/63—Steroids; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
    • A61K8/645—Proteins of vegetable origin; Derivatives or degradation products thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/86—Polyethers
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/88—Polyamides
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9789—Magnoliopsida [dicotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00—Preparations for care of the hair
    • A61Q5/006—Antidandruff preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00—Preparations for care of the hair
    • A61Q5/02—Preparations for cleaning the hair
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00—Preparations for care of the hair
    • A61Q5/12—Preparations containing hair conditioners
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59—Mixtures
    • A61K2800/592—Mixtures of compounds complementing their respective functions

Definitions

  • the invention relates to a natural edible shampoo and a preparation method thereof.
  • Shampoo is one of the products with the largest market scale, the most difficult technology and market competition, and the broadest development prospect in the cosmetics industry and even the daily chemical industry.
  • the quality of its ingredients directly affects human health.
  • people With the progress of society and the increase in health awareness of the whole people, people are more and more concerned about the hidden dangers caused by long-term application of shampoo composed of synthetic chemical ingredients on the scalp closest to the brain.
  • Rational consumers are no longer blindly pursuing famous brands. Enterprise products follow the trend of fashion styles, but advocate safe, environmentally friendly and healthy natural cosmetics and high-tech shampoo products with both washing and care. We look forward to the launch of such safe and hygienic daily necessities.
  • the raw materials selected for the product are all food grade, which can be used to make food;
  • the raw materials selected for the product are natural products, or, the raw materials selected for the product are natural products as raw materials, and are scientifically combined (by chemical bonds) through a green environmentally friendly chemical reaction process, without introducing non-natural formations (ie artificially synthesized Rather than naturally occurring) groups, the core groups of the products are all natural, and can be decomposed by nature or by the human body’s biological enzymes and other biological decomposition systems into the same structural products as natural products that exist in nature, and their decomposition Green environmental protection products that do not harm human health with intermediates;
  • P&G has realized continuous product innovation and brand building. Its five major brands are Head & Shoulders-Anti-dandruff, Rejoice-Supple, Pantene-Nutrition, Sassoon-Moisturizing, and Ikalu-Natural. Together with Unilever's Lux, Sunsilk, Qingyang and other brands, it is the No.
  • silicone oil that is, polydimethylsiloxane in the shampoo ingredient list (on the market).
  • silicone oil can help smooth hair scales, reduce friction damage, and make hair smooth.
  • silicone oil is adsorbed on the surface of the hair and has a protective effect, but silicone oil is insoluble in water and can block hair follicles and cause dandruff , Itchy head, oily head, dry and damaged hair, and even hair loss.
  • the non-silicone oil shampoo which has the function of preventing clogged pores, is emerging as the new favorite of daily chemical companies, attracting the follow-up of famous daily chemical giants. Silicone-free shampoo products that claim to be more effective in cleaning hair roots have become the object of pursuit of major daily chemical brands. Unilever also joined the competition for silicone-free shampoos and launched Qingyang’s high-end anti-dandruff products without silicone oil. Procter & Gamble's Icarlo 0-Sense Natural Series and Pantene Pure Brightening Repairing Silicone-free Shampoo have also been launched. Henkel's Silk Yun, L'Oreal Paris, and Hong Kong Uniasia have all launched their own silicone-free shampoo and hair care products. , Which makes the core functional additives of shampoo take a big step towards green and environmental protection and safety.
  • 3Surfactants that can be used for food processing have low HLB value, most of which are emulsifying and dispersing agents, with weak cleaning ability, extremely poor foaming performance, and short foam duration, which cannot pass cleaning, suspension and anti-resettling methods Come to wash away a variety of dirt in the scalp and hair;
  • a stable mixture of surfactant/cationic polymer/oily agent that can be used as a detergent When diluted with water in a large amount, the oily substance that was originally solubilized will break away from the micellar solubilization system, demulsify and precipitate, with the help of synthetic cationic high The flocculation of molecules adsorbs on the surface of the hair to achieve a closed slipping "hair care” effect, thus completing the shampoo and hair care process.
  • This "shampoo and care mechanism” has always dominated the research and development of shampoo industry products, and it has also become an important obstacle to the breakthrough of natural edible shampoo-related products.
  • the technical problem to be solved by the present invention is to provide a natural edible shampoo that can resist static electricity, improve hair smoothness, prevent clogging of pores, and have good fluidity at low temperatures in view of the current state of the art.
  • Another technical problem to be solved by the present invention is to provide a method for preparing the above-mentioned naturalized edible shampoo according to the current state of the art, which is safe and environmentally friendly, easy to operate, and prepared naturalized edible shampoo It has the unique advantages of wet and dry combing and smooth combing, hair fluffy and flowing after washing and drying, and moisturizing and nourishing the scalp, removing dandruff and relieving itching, and is safe It is non-toxic and does not harm human health.
  • a natural edible shampoo which is characterized in that: in parts by weight, it includes the following components
  • the above components are selected from food-grade raw materials that can be used in cosmetics, and can be used to make food.
  • the components themselves or each group of the components are derived from nature and can be decomposed into natural products.
  • the natural edible shampoo of the present invention adopts a true sulfate-free formula, special for mothers and infants, and has less stimulation data than the most environmentally friendly, safe and healthy amino acid surface active preparation similar products currently on the market (still non-cosmetic homologous products) ).
  • the above shampoo overturns the existing classic concept of cationic hair care (more irritating). It uses almost non-irritating natural anionic wash and care ingredients, and relies on non-blocked protein peptides/low HLB oily agents to form a smooth film.
  • the system avoids the cationic polymer/silicone oil hair care model with strong negative effects, protects the original ecological environment of the hair and scalp, and makes the final product achieve the smooth experience of silicone oil. It is a two-in-one shampoo for cosmetics The research and development of the company has created a new path.
  • the fatty acyl lactoyl lactic acid is prepared by a medium temperature esterification process, and the preparation method is as follows:
  • a Mix the food grade lactic acid with the food grade fatty acid according to the molar ratio of 1.2 ⁇ 1.28:1, and add the mixture to an inert solvent with water.
  • the weight of the inert solvent is 2% of the total weight of the mixture of food grade lactic acid and food grade fatty acid. ⁇ 5 times, continue to add food grade phosphoric acid catalyst accounting for 0.5% of the total material weight into the system, and carry out the esterification dehydration reaction at 110-116°C; the above-mentioned food grade fatty acids are selected from ten to sixteen carbon fatty acids;
  • the product is recrystallized and purified, decolorized and deodorized in a food-grade solvent, and finally recrystallized and purified again to obtain the fatty acyl lactoyl lactic acid.
  • the arginine is anhydrous arginine recrystallized from ethanol.
  • the nutritional type of the present invention The shampoo mode exerts the excellent antistatic and smooth hair care properties of fatty acyl lactoyl lactic acid arginine salt, avoids many negative effects caused by strong cationic polymers, and has the effect of smoothing hair.
  • the vegetable oleic acid monoglyceride is the product of a monoesterification reaction between food grade twelve to thirty-two carbon fatty acids and glycerol;
  • the vegetable phospholipid is selected from soybean phospholipids, peanut phospholipids, and sunflower seed phospholipids.
  • Commercially available soybean lecithin is preferred.
  • the above-mentioned vegetable oleic acid monoglycerides are preferably commercially available olive oil monoglycerides.
  • the ⁇ -polylysine is a cationic polymerized polypeptide composed of 25-30 lysine residues used as a food preservative, with a polymerization degree higher than decapeptide, and a molecular weight between 3600-4300.
  • the inulin is an edible chicory root extract
  • the potassium glycyrrhizinate is an edible licorice extract
  • the dipolyglycerol fatty acid ester is an esterification product of food-grade eight to twelve-carbon fatty acid and a food-grade dipolyglycerol mainly linear and containing a small amount of cyclic chains.
  • the first choice is commercially available dipolyglycerol sesquicaprylate.
  • the tetraglycerol olive oil is an esterification product of food-grade oleic acid and food-grade tetraglycerol mainly linear and containing a small amount of cyclic chains;
  • the polyglycerol monofatty acid Ester is the esterification product of food-grade eight to twelve-carbon fatty acids and food-grade six to ten polyglycerols with mainly straight-chain type and containing a small amount of cyclic chains.
  • the soluble vegetable protein glycerin solution is a glycerin solution of alcohol-soluble wheat protein or zein with a molecular weight of 10000-30000D, and the protein content is greater than 6%.
  • the commercially available tasteless alcohol-soluble wheat protein is preferred.
  • the polyhydric alcohol is selected from glycerol, xylitol, sorbitol or a mixture thereof, and preferably pharmaceutical grade or cosmetic grade glycerin.
  • the components of the naturalized edible shampoo of the present invention may also contain natural fragrances, and the natural fragrances are commercially available natural essential oils, such as jasmine essential oil, quince essential oil, chamomile essential oil, or ylang ylang essential oil.
  • step (2) The material obtained in step (2) is aged at room temperature for 20-30 hours to obtain the natural edible shampoo.
  • the present invention utilizes the antistatic properties of arginine on the hair, exerts the excellent antistatic hair care effect of anionic surfactant fatty acyl lactoyl lactate arginine salt, and creates a precedent for the use of edible anionic surfactant as an antistatic agent.
  • anionic surfactant fatty acyl lactoyl lactate arginine salt
  • creates a precedent for the use of edible anionic surfactant as an antistatic agent With the combination of lysine/lauroylarginine ethyl ester hydrochloride/fatty acid polyglycerol ester/inulin synergistic natural edible oily agent system, the hair has a significant smoothing and drag reduction effect, and the hair is safe and nutritious Care enters a brand-new model;
  • the inulin (chicory root extract) used in the health food of the present invention is a non-ionic fructose polymer, in the amine salt of lactoyl lactic acid, it exhibits obvious antistatic and hair-increasing smoothing properties. It can easily eliminate static electricity when drying hair and combing;
  • the alcohol-soluble vegetable protein glycerin dispersion and cationic lauroyl arginine ethyl ester hydrochloride and polylysine work together to combine the non-ionic natural oily surface activity with low HLB value (moderate membrane permeability Unlike silicone oil film which is neither air permeable nor water permeable), it firmly adsorbs on the surface of the hair to form a moderately permeable but well-permeable protective film, which maintains the original ecological environment of the hair and has a long-lasting effect, creating a similar effect to silicone oil.
  • the alcohol-soluble vegetable protein/plant phospholipid (containing natural quaternary ammonium structure) system of the present invention shows excellent affinity and permeability to hair due to the bonding effect, which is easy to increase the plasticity of hair keratin and is super strong
  • the water retention phospholipids are colloidal in water to show the function of high water retention resin
  • antistatic synergistic effect which greatly improves the hair's fluffy effect
  • the invention uses 5 fatty acyl lactoyl lactic acid and ideal foam stabilizing basic amino acid-arginine to neutralize the salt in the best proportion, low cost, easy to popularize, strong foaming during shampoo operation, large and large foam And long-lasting, it can effectively suspend the deep hidden hair dirt from the roots and scalp, and effectively reduce the return of fine dirt to the scalp and block some pores;
  • the present invention uses cheap polyol as a carrier to construct an anhydrous system, which solves the problem of long-term storage of fatty acyl lactyl lactate, moisture absorption and hydrolysis, and the product storage period can be extended to more than two years.
  • the lauroyl arginine ethyl ester hydrochloride and polylysine which can be used as food preservatives in the present invention, have a moderate inhibitory effect on a variety of pathogenic microorganisms including fungi that cause scalp inflammation.
  • the formula of the present invention contains more water-retaining groups such as lactoyl lactic acid and polyglycerin, which act on related parts, moisturize the hair and scalp while washing, maintain the oil-water balance to maintain the original micro-ecological environment, and can use the same product for a long time.
  • water-retaining groups such as lactoyl lactic acid and polyglycerin, which act on related parts, moisturize the hair and scalp while washing, maintain the oil-water balance to maintain the original micro-ecological environment, and can use the same product for a long time.
  • the shampoo of the present invention is easy to wash, and the scalp residues are edible ingredients, which completely eliminates consumers’ concerns about the numerous scalp pores closest to the brain and chemical shampoo residues are unhealthy Over-absorption of ingredients leads to concerns about health hazards.
  • the naturalized edible shampoo of this embodiment includes the following components:
  • the above components are selected from food-grade raw materials that can be used in cosmetics, among which:
  • ⁇ -polylysine was purchased from Zhengzhou Binafo Bioengineering Co., Ltd.;
  • Anhydrous inulin is a chicory root extract from Xian Ting, France, with the product name "NATULIN NC100 chicory root conditioner";
  • the remaining components are commercially available products.
  • step (2) The material obtained in step (2) is aged at room temperature for 24 hours to obtain the naturalized edible shampoo, which is a flowable micro-thick transparent liquid, and the consistency does not exceed 3500mPa in winter (0 ⁇ 4°C) .s.
  • the naturalized edible shampoo of this embodiment includes the following components:
  • the above components are selected from food-grade raw materials that can be used in cosmetics, among which:
  • the 6% alcohol-soluble vegetable protein glycerin solution was supplied from Chongqing Haifan Biochemical Technology Co., Ltd.;
  • Anhydrous inulin is a chicory root extract from Xian Ting, France, with the product name "NATULIN NC100 chicory root conditioner";
  • the remaining components are commercially available products.
  • the material obtained in step (2) is aged at room temperature for 24 hours to obtain the natural edible shampoo gel with good transparency.
  • the consistency at room temperature is not less than 8000mPa.s, and it can be filled into an extruded paste. In the tube.
  • the acute oral toxicity LD50 of the above natural edible shampoo to rats is measured to be greater than 24800mg /kg, which proves that the product series of the present invention belongs to the non-toxic grade range, thereby indirectly proves that the natural edible shampoo of the present invention occasionally strays into the human body and does not harm health because the intermediate and final products of human metabolism are in the non-toxic grade range.
  • zein which is almost completely insoluble in water, interacts with surfactants, and its water solubility increases.
  • the more irritating surfactants dissolve zein more easily than the weakly irritating surfactants. Therefore, according to the changes in the nitrogen content before and after the action of the surfactant in the aqueous solution, the solubility of zein after the action of the surfactant is determined, and the nitrogen content in the dissolved zein (the unit of zein value is in g/L) and the surface activity
  • the skin irritation caused by the agent is proportional to the irritation of the surfactant.
  • the hair strands using the natural edible shampoo of the present invention after blowing at high temperature (60°C) (5 minutes each time) for 50 times, it still remains soft and shiny, which proves that it can protect the hair quality without fear of blowing. After 20 times of combing and pulling, there is no broken hair on the glassware, indicating that the product can effectively nourish the hair and reduce the breakage.
  • the tensile tester is a test instrument specially used to evaluate the combing performance of hair. It uses a standard comb to imitate the action of combing human hair, combing a bunch of hair and recording it by the terminal. When the comb passes through the hair fiber, it shows the force (unit: gf) loaded in the specified displacement (unit: mm) when it overcomes the resistance of the hair and stretches. To evaluate the care effect of shampoos or hair care products by testing the dry and wet combing strength index of the hair before and after use of the sample.
  • the natural edible shampoo of the present invention and commercially available shampoos (including two-in-one silicone oil shampoos such as Suporin Antidandruff Silky Shampoo and amino acid-free silicone oil shampoos such as Suporin Heng no silicone oil shampoo)
  • two-in-one silicone oil shampoos such as Suporin Antidandruff Silky Shampoo
  • amino acid-free silicone oil shampoos such as Suporin Heng no silicone oil shampoo
  • Tress shampoo treatment Weigh 4g of the tested shampoo sample, knead it on the treated hair tress until the foam is uniform, let it stand for 5 minutes, rinse the hair tress with tap water until there is no foam, and let it dry naturally.
  • This test mainly examines the natural edible shampoo of the present invention, the commercially available two-in-one silicone oil shampoo, Suporandidehen anti-dandruff silky shampoo, and the commercially available amino acid-free silicone oil shampoo, Suporandidehen non-silicone oil shampoo.
  • the degree of improvement of the combability of the hair after shampooing was tested by a tensile tester and the average load (gf) of the hair bundles treated with the three shampoos was recorded to compare the combing force of dry hair.
  • the data results are as follows:
  • the average dry combing load (gf) of the naturalized edible shampoo after washing the hair is less than the commercial two-in-one silicone oil shampoo and the commercial amino acid-free silicone oil shampoo, indicating that it can obviously give the hair Brings a moisturizing feeling, counteracts and balances the dryness caused by surfactant degreasing, and has better dry combability than commercially available amino acid-free silicone oil shampoos, achieving similar experience effects as commercially available 2-in-1 silicone oil shampoos.

Abstract

一种天然化可食性洗发剂及其制备方法，包括组分脂肪酰乳酰乳酸、精氨酸、植物油酸单甘油酯、植物磷脂、ε‑聚赖氨酸、月桂酰精氨酸乙酯盐酸盐、菊粉、多元醇等，能抗静电、提高头发顺滑度、防止毛孔堵塞、低温下流动性好；其推翻了现有阳离子护发(刺激较大)的经典理念，运用几乎无刺激的天然化阴离子型洗护主料，依托非封闭型蛋白肽/低HLB值油性剂成膜顺滑体系，规避负面效应强烈的阳离子高聚物/硅油护发模式，保护头发与头皮的原生态环境，使最终产品达到有机硅油的顺滑体验感，为食妆型洗护二合一洗发剂的研发创出一条新路。

Description

一种天然化可食性洗发剂及其制备方法 技术领域
本发明涉及一种天然化可食性洗发剂及其制备方法。
背景技术
洗发剂是化妆品行业乃至日化产业中市场规模最大，技术及市场竞争难度最大且发展前景最广阔的产品之一，其配料的优劣直接影响人体健康。随着社会的进步，全民健康意识的增强，人们对离大脑最近的头皮长期涂抹由合成化学成份构成的洗发剂而引发的诸多隐患的担忧越发强烈，理性的消费者已不再盲目追求名牌企业产品，跟风时尚款式，而是崇尚安全、环保、健康的天然化妆食同源且洗护兼备的高科技洗发产品，期待该类安全卫生的日用生活必需品的面市。
本发明述及“天然化可食性产品”概念界定如下：
(1)产品所选原料都是食品级，可用于制作食品；
(2)产品所选原料为自然界天然产物，或者，产品所选原料是以自然界天然产物为原料，经绿色环保化学反应工艺科学结合(以化学键结合)，不引入非天然形成(即人工合成的而非天然存在的)的基团，产物核心基团都是天然的，可被自然界分解或被人体的生物酶及其他生物分解系统分解成自然界存在的天然产物相同的结构产物，且其分解的中间物无损人体健康的绿色环保产物；
(3)产品所选原料符合化妆品规范要求，无刺激过敏。
用妆食同源方案，结合天然化工艺，制备洗护兼备的洗发剂，一直是业界追求的崇高目标。各大名牌公司已经为推进洗发剂的绿色环保化进程作了不懈的努：
70年代末，中国诞生了第一瓶洗发露——蜂花牌洗发露；80年代采用简单中国药草配方的香波开始流行，并采用传统的功能定位，例如黑发型、防脱发型、止痒型等。1988年以前中国洗发水市场以海欧、蜂花、美加净等国内洗发水品牌为主，价格低廉，洗发、护发产品分开，除了洁净能力外，没有其它显著的功能差异。
1986年联合利华进入中国市场生产力士洗发水，随后1988年宝洁公司进入中国后敏锐把握住了中国消费者的认知缺口，快捷推出国内第一支去头屑洗发水“海飞丝”，海飞丝令中国消费者对头屑问题的认识发生根本的变化。随后宝洁又陆续推出飘柔“二合一”洗发水，就是方便的2合1概念，奠定了中国未来洗发水产品研发的主流。加上随后的潘婷营养洗发露，宝洁运用先进的技术及营销手段迅速占据市场领导地位。仅三个品牌在全国洗护发市场的市场占有率最高时达60％。宝洁的成功又吸引了联合利华、花 王等跨国公司相继推出力士、夏士莲、花王飞逸、诗芬、蓝蓓丝等洗发水品牌来共同瓜分市场，并带动这一市场向高品质、多品种、功能化迅速发展。
面对宝洁公司的垄断地位，奥妮、舒蕾分别发起了两次有力的挑战，以植物概念定位，很大程度上改变了中国洗发水市场面貌。随着市场缺口的打开，一些企业也纷纷运用独创技术或品牌延伸战略抢入市场。在此期间，宝洁公司除推出沙宣、润妍品牌外，又争相推出多样化产品品种包装，中国洗发水市场竞争空前激烈起来。
宝洁凭借高科技多品牌战略和本土化战略，实现了持续的产品创新和品牌塑造，旗下形成海飞丝—去屑、飘柔—柔顺、潘婷—营养、沙宣—保湿、伊卡璐—天然五大品牌，与联合利华旗下的力士、夏士莲、清扬等品牌，稳坐第一集团，市占率逾越70％；欧莱雅、丝宝集团的舒蕾、霸王、广东名臣(蒂花之秀、美王、依采、高新康效)、拉芳等品牌洗发水形成第二集团；其余国产品牌如采乐、好迪、奥妮、拉芳等形成第三集团。洗发水品牌之间将继续发展和互相侵入对方的细分市场，推动了市场价格的下降、形成垄断竞争的格局。
作为对仅具洁净作用的传统洗发剂的升级，宝洁倡导的飘柔“二合一”洗发水因添加硅油，即洗发水成分表中的聚二甲基硅氧烷类的物质(市场上近九成洗发水含有硅油)，能帮助抚平毛鳞片，减少摩擦损伤，使头发顺滑，同时，硅油吸附在头发表层，有保护作用，但硅油不溶于水，会堵住毛囊导致头屑、头痒、头油，使头发干枯受损，甚至脱发。
应运而生的有防止毛孔堵塞功能的无硅油洗发水正在成为日化企业新宠，吸引了著名日化巨头的跟进。宣称对发根清洁更具效果的无硅油洗发水产品已成为各大日化品牌追捧的对象。联合利华也加入了无硅油洗发水的竞争行列，推出清扬无硅油高端去屑系列产品。宝洁旗下伊卡璐0感自然系列、潘婷纯净莹亮修护无硅油洗发乳也相继面市，德国汉高旗下丝蕴、巴黎欧莱雅、香港环亚均推出了各自的无硅油洗发护发产品，这使洗发剂核心功能添加剂向绿色环保安全化方向跨出了一大步。
与此同时，洗发剂的主料表活也经历了从化学合成的脂肪醇硫酸盐、脂肪醇聚氧乙烯醚硫酸盐(AES)向绿色环保安全的烷基葡萄糖苷(APG)、脂肪酰氨基酸盐(氨基酸表活)、脂肪酰牛磺酸盐及至脂肪酸聚甘油酯的飞跃，例如广州环亚的滋源无硅油氨基酸洗发水系列，已得到市场的认可。
但时及至今，符合上述天然化可食性洗发剂概念定位的相关产品仍未大众化，技术界总结出配方及制备工艺上存在的许多制约瓶颈，集中体现为以下几点：
①能完全替代有机硅油的对头发有极佳顺滑效果的天然化可食性梳理减摩擦剂仍没找到，导致目前任何一款绿色健康型的洗发水的梳理顺滑性未能达到或超越经典的硅油类洗发剂；
②支撑洗发剂抗静电及干梳减摩持久性的核心助剂始终是化学合成的聚季铵盐高 聚物或化学改性(接化学阳离子化试剂)的天然胶，该类物质的天然化可食性替代物或协同组合体系的採索仍无实质性突破；
③可作食品加工用的表面活性剂HLB值较小，大多是乳化分散剂，净洗能力薄弱，发泡性能极差，且泡沫持续时间短，无法通过净洗、悬浮及抗再沉的方式来洗干净头皮及头发中的多种污垢；
④天然化可食性表活极易水解失效，难以抵抗微生物致腐而变质，天然化可食性防腐剂筛选困难,导致产品稳定性较差，货架期短，难以商品化；
⑤天然化可食性组份大多功能单一，功效强劲度不足，显效速度缓慢，去屑止痒方面更为逊色，导致由其组合物构成的洗发体系无法与化学合成的洗发剂抗争而全民普及。
另外，品种繁多，迭代快捷的市售二合一洗护型洗发剂所遵循的“洗护机理”依旧如下：
可充当净洗剂的表面活性剂/阳离子高聚物/油性剂组成的稳定混合物，当用水大量稀释时，原先被增溶的油性物质脱离胶束增溶体系，破乳析出，借助合成阳离子高分子物的絮凝作用，吸附在头发表面，达到封闭型增滑“护发”效果，从而完成洗发护发过程。该“洗护机理”一直主宰洗发剂行业产品的研发，亦成为天然化可食性洗发剂相关产品获得突破的重要障碍。
发明内容
本发明所要解决的技术问题是针对现有技术的现状，提供一种能抗静电、提高头发顺滑度、防止毛孔堵塞、低温下流动性好的天然化可食性洗发剂。
本发明所要解决的另一个技术问题是针对现有技术的现状，提供一种上述天然化可食性洗发剂的制备方法，该方法安全环保、操作易捷，制备的天然化可食性洗发剂具有已使大众消费者“上瘾"的洗护二合一经典硅油洗发剂所特有的湿干梳顺滑、洗吹干后头发蓬松飘逸等优点，并且保湿滋养头皮、去屑止痒，安全无毒，无损人体健康。
本发明解决上述技术问题所采用的技术方案为：一种天然化可食性洗发剂，其特征在于：按照重量份数计，包括以下组分
Figure PCTCN2020128681-appb-000001
Figure PCTCN2020128681-appb-000002
上述各组分均选自可用于化妆品的食品级原料，可用于制作食品，组份本身或组份每个基团均源自天然，可分解成天然产物。本发明的天然化可食性洗发剂采用真正的无硫酸盐配方，母婴孕专用，刺激数据小于目前面市的最环保安全健康的氨基酸表活调制的类似产品(仍属非妆食同源型)。
上述洗发剂推翻了现有阳离子护发(刺激较大)的经典理念，运用几乎无刺激的天然化阴离子型洗护主料，依托非封闭型蛋白肽/低HLB值油性剂成膜顺滑体系，规避负面效应强烈的阳离子高聚物/硅油护发模式，保护头发与头皮的原生态环境，使最终产品达到有机硅油的顺滑体验感，为食妆型洗护二合一洗发剂的研发创出一条新路。
在上述方案中，所述的脂肪酰乳酰乳酸由中温酯化工艺制备得到，制备方法为：
a、按照摩尔比1.2～1.28:1将食用级乳酸与食用级脂肪酸混合，并将该混合物加入带水的惰性溶剂中，该惰性溶剂的重量为食用级乳酸与食用级脂肪酸混合物总重量的2～5倍，继续向该体系中加入占总物料重量0.5％的食品级磷酸催化剂，于110～116℃进行酯化脱水反应；上述食用级脂肪酸选用十至十六碳脂肪酸；
b、反应完毕后，对生成物进行重结晶提纯，并在食用级溶剂中进行脱色、脱味，最后再次重结晶提纯得到所述的脂肪酰乳酰乳酸。
优选地，所述的精氨酸为乙醇中重结晶后的无水精氨酸。
现有技术中以传统硫酸盐表活如脂肪醇硫酸盐(K12)、脂肪醇聚氧乙烯醚硫酸盐(AES)为主料的二合一洗发剂，当用大量水冲时，浓度降至微量，原先被增溶的油性物质(如有机硅油)破乳析出，借助合成阳离子高分子物质或阳离子改性的天然胶的絮凝作用，吸附在头发表面，达到封闭型增滑“护发”效果，然而过度使用硅油会使其沉积在头发表面与毛囊处，影响头发新陈代谢，并且电荷密度较高的阳离子高聚物在头发表面的累积残留是困惑业界的永远的痛，本发明的营养型洗发模式发挥肪酰乳酰乳酸精氨酸盐优异的抗静电及护发顺滑特性，避开了强劲的阳离子高聚物所致的诸多负面影响，而起到增滑护发效果。
优选地，所述的植物油酸单甘油酯为食品级十二至三十二碳脂肪酸与甘油进行单酯化反应的产物；所述的植物磷脂选自大豆磷脂、花生磷脂、葵花籽磷脂。首选市售大豆磷脂。上述植物油酸单甘油酯首选市售橄榄油酸单甘酯。
优选地，所述的ε-聚赖氨酸为用作食品防腐剂的由25-30个赖氨酸残基组成的阳 离子聚合多肽，聚合度高于十肽，分子量在3600—4300之间。
优选地，所述的菊粉为食用菊苣根提取物，所述的甘草酸钾为食用甘草提取物。
优选地，所述的二聚甘油脂肪酸酯为食品级八至十二碳脂肪酸与直链型为主并含微量环链的食品级二聚甘油的酯化产物。首选市售二聚甘油倍半辛酸酯。
优选地，所述的四聚甘油橄榄油酸酯为食品级橄榄油酸与直链型为主并含微量环链的食品级四聚甘油的酯化产物；所述的多聚甘油单脂肪酸酯为食品级八至十二碳脂肪酸与直链型为主并含微量环链的食品级六至十聚甘油的酯化产物，首选市售十聚甘油辛酸酯；所述的食品级醇溶性植物蛋白甘油溶液系分子量为10000-30000D的醇溶性麦蛋白或玉米蛋白的甘油溶液，蛋白质含量大于6％，首选市售无味型醇溶性麦蛋白。
优选地，所述的多元醇选自甘油、木糖醇、山梨醇或其混合物等，首选药用级或化妆品级甘油。
本发明天然化可食性洗发剂的组分中还可以包含有天然香料，所述的天然香料为市售天然精油，如茉莉精油、玟瑰精油、洋甘菊精油或依兰精油等。
一种上述天然化可食性洗发剂的制备方法，其特征在于包括以下步骤：
(1)预配料配制
中和过程：
在搅拌条件下，将精氨酸投入占多元醇总量1/2的多元醇中，底部鼓入高纯氮气保护，升温至80～85℃，溶解并脱水至少1小时，待物料完全透明，含水量小于0.1％，得A料；
在搅拌条件下，将脂肪酰乳酰乳酸投入占多元醇总量1/4的多元醇中，底部鼓入高纯氮气保护，升温至80～85℃，溶解并脱水至少二十分钟，待物料呈均质态，含水量小于0.1％，得B料；
在搅拌条件下，控温80～85℃，将A料分批缓慢倒入B料中，严格控制PH值小于7.2，底部鼓入高纯氮气保护，中和反应至少1.5小时，至体系完全透明，得C料；
微乳化过程：
在搅拌条件下，控温60～75℃，将植物油酸单甘油酯、二聚甘油脂肪酸酯、四聚甘油橄榄油酸酯和多聚甘油单脂肪酸酯依次缓慢投入C料中，混合充分至少0.5小时，投入甘草酸钾，继续搅拌至少1.5小时，至体系完全透明，得D料；
(2)调合料制备
在搅拌条件下，将食品级植物磷脂投入占多元醇总量1/12的多元醇中，底部鼓入高纯氮气保护，升温至55～60℃，化融分散至少4小时，待物料呈均质可流动稠状液，得E料；
在搅拌条件下，将食品级ε-聚赖氨酸和月桂酰精氨酸乙酯盐酸盐投入占多元醇总量1/12的多元醇中；升温至65～70℃，溶解至少0.5小时，待物料呈完全透明液，得F料；
在搅拌条件下，将食品级菊粉投入剩余的多元醇中，升温至65～70℃，溶解至少0.5小时，待物料呈完全透明液，得G料；
将D料投入调合锅中，严格控温70～75℃，控制转速100～150rpm，将E料于30分钟内倒入D料中，恒温搅拌15分钟至物料体系完全透明；接着于30分钟内滴加完F料和G料，继续控温70～75℃，控制转速150～250rpm，搅拌15分钟至物料体系完全透明；将物料冷却至55～60℃，于30分钟内将食品级醇溶性植物蛋白甘油溶液分批加入上述物料中，控制转速80～100rpm，搅拌至少45分钟至物料体系呈完全透明低稠态，然后控制转速30～40rpm，边冷却边搅拌至少20分钟，至物料达35℃以下，加入天然香料，搅拌至少20分钟，至物料呈透明高稠可流动胶态状为止；
(3)陈化
将步骤(2)所得物料置于室温下陈化20～30小时，即得到所述的天然化可食性洗发剂。
与现有技术相比，本发明的优点在于：
本发明利用精氨酸对头发的抗静电特性，发挥阴离子表活脂肪酰乳酰乳酸精氨酸盐的优异抗静电护发效果，开创了可食性阴离子表活用作抗静电剂的先例，在聚赖氨酸/月桂酰精氨酸乙酯盐酸盐/脂肪酸聚甘油酯/菊粉协同天然化可食性油性剂体系的配合下，头发获得显著的顺滑减阻效果，头发的安全且营养化洗护进入一种全新的模式；
本发明中用于保健食品的菊粉(菊苣根提取物)虽属非离子型的果糖聚合物，却在乳酰乳酸的胺盐中，表现出了明显的抗静电及增头发顺滑特性，可轻松消除吹干头发梳理时的静电；
本发明中醇溶性植物蛋白甘油分散液与阳离子型月桂酰精氨酸乙酯盐酸盐和聚赖氨酸共同作用，结合低HLB值的非离子天然化油性表活(成膜通透性适中，不同于硅油膜既不透气也不透水)，牢固地吸附在头发表面，形成适中透水但透气性良好的保护膜，保持了头发的原生态环境，且效果持久，营造出与有机硅油类似的丝滑效果，但避免了硅油封死头发毛鳞片导致的多种不良后果，也规避了业界长期依赖的如聚季铵盐等全合成或化学改性的易累积的高分子聚合物作头发湿干梳顺滑长效增强剂的被动局面；
本发明中的醇溶性植物蛋白/植物磷脂(含天然季铵化结构)体系因键合作用而对头发显示出极好的亲合性和渗透性，易使头发角蛋白塑性增强，加之超强的保水性(磷脂遇水呈胶体而显高保水树脂的功能)及抗静电增效作用，大幅度提升头发的蓬松效果；
现有食妆型洗涤剂原料除昂贵价格的人参皂苷、绞股蓝皂苷及大豆皂苷稍能发泡外，绝大多数适合作净洗剂(HLB值大于20)的表面活性剂发泡极难，本发明采用5脂肪酰乳酰乳酸与稳泡性理想的碱性氨基酸-精氨酸以最佳比例中和而成的盐，成本低廉，易于大众化，洗发操作时发泡强劲，泡沫大而多且持久，可有效悬浮源自发根及头皮处而深藏不露的头发污垢，并有效减少细垢重返头皮处而堵塞部分毛孔；
本发明采用廉价多元醇作载体构筑的无水体系，解决了脂肪酰乳酰乳酸盐久贮吸潮水解之难题，产品贮存期可延长至二年以上，为长效型乳酰乳酸盐表活产品的研发拓出一条新思路；同时，针对多元醇作载体构筑的无水体系，当表活含量高时，稠度偏大，低温无法流动甚至硬结等难题，本发明使用可食性醇溶性植物蛋白作强效降凝剂，使产品在冬季低温(0～5℃)时仍能轻易流动而不固结，便于大众化应用；
本发明中可作食品防腐剂的月桂酰精氨酸乙酯盐酸盐与聚赖氨酸对包括引起头皮炎症的真菌在内的多种致病微生物有适中的抑制作用，在抗敏舒缓剂甘草酸钾的协同下，营造出无刺激型止痒去屑效果，且长期使用安全卫生无损健康，规避了使用化学合成型烈性去屑剂(如ZTP、OCT等)导致的抗药性和依赖性以及对头发健康产生的诸多负面影响(如破坏头皮微生物平衡、产生新的过敏等)；食用级月桂酰精氨酸乙酯盐酸盐与自身就有抑菌作用的聚赖氨酸和聚甘油酯类表活构筑自防腐体系，避开化学防腐剂；高HLB值的脂肪酰乳酰乳酸精氨酸盐协同HLB值大于20的脂肪酸多聚甘油酯，组成的体系净洗有机硅油及合成高分子日积月累的残垢能力强劲，泡沫深入头皮毛孔，带走深层污垢，清洁发根，还头皮一个清新轻松的原生态环境，本发明产品可拓展出硅油清除剂系列；
本发明配方组份含较多乳酰乳酸及多聚甘油等保水基团，作用相关部位，洗涤同时保湿头发及头皮，保持油水平衡以维持原有的微生态环境，可长期使用同一种产品而无需频繁更换规格型号；本发明的洗发剂易冲洗，头皮极微量残遗留物属可食性成份，彻底消除了广大消费者对因离脑部最近的头皮毛孔众多，化学洗发剂残留非健康成份过度吸收而导致健康危害的担忧。
具体实施方式
以下结合实施例对本发明作进一步详细描述。
实施例1：
按照重量份数计，本实施例的天然化可食性洗发剂包括以下组分：
Figure PCTCN2020128681-appb-000003
Figure PCTCN2020128681-appb-000004
上述各组分均选自可用于化妆品的食品级原料，其中：
99.8％脂肪酰乳酰乳酸和99.8％月桂酰精氨酸乙酯盐酸盐购自郑州明德生物科技有限公司；
99.5％二聚甘油倍半辛酸酯和99.5％十聚甘油单辛酸酸酯购自佛山市银美联合化工科技有限公司；
99.5％四聚甘油橄榄油酸酯由上海易亨化工有限公司供货；
99.8％ε-聚赖氨酸购自郑州拜纳佛生物工程股份有限公司；
6％醇溶性植物蛋白甘油溶液购自重庆海帆生化科技有限公司；
无水菊粉为法国仙婷的菊苣根提取物，品名“NATULIN NC100菊苣根调理剂”；
其余组份为市售产品。
本实施例中天然化可食性洗发剂的制备方法包括以下步骤：
(1)预配料配制
中和过程：
在搅拌条件下，控制转速100rpm，将无水精氨酸58千克投入285千克甘油中，底部鼓入高纯氮气保护，升温至80～85℃，溶解并脱水2小时，待物料完全透明，含水量小于0.1％，得A料。
在搅拌条件下，控制转速80rpm，将99.8％月桂酰乳酰乳酸120千克投入142千克甘油中，底部鼓入高纯氮气保护，升温至80～85℃，溶解并脱水至少三十分钟，待物料呈均质态，含水量小于0.1％，得B料。
在搅拌条件下，控制转速80rpm，控温80～85℃，将A料分批缓慢倒入B料中，严格控制PH值小于7.2，底部鼓入高纯氮气保护，中和反应2小时，至体系完全透明，得C料。
微乳化过程：
在搅拌条件下，控制转速100rpm，控温60～75℃，将99.5％油酸单甘油酯45千克、99.5％二聚甘油倍半辛酸酯23千克，、99.5％四聚甘油橄榄油酸酯55千克和99.5％十聚甘油单辛酸酯50千克依次缓慢投入C料中，混合充分至少1小时，投入99.5％甘草酸钾2千克，继续搅拌2小时，至体系完全透明，得D料。
(2)调合料制备
在搅拌条件下，控制转速80rpm，将食品级无水大豆磷脂3.5千克投入47.4千克 甘油中，底部鼓入高纯氮气保护，升温至55～60℃，化融分散4.5小时，待物料呈均质可流动稠状液，得E料。
在搅拌条件下，将控制转速80rpm，食品级99.8％ε-聚赖氨酸5千克和99.8％月桂酰精氨酸乙酯盐酸盐6千克投入47.4千克甘油中，升温至65～70℃，溶解1小时，待物料呈完全透明液，得F料。
在搅拌条件下，将控制转速80rpm，食品级无水菊粉12千克投入47.3千克甘油中，升温至65～70℃，溶解至少1小时，待物料呈完全透明液，得G料。
将D料投入调合锅中，严格控温70～75℃，控制转速100rpm，将E料于30分钟内倒入D料中，恒温搅拌15分钟至物料体系完全透明；接着于30分钟内滴加完F料和G料，继续控温70～75℃，控制转速150rpm，搅拌15分钟至物料体系完全透明；将物料冷却至55～60℃，于30分钟内将食品级6％醇溶性植物蛋白甘油溶液50千克分三批加入上述物料中，控制转速80rpm，搅拌至少1小时至物料体系呈完全透明低稠态，然后控制转速30rpm，边冷却边搅拌至少20分钟，至物料达35℃以下，加入玫瑰精油2千克，搅拌至少30分钟，至物料呈透明高稠可流动胶态状为止；
(3)陈化
将步骤(2)所得物料置于室温下陈化24小时，即得到所述的天然化可食性洗发露，外观呈可流动微稠透明液体，冬季时(0～4℃)稠度不超过3500mPa.s。
实施例2：
按照重量份数计，本实施例的天然化可食性洗发剂包括以下组分：
Figure PCTCN2020128681-appb-000005
上述各组分均选自可用于化妆品的食品级原料，其中：
99.8％椰油酰乳酰乳酸和99.8％月桂酰精氨酸乙酯盐酸盐供自郑州明德生物科技有限公司；
99.5％二聚甘油倍半辛酸酯和99.5％六聚甘油单辛酸酸酯供自佛山市银美联合化工科技有限公司；
99.5％橄榄油酸单甘油酯和99.5％四聚甘油橄榄油酸酯由上海易亨化工有限公司供货；
99.8％ε-聚赖氨酸供自郑州拜纳佛生物工程股份有限公司；
6％醇溶性植物蛋白甘油溶液供自重庆海帆生化科技有限公司；
无水菊粉为法国仙婷的菊苣根提取物，品名“NATULIN NC100菊苣根调理剂”；
其余组份为市售产品。
本实施例中天然化可食性洗发剂的制备方法包括以下步骤：
(1)预配料配制
中和过程：
在搅拌条件下，控制转速150rpm，将无水精氨酸65千克投入256.5千克甘油中，底部鼓入高纯氮气保护，升温至80～85℃，溶解并脱水2小时，待物料完全透明，含水量小于0.1％，得A料。
在搅拌条件下，控制转速100rpm，将99.8％椰油酰乳酰乳酸140千克投入128.3千克甘油中，底部鼓入高纯氮气保护，升温至80～85℃，溶解并脱水至少三十分钟，待物料呈均质态，含水量小于0.1％，得B料。
在搅拌条件下，控制转速100rpm，控温80～85℃，将A料分批缓慢倒入B料中，严格控制PH值小于7.2，底部鼓入高纯氮气保护，中和反应2小时，至体系完全透明，得C料。
微乳化过程：
在搅拌条件下，控制转速150rpm，控温60～75℃，将99.5％橄榄油酸单甘油酯50千克、99.5％二聚甘油倍半辛酸酯30千克，99.5％四聚甘油橄榄油酸酯60千克和99.5％六聚甘油单辛酸酯60千克依次缓慢投入C料中，混合充分至少1小时，投入99.5％甘草酸钾6千克，继续搅拌2小时，至体系完全透明，得D料。
(2)调合料制备
在搅拌条件下，控制转速100rpm，将食品级无水大豆磷脂4.5千克投入42.75千克甘油中，底部鼓入高纯氮气保护，升温至55～60℃，化融分散4.5小时，待物料呈均质可流动稠状液，得E料。
在搅拌条件下，将控制转速100rpm，食品级99.8％ε-聚赖氨酸8千克和99.8％月桂酰精氨酸乙酯盐酸盐8千克投入千42.75克甘油中，升温至65～70℃，溶解1小时，待 物料呈完全透明液，得F料。
在搅拌条件下，将控制转速100rpm，食品级无水菊粉18千克投入42.75千克甘油中，升温至65～70℃，溶解至少1小时，待物料呈完全透明液，得G料。
将D料投入调合锅中，严格控温70～75℃，控制转速150rpm，将E料于30分钟内倒入D料中，恒温搅拌15分钟至物料体系完全透明；接着于30分钟内滴加完F料和G料，继续控温70～75℃，控制转速250rpm，搅拌15分钟至物料体系完全透明；将物料冷却至55～60℃，于30分钟内将食品级6％醇溶性植物蛋白甘油溶液35千克分三批加入上述物料中，控制转速100rpm，搅拌至少1小时至物料体系呈完全透明低稠态，然后控制转速40rpm，边冷却边搅拌至少20分钟，至物料达35℃以下，加入茉莉精油2.5千克，搅拌至少30分钟，至物料呈透明高稠可流动胶态状为止；
(3)陈化
将步骤(2)所得物料置于室温下陈化24小时，即得到透明度良好的所述的天然化可食性洗发凝胶，室温稠度不低于8000mPa.s，可装入挤压式膏体管中。
参照有关国家标准及行业标准，就本发明的天然化可食性洗发露与市售洗发水相关性能指标进行对比检测，详述如下：
(一)本发明的天然化可食性洗发露与市售氨基酸无硅油洗发水舒泊阑肽亨无硅油洗发露对比样品的针对头皮护理方面的基本性能进行测定，详见表1。
表1
Figure PCTCN2020128681-appb-000006
表1相关数据表明，本发明的天然化可食性洗发露在PH值、头皮保湿效果等关健指标上均比市售氨基酸无硅油洗发水优异。
(二)毒理学评价
参照GBZ/T240.2-2011化学品毒理学评价程序和试验方法第2部分急性经口毒性试验的相关步骤，测得上述天然化可食性洗发剂对大白鼠的急性经口毒性LD50大于 24800mg/kg，证明本发明的产品系列属无毒级范围，从而间接证明本发明天然化可食性洗发剂偶尔误入人体也因其人体代谢中间及最终产物属无毒级范围而无损健康。
(三)本发明天然化可食性洗发剂与市售洗发水(包括二合一硅油洗发水和氨基酸无硅油洗发水)刺激性对比
测试方法：玉米醇溶蛋白法
方法原理：几乎完全不溶于水的玉米醇溶蛋白(zein)与表面活性剂相互作用，其水溶性加大，较强刺激性的表面活性剂比弱刺激表面活性剂更易溶解zein。因此根据水溶液中表面活性剂作用前后氮含量的变化情况，测定出zein与表面活性剂作用后的溶解度，而所溶解的zein中的含氮量(zein值单位以g/L计)与表面活性剂引起的皮肤刺激性成正比，由此可以了解表面活性剂刺激性的大小。
判断依据：Zein＞4强刺激性；2＜Zein＜4低刺激性；Zein＜2无刺激性。
检测结果相关数据如表2。
表2
Figure PCTCN2020128681-appb-000007
由表2数据可知，本发明的天然化可食性洗发露对头部皮肤的刺激性比市售各种洗发水小得多。
(四)本发明天然化可食性洗发剂与市售洗发水(包括二合一硅油洗发水如舒泊阑肽亨去屑丝柔洗发露和氨基酸无硅油洗发水如舒泊阑肽亨无硅油洗发露)对洗后发束耐高温吹风测试对比
经过吹风机高温(60℃)吹风(每次5分钟)测试，使用市售洗发水(包括二合一硅油洗发水和氨基酸无硅油洗发水)产品的发束被吹风10次后就有些发黄，毛躁干枯；束经过梳拉后，可以看到有不少发丝断落；
而使用本发明天然化可食性洗发露的发束，在高温(60℃)吹风(每次5分钟)达50次后，依然保持柔亮，证明它能保护发质，无惧吹风，发束经过20次梳拉后，玻璃器皿上没有碎发断发，说明该产品能有效滋养发丝，减少断发。
(五)拉力测定仪法测试本发明天然化可食性洗发露与市售洗发水(包括二合一硅油洗发水如舒泊阑肽亨去屑丝柔洗发露和氨基酸无硅油洗发水如舒泊阑肽亨无硅油洗发露)洗后梳理性改善程度相关力学数据对比
1、概述
拉力测试仪是一种专门用于头发梳理性能评价的测试仪器，通过一支标准梳子模仿人梳理头发动作，对一束头发进行梳理并由终端记录。当梳子经过头发纤维时，显示其克服头发阻力拉伸时指定位移(单位：mm)内所载荷的力量(单位：gf)。通过检测样品使用前后发束干、湿梳理力量下降指数，来评价香波或护发产品的护理效果。
所有改变头发发质(如化学处理，去脂和聚合物处理头发)，可通过梳理阻力测定，以上都会造成干发梳理阻力增加。通过拉力仪测试干发梳理性，评价各类型的组分对头发梳理效果的影响。
2、材料与方法
2.1主要仪器及材料
拉力仪；
恒温恒湿培养箱；
若干发束：长度50cm，重量约16g；
洗发剂：本发明天然化可食性洗发露与市售洗发水(包括二合一硅油洗发水如舒泊阑肽亨去屑丝柔洗发露和氨基酸无硅油洗发水如舒泊阑肽亨无硅油洗发露)
2.2发束预处理
准备相同长度(50cm)和重量(约16g)的若干发束。首先，用40℃的自来水清洗两次；然后将发束放置在装有5g十二烷基硫酸钠和1000ml水的烧杯中加热至80℃浸泡；然后将烧杯放置于45℃的恒温恒湿箱中两小时；最后，用自来水冲洗，直至无泡沫，并自然晾干。
发束洗发水处理：称取4g被测洗发剂样品，揉搓至处理后的发束上，至泡沫均匀，静置5分钟，用自来水冲洗发束，直至无泡沫，并自然晾干。
2.3梳理性测试
在拉力仪上分别测定洗发剂处理后发束的干梳理性：
(1)连接主机电源，打开电脑，仪器预热半小时以上；
(2)将组成试验样品的所有试样收集到一起，标识每个试样；打开软件，创建新样品，选择试验方法，命名新样品；
(3)用塑料梳子先梳理头发，然后用合适的夹具固定待测头发样品，将发束自然地放置于梳子中间；
(4)完成仪器的标定和调零后，开始测试发束，以300mm/min的速度拉伸发束，位移200ram，取位移100～200mm之间的载荷值。为了减少因发束不同而带来的测量误差，同一发束重复测试5次，取平均值(程序自动记录数据并计算平均值)。
3、结果与讨论
本测试主要考查本发明天然化可食性洗发露、市售二合一硅油洗发水舒泊阑肽亨去屑丝柔洗发露和市售氨基酸无硅油洗发水舒泊阑肽亨无硅油洗发露洗后对头发梳理性 改善程度，通过拉力仪测试并记录三款洗发剂处理后发束的载荷平均值(gf)来比较干发梳理力大小，数据结果如下：
Figure PCTCN2020128681-appb-000008
由上表可见，发明天然化可食性洗发露洗后对头发干梳载荷平均值(gf)均小于市售二合一硅油洗发水和市售氨基酸无硅油洗发水，说明其能明显给头发带来滋润感，抵消和平衡由于表面活性剂脱脂带来的干涩，干梳理性比市售氨基酸无硅油洗发水更好，达到市售二合一硅油洗发水类似的体验效果。
Figure PCTCN2020128681-appb-000009

Claims (5)

  1. 根据权利要求1或2所述的天然化可食性洗发剂，其特征在于：所述的菊粉为食用菊苣根提取物，所述的甘草酸钾为食用甘草提取物。
  2. 根据权利要求1或2所述的天然化可食性洗发剂，其特征在于：所述的二聚甘油脂肪酸酯为食品级八至十二碳脂肪酸与直链型为主并含微量环链的食品级二聚甘油的酯化产物。
  3. 根据权利要求1或2所述的天然化可食性洗发剂，其特征在于：所述的四聚甘油橄榄油酸酯为食品级橄榄油酸与直链型为主并含微量环链的食品级四聚甘油的酯化产物；所述的多聚甘油单脂肪酸酯为食品级八至十二碳脂肪酸与直链型为主并含微量环链的食品级六至十聚甘油的酯化产物；所述的食品级醇溶性植物蛋白甘油溶液系分子量为10000-30000D的醇溶性麦蛋白或玉米蛋白的甘油溶液，蛋白质含量大于6％。
  4. 根据权利要求1或2所述的天然化可食性洗发剂，其特征在于：所述的多元醇选自甘油、木糖醇、山梨醇或其混合物。
  5. 一种权利要求1～9中任一权利要求所述天然化可食性洗发剂的制备方法，其特征在于包括以下步骤：
    (1)预配料配制
    中和过程：
    在搅拌条件下，将精氨酸投入占多元醇总量1/2的多元醇中，底部鼓入高纯氮气保护，升温至80～85℃，溶解并脱水至少1小时，待物料完全透明，含水量小于0.1％，得A料；
    在搅拌条件下，将脂肪酰乳酰乳酸投入占多元醇总量1/4的多元醇中，底部鼓入高纯氮气保护，升温至80～85℃，溶解并脱水至少二十分钟，待物料呈均质态，含水量小于0.1％，得B料；
    在搅拌条件下，控温80～85℃，将A料分批缓慢倒入B料中，严格控制PH值小于7.2，底部鼓入高纯氮气保护，中和反应至少1.5小时，至体系完全透明，得C料；
    微乳化过程：
    在搅拌条件下，控温60～75℃，将植物油酸单甘油酯、二聚甘油脂肪酸酯、四聚甘油橄榄油酸酯和多聚甘油单脂肪酸酯依次缓慢投入C料中，混合充分至少0.5小时，投入甘草酸钾，继续搅拌至少1.5小时，至体系完全透明，得D料；
    (2)调合料制备
    在搅拌条件下，将食品级植物磷脂投入占多元醇总量1/12的多元醇中，底部鼓入高纯氮气保护，升温至55～60℃，化融分散至少4小时，待物料呈均质可流动稠状液，得E料；
    在搅拌条件下，将食品级ε-聚赖氨酸和月桂酰精氨酸乙酯盐酸盐投入占多元醇总量 1/12的多元醇中；升温至65～70℃，溶解至少0.5小时，待物料呈完全透明液，得F料；
    在搅拌条件下，将食品级菊粉投入剩余的多元醇中，升温至65～70℃，溶解至少0.5小时，待物料呈完全透明液，得G料；
    将D料投入调合锅中，严格控温70～75℃，控制转速100～150rpm，将E料于30分钟内倒入D料中，恒温搅拌15分钟至物料体系完全透明；接着于30分钟内滴加完F料和G料，继续控温70～75℃，控制转速150～250rpm，搅拌15分钟至物料体系完全透明；将物料冷却至55～60℃，于30分钟内将食品级醇溶性植物蛋白甘油溶液分批加入上述物料中，控制转速80～100rpm，搅拌至少45分钟至物料体系呈完全透明低稠态，然后控制转速30～40rpm，边冷却边搅拌至少20分钟，至物料达35℃以下，加入天然香料，搅拌至少20分钟，至物料呈透明高稠可流动胶态状为止；
    (3)陈化
    将步骤(2)所得物料置于室温下陈化20～30小时，即得到所述的天然化可食性洗发剂。
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