CN115487127A - Anti-hair loss oil-control silicone-oil-free shampoo and preparation method thereof - Google Patents
Anti-hair loss oil-control silicone-oil-free shampoo and preparation method thereof Download PDFInfo
- Publication number
- CN115487127A CN115487127A CN202210828320.0A CN202210828320A CN115487127A CN 115487127 A CN115487127 A CN 115487127A CN 202210828320 A CN202210828320 A CN 202210828320A CN 115487127 A CN115487127 A CN 115487127A
- Authority
- CN
- China
- Prior art keywords
- surfactant
- oil
- oil control
- hair loss
- zinc
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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]
- A61K8/9794—Liliopsida [monocotyledons]
-
- 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
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/42—Amides
-
- 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
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/4906—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom
- A61K8/4913—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom having five membered rings, e.g. pyrrolidone carboxylic acid
-
- 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
- A61K8/737—Galactomannans, e.g. guar; 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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/8141—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- A61K8/8152—Homopolymers or copolymers of esters, e.g. (meth)acrylic acid esters; Compositions of derivatives of such polymers
-
- 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
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
-
- 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
- A61K8/9755—Gymnosperms [Coniferophyta]
- A61K8/9761—Cupressaceae [Cypress family], e.g. juniper or cypress
-
- 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
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/005—Antimicrobial 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
- A61Q5/008—Preparations for oily 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
- A61Q5/02—Preparations for cleaning the hair
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q7/00—Preparations for affecting hair growth
-
- 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
- A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
- A61K2800/30—Characterized by the absence of a particular group of ingredients
- A61K2800/34—Free of silicones
-
- 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
-
- 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
- A61K2800/596—Mixtures of surface active compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Epidemiology (AREA)
- Birds (AREA)
- Engineering & Computer Science (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Dermatology (AREA)
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Emergency Medicine (AREA)
- Cosmetics (AREA)
Abstract
The invention relates to the technical field of cosmetics, in particular to the field of IPC A61K8, and more particularly relates to an anti-hair loss and oil control silicone-free shampoo and a preparation method thereof. The oil control agent is compounded from the functional components such as the surfactant, the amino acid compound, the conditioner, the plant extract and the derivatives thereof, the zinc compound and the like, so that the oil control effect can be prolonged for 7 days, the oil control capability of the product is improved, and the micro-ecological environment of the scalp is protected. The anti-hair loss and oil control silicone-free shampoo prepared by the invention is suitable for various hair qualities, such as easily-oiled hair quality, dry hair quality, damaged hair quality, split hair quality and the like.
Description
Technical Field
The invention relates to the technical field of cosmetics, in particular to the field of IPC A61K8, and more particularly relates to an anti-hair loss and oil control silicone-free shampoo and a preparation method thereof.
Background
The Chinese hair care market mainly takes basic hair washing and caring products, and the products tend to be high-end and high-efficiency. Nearly 90% of the Chinese hair care market is the basic hair washing and caring product, and the high-end efficacy product has high demand and is in a high-speed increasing state year by year, and the market proportion is continuously improved. The market share of the medium-high end price level on the e-commerce platform is gradually expanded, the upgrading of the consumption capability is mainly reflected on the products of the medium-high end price level, and the commodities with quality and high-end experience are favored, for example, the commodities with plant high-end components such as oil control, dandruff removal and the like are all increased in an explosive manner. The scalp is exposed to external environment for a long time, is easily affected by ultraviolet rays, heat sources, PM 2.5 and other adverse factors, and if health care of the scalp is not taken, problems of the hair and the scalp appear, such as oily hair, itchy hair, alopecia, much scurf and the like. With the increasing strength of brand merchants, the health relationship between the scalp and the hair is declared, and the maintenance of oil control and hair loss prevention of the scalp becomes a current popular trend.
In the prior art, a patent application document with an authorization publication number of CN101889967B discloses a shampoo or hair conditioner additive and a preparation method of the shampoo or hair conditioner.
The patent application document with the publication number of CN107582455B discloses an anti-dandruff and itching-relieving shampoo and a preparation method thereof, and the anti-dandruff and itching-relieving shampoo also has the effects of hair care and hair nourishing by taking a rhus chinensis extract as an active ingredient for removing dandruff and relieving itching, but the preparation method is complex and the oil control effect is not obviously improved.
The oil control capability of the commercially available silicone oil-free shampoo is improved, but the using flexibility of the product is poor, the oil removal capability of the product in a short time is generally good, and the condition of scalp oil return after washing is obvious. Therefore, the shampoo for preventing hair loss and controlling oil needs to be developed, the preparation method is simple, the prepared shampoo is non-irritating, good in oil removal and control effect, and smooth and non-dry after washing.
Disclosure of Invention
In order to solve the above problems, in a first aspect of the present invention, there is provided an anti-hair loss and oil control silicone-free shampoo, comprising, by weight: 12-25% of surfactant, 5-10% of amino acid compound, 0.01-0.2% of chelating agent, 0.1-11% of plant extract and derivatives thereof, 0.05-2% of emulsifier, 0.02-4% of zinc compound, 0.01-0.2% of pH regulator, 0.001-0.01% of preservative and the balance of water to 100%.
Preferably, the surfactant comprises one or more of ionic surfactant, nonionic surfactant, amphoteric surfactant and compound surfactant; further preferred are ionic surfactants, nonionic surfactants and amphoteric surfactants.
Preferably, the weight ratio of the ionic surfactant, the nonionic surfactant and the amphoteric surfactant is (30-40): (2-10): 1; further preferably (30-35): (4-8): 1; further, the ratio is 32.
Preferably, the ionic surfactant is one or two of an anionic surfactant and a cationic surfactant; further preferably, it is an anionic surfactant.
Preferably, the anionic surfactant is one or more of sodium laureth sulfate, sodium lauryl sulfate, anionic polyacrylamide, sodium dodecyl benzene sulfonate, fatty alcohol-polyoxyethylene ether sulfate, potassium laureth phosphate, sodium lauryl sulfate and fatty alcohol-polyoxyethylene ether sulfate; further preferred is sodium laureth sulfate.
Preferably, the nonionic surfactant is one or more of cocamide methyl MEA, lauryl alcohol polyoxyethylene ether, fatty acid methyl ester polyoxyethylene ether, isomeric tridecanol ether, nonylphenol polyoxyethylene ether and octylphenol polyoxyethylene ether; further preferred is cocamide methyl MEA.
In some preferred schemes, cocamide methyl MEA is used as the nonionic surfactant, and the weight ratio of the ionic surfactant to the nonionic surfactant to the amphoteric surfactant is (30-40): (2-10): 1, the stability of the shampoo can be improved while the richness and the fineness of the foam are further improved. The formulation of the cocamide methyl MEA is good, the compatibility of the cocamide methyl MEA and other two surfactants is good, the cocamide methyl MEA and other surfactants can play a synergistic effect, and a good synergistic tackifying effect is achieved, so that the shampoo is good in stability at high and low temperatures, and the change of the viscosity of the shampoo at high and low temperatures is reduced.
Preferably, the amphoteric surfactant is one or more of amino acid amphoteric surfactants and betaine amphoteric surfactants; further preferably, the surfactant is a betaine amphoteric surfactant.
Preferably, the betaine amphoteric surfactant is one or more of dodecyl dimethyl hydroxypropyl sulfobetaine, cocamidopropyl hydroxy sulfobetaine, tetradecanamopropyl hydroxypropyl sulfobetaine, cocamidopropyl betaine, lauryl betaine, dodecyl ethoxy sulfobetaine and dodecyl dimethyl sulfopropyl betaine; further preferably, the compound is any one of cocamidopropyl hydroxysultaine, cocamidopropyl betaine, and lauryl betaine.
Preferably, the amino acid compound is one or more of sarcosine, glycine, glutamic acid, methyltaurine and alanine; further preferably, sarcosine.
Preferably, the weight ratio of the amino acid compound to the betaine amphoteric surfactant is (2-10): (0.01-1); further preferably (10-20): 1; further, 15.
In some preferable schemes, sodium laureth sulfate is selected as an anionic surfactant and applied to shampoo, so that the effects of foaming, decontaminating and emulsifying can be achieved well, the grease on the scalp can be removed, but the scalp can be stimulated, the symptoms such as itching and sensitivity of the scalp can be caused, and even alopecia can be caused in severe cases. The applicant finds that sarcosine is selected as an amino acid compound and a specific betaine amphoteric surfactant, and the weight ratio of the amino acid compound to the betaine amphoteric surfactant is (2-10): (0.01-1), the shampoo can improve the richness of foam, thereby increasing the effects of decontamination and oil removal, reducing the stimulation to scalp, and reducing the phenomena of itching and alopecia, etc., and can reduce the degreasing force, avoid the condition that hair is dry and knotted after washing the hair, and also has certain antibacterial property.
Preferably, the conditioner is one or more of hydroxypropyl guar hydroxypropyl trimethyl ammonium chloride, polyquaternium-47, polyquaternium-10, polyquaternium-39 and polyquaternium-7; further preferred are hydroxypropyl guar hydroxypropyl trimonium chloride and polyquaternium-47.
Preferably, the weight ratio of the hydroxypropyl guar hydroxypropyl trimethyl ammonium chloride to the polyquaternium-47 is (1-5): (1-30); further preferably, the ratio is 1.
The applicant unexpectedly found that the weight ratio of (1-5): (1-30) hydroxypropyl guar hydroxypropyl trimonium chloride and polyquaternium-47 are used as conditioners, so that silky feeling and wet hair combing performance of the shampoo in flushing can be improved, and dry feeling and easiness in combing performance of the hair after the hair is dried can be improved. The cationic polymer film is formed by combining hydroxypropyl guar hydroxypropyl trimethyl ammonium chloride and polyquaternium-47, and then the quaternary ammonium groups with positive charges can be adsorbed on the surface of hair to form the cationic polymer film, so that the cationic polymer film has the effects of improving the hair quality, the combing property and the softness, and further the brittle fracture and the falling of the hair are reduced, and on the other hand, effective substances can be remained on the hair, the tangling and the drying of the hair are reduced, and the glossiness and the nutrition of the hair are improved.
Preferably, the chelating agent is disodium EDTA.
Preferably, the plant extract and its derivatives are one or more of cacumen Platycladi extract, ginger root oil, polygoni Multiflori radix extract, radix Angelicae sinensis extract, scutellariae radix extract, and Gleditsia sinensis root extract; more preferably, it is cacumen Platycladi extract and ginger root oil.
Preferably, the weight ratio of the cacumen biotae extract to the ginger root oil is (0.1-10): (0.01-1); further preferably (5-15): 1; further, 10.
The applicant has unexpectedly found that the weight ratio of (0.1-10): (0.01-1) the cacumen biotae extract and the ginger root oil can improve the bacteriostatic effect and reduce alopecia. The reason is probably that the compounding effect of the cacumen biotae extract and the ginger root oil can stimulate hair follicles and promote the growth and development of hairs so as to thicken the hairs, and can prevent alopecia, reduce symptoms such as alopecia areata and premature graying of hairs and realize healthy and thick hairs under double ducts. The ginger root oil also has a certain sterilization and deoiling effect, can effectively clean garbage and grease accumulated on the scalp, and increases the refreshing feeling after the shampoo is used, but the ginger root can have certain irritation on eyes, and the plant extract has lower stability in a system.
Preferably, the emulsifier is one or more of avocado oil PEG-11 esters, PEG-100 stearate, polysorbate-60, cetearyl glucoside, glyceryl stearate, sodium stearoyl lactylate and stearyl alcohol polyether-2; more preferably, the avocado oil PEG-11 ester is used.
In some preferable schemes, a certain amount of avocado oil PEG-11 esters are selected as the emulsifier, so that on one hand, the stability of the shampoo can be improved, and on the other hand, the irritation of other components in the formula can be reduced, so that the prepared shampoo not only has high cleaning power, but also has high stability, can resist allergy, reduces irritation, and is particularly suitable for sensitive people.
Preferably, the zinc compound is one or more of zinc pyrrolidone carboxylate (PCA zinc), zinc lactate, zinc chloride, zinc pyrithione and zinc gluconate; further preferred are zinc PCA and zinc lactate.
Preferably, the weight ratio of the PCA zinc and the zinc lactate is (1-2): (1-2); more preferably, it is 1:1.
In some preferred schemes, the weight ratio of (1-2): the zinc PCA and the zinc lactate in the formula (1-2) are used as zinc compounds, so that the bacteriostatic effect of the shampoo can be improved, and the scalp barrier health can be maintained. The reason is probably that zinc element in zinc PCA and zinc lactate has certain antibacterial and anti-inflammatory effects, can inhibit sebum secretion excessive grease and scalp bacteria propagation, pyrrolidone carboxylic acid in the zinc PCA can also combine moisture to keep the moisture content and barrier health of scalp skin, and in addition, the zinc lactate can also promote the solubility of the zinc PCA in a system, so that the antibacterial and oil-controlling effects of the zinc PCA and the zinc lactate are further improved.
Preferably, the pH regulator is one or more of malic acid, citric acid, triethylamine, sodium bicarbonate, oxalic acid and succinic acid; further preferably, citric acid.
Preferably, the preservative is any one of phenoxyethanol, benzyl alcohol, sodium benzoate and chlorphenesin.
The invention provides a preparation method of an anti-hair loss and oil control silicone-oil-free shampoo, which comprises the following steps: mixing the raw materials uniformly to obtain the product.
Preferably, the preparation method of the anti-hair loss and oil control silicone-oil-free shampoo comprises the following steps:
s1, adding deionized water and hydroxypropyl guar hydroxypropyl trimethyl ammonium chloride, stirring for 1-3 minutes, adding EDTA disodium, and stirring until the EDTA disodium is completely dissolved;
s2, adding sodium laureth sulfate, cocamidopropyl hydroxysultaine/cocamidopropyl betaine/lauryl betaine, and stirring for 10-30 minutes until the raw materials are completely dissolved;
s3, adding avocado oil PEG-11 esters, cacumen biotae extract, sarcosine, ginger root oil, PCA zinc, zinc lactate, polyquaternium-47 and preservative, and stirring for 10-30 minutes until the raw materials are completely dissolved;
and S4, adding citric acid to adjust the pH value, and adding cocoamide methyl MEA to adjust the consistency to obtain the oil-water retention agent.
Has the advantages that:
1. sarcosine is selected as an amino acid compound and a specific betaine amphoteric surfactant, and the weight ratio of the amino acid compound to the betaine amphoteric surfactant is (2-10): (0.01-1), the shampoo can improve the richness of foam, thereby increasing the effects of decontamination and oil removal, reducing the stimulation to scalp, and reducing the phenomena of itching and alopecia, etc., and can reduce the degreasing force, avoid the condition that hair is dry and knotted after washing the hair, and also has certain antibacterial property.
2. The method comprises the following steps of selecting cocoamide methyl MEA as a nonionic surfactant, wherein the weight ratio of the ionic surfactant to the nonionic surfactant to the amphoteric surfactant is (30-40): (2-10): 1, the stability of the shampoo can be improved while the richness and the fineness of the foam are further improved.
3. Selecting the components in the weight ratio of (1-2): the zinc PCA and the zinc lactate in the formula (1-2) are used as zinc compounds, so that the bacteriostatic effect of the shampoo can be improved, and the scalp barrier health can be maintained.
4. Selecting the following components in percentage by weight (0.1-10): (0.01-1) the cacumen biotae extract and the ginger root oil can improve the bacteriostatic effect and reduce alopecia.
5. Selecting the components in the weight ratio of (1-5): (1-30) hydroxypropyl guar hydroxypropyl trimonium chloride and polyquaternium-47 are used as conditioners, so that silky feeling and wet hair combing performance of the shampoo in flushing can be improved, and dry feeling and easiness in combing performance of the hair after the hair is dried can be improved.
6. By selecting a certain amount of avocado oil PEG-11 esters as the emulsifier, on one hand, the stability of the shampoo can be improved, and on the other hand, the irritation of other components in the formula can be reduced, so that the prepared shampoo not only has high cleaning power, but also has high stability, can resist allergy, reduces irritation, and is particularly suitable for sensitive people.
7. The invention can achieve long-acting oil control for 7 days by compounding the functional components such as the surfactant, the amino acid compound, the conditioner, the plant extract and the derivatives thereof, the zinc compound and the like, and can protect the micro-ecological environment of the scalp while improving the oil control capability of the product.
8. The invention emphasizes the anti-dropping and oil-controlling effects of the product and simultaneously considers the softness of the product, thereby improving the use comfort of the product.
9. The anti-hair loss and oil control silicone-free shampoo prepared by the invention is suitable for various hair qualities, such as easily-oiled hair quality, dry hair quality, damaged hair quality, split hair quality and the like.
Drawings
Fig. 1 shows the use feeling test data of 34 consumers who used the shampoo prepared in example 1 of the present application.
Detailed Description
Examples
Example 1
Embodiment 1 provides an anti-hair loss and oil control silicone-free shampoo, which comprises the following components in percentage by weight: 19.5% of surfactant, 7.5% of amino acid compound, 2.2% of conditioner, 0.05% of chelating agent, 5.5% of plant extract and derivatives thereof, 1% of emulsifier, 2% of zinc compound, 0.05% of pH regulator, 0.005% of preservative and water to make up the balance to 100%.
The surfactant is ionic surfactant, nonionic surfactant and amphoteric surfactant.
The weight ratio of the ionic surfactant to the nonionic surfactant to the amphoteric surfactant is 32.
The ionic surfactant is an anionic surfactant.
The anionic surfactant is sodium laureth sulfate.
The sodium laureth sulfate was purchased from Onwei Kogyo, guangdong.
The nonionic surfactant is cocamide methyl MEA.
The cocamide methyl MEA was purchased from kemei oleochemical co ltd, zhongshan.
The amphoteric surfactant is betaine amphoteric surfactant.
The betaine amphoteric surfactant is cocamidopropyl hydroxysultaine.
The cocamidopropyl hydroxysultaine was purchased from Guangzhou florist Fine chemical Co.
The amino acid compound is sarcosine.
The sarcosine was purchased from basf new materials, inc.
The conditioner is hydroxypropyl guar hydroxypropyl trimethyl ammonium chloride and polyquaternium-47.
The weight ratio of the hydroxypropyl guar hydroxypropyl trimethyl ammonium chloride to the polyquaternium-47 is 1.
The hydroxypropyl guar hydroxypropyl trimonium chloride was purchased from RHODIA oper rates.
The polyquaternium-47 is purchased from Kyoho scientific research center, inc.
The chelating agent is disodium EDTA.
The disodium EDTA was purchased from Akzo Nobel Chemicals.
The plant extract and its derivatives are folium Platycladi extract and ginger root oil.
The weight ratio of the cacumen biotae extract to the ginger root oil is 10.
The cacumen biotae extract was purchased from the bergamot green extract biotechnology limited.
The ginger root oil was purchased from sienna green biotechnology limited.
The emulsifier is avocado oil PEG-11 esters.
The avocado oil PEG-11 esters are purchased from RES PHARMA INDUSTRIALE SRL.
The zinc compounds are PCA zinc and zinc lactate.
The weight ratio of zinc PCA to zinc lactate is 1:1.
The zinc PCA was purchased from Xiantting, inc.
The zinc lactate was purchased from cobion, pecan.
The pH regulator is citric acid.
The citric acid purchase was from Weifang Yinxuan industry Co., ltd.
The preservative is sodium benzoate.
The invention provides a preparation method of an anti-hair loss and oil control silicone-oil-free shampoo, which comprises the following steps:
s1, adding deionized water and hydroxypropyl guar hydroxypropyl trimethyl ammonium chloride, stirring for 2 minutes, adding EDTA disodium, and stirring until the EDTA disodium is completely dissolved;
s2, adding sodium laureth sulfate and cocamidopropyl hydroxysultaine, and stirring for 20 minutes until the raw materials are completely dissolved;
s3, adding avocado oil PEG-11 esters, cacumen biotae extract, sarcosine, ginger root oil, PCA zinc, zinc lactate, polyquaternium-47 and sodium benzoate, and stirring for 20 minutes until the raw materials are completely dissolved;
and S4, adding citric acid to adjust the pH value, and adding cocoamide methyl MEA to adjust the consistency to obtain the oil-water retention agent.
Example 2
Embodiment 2 provides an anti-hair loss and oil control silicone-oil-free shampoo, and the specific implementation manner is the same as that of embodiment 1, except that: the betaine amphoteric surfactant is cocamidopropyl betaine.
The cocamidopropyl betaine was purchased from kemei oleochemistry ltd, zhongshan.
Example 3
Embodiment 3 provides an anti-hair loss and oil control silicone-oil-free shampoo, and the specific implementation manner is the same as that of embodiment 1, except that: the betaine amphoteric surfactant is lauryl betaine.
The lauryl betaine was purchased from the Guangzhou Tiancigao New materials GmbH.
Comparative example 1
Comparative example 1 provides an anti-hair loss and oil control silicone-free shampoo, and the specific implementation manner is the same as that of example 1, and the differences are that: the surfactant is ionic surfactant and nonionic surfactant.
The weight ratio of the ionic surfactant to the nonionic surfactant is 16.
Comparative example 2
Comparative example 2 provides an anti-hair loss and oil control silicone-free shampoo, and the specific implementation manner is the same as that of example 1, except that: comprises the following components in percentage by weight: 19.5% of surfactant, 2.2% of conditioner, 0.05% of chelating agent, 5.5% of plant extract and derivatives thereof, 1% of emulsifier, 2% of zinc compound, 0.05% of pH regulator, 0.005% of preservative and water to make up the balance to 100%.
The surfactant is ionic surfactant and nonionic surfactant.
The weight ratio of the ionic surfactant to the nonionic surfactant is 16.
Comparative example 3
Comparative example 3 provides an anti-hair loss and oil control silicone-oil-free shampoo, and the specific implementation manner is the same as that of example 1, and the differences are that: the zinc compound is PCA zinc.
Comparative example 4
Comparative example 4 provides an anti-hair loss and oil control silicone-oil-free shampoo, and the specific implementation manner is the same as that of example 1, and the differences are that: the plant extract and its derivatives are cacumen Platycladi extract.
Comparative example 5
Comparative example 5 provides an anti-hair loss and oil control silicone-free shampoo, and the specific implementation manner is the same as that of example 1, except that: comprises the following components in percentage by weight: 19.5% of surfactant, 7.5% of amino acid compound, 2.2% of conditioner, 0.05% of chelating agent, 5.5% of plant extract and derivatives thereof, 0.01% of emulsifier, 2% of zinc compound, 0.05% of pH regulator, 0.005% of preservative and water to make up the balance to 100%.
Performance test method
1. Stability of
The stability of the products of examples 1-3 and comparative examples 1-5 is respectively tested from two dimensions of appearance and aroma, the products are respectively placed in six environments of 48 ℃, 5 ℃, 18-48 ℃, normal temperature (25 ℃) and illumination (under natural light) to test the stability, the one-time test time is 24h, wherein the high-low temperature cycle test of-18-48 ℃ is 12h after 12h at-18 ℃. The cycle was repeated 7 times and compared with the initial state, and the results are shown in tables 1 to 8.
2. Usage sensing test
By making a trial survey of consumers (34) on the product, evaluation tests were conducted on consumers in terms of the degree of foam richness, fresh and non-dry scalp, smooth and supple hair, easy rinsing, wet combing, dry combing, natural refreshing and non-greasy hair, improvement of scalp frizz, reduction of oil output of scalp, improvement of dandruff, recognition of oil control efficacy of the product, recognition of hair loss prevention efficacy of the product, and comparison of the degree of foam richness after use of the shampoo prepared in example 1, and the scores in this respect were: the number of people/34 x 100% of this advantage was selected, and the results are shown in figure 1.
3. Testing oil control ability of product
Selecting 30 volunteers aged 25-55 years, using the shampoo prepared in the embodiment 1 for the first half of a single time, washing hair at the other side of the shampoo as a control, testing the scalp oil content before, 4h after, 8h after and 24h after use by using a scalp oil tester, and evaluating the 24h instant oil control effect of the product; the samples were then used daily and after 7 days of use the scalp oil content was tested and the product was evaluated for long-lasting oil control efficacy for 7 days, with the results shown in tables 9 and 10.
Table 1 stability results for example 1
Table 2 stability results for example 2
Table 3 stability results for example 3
Table 4 stability results for comparative example 1
Table 5 stability results for comparative example 2
Table 6 stability results for comparative example 3
Table 7 stability results for comparative example 4
Table 8 stability results for comparative example 5
Table 9 scalp oil content descriptive statistics (n = 30)
Table 10 scalp oil content statistical analysis results (n = 30)
Note: 1. the statistical method comprises the following steps: analyzing by using a t-test method, and testing the standard level alpha =0.05
2. The significance labeling method comprises the following steps: "n.s." means p.gtoreq.0.05 with no statistical difference; p < 0.05, indicating a statistical difference (") indicates 0.01. Ltoreq. P < 0.05;" "indicates 0.001. Ltoreq. P < 0.01;". Indicates p < 0.001).
Claims (10)
1. The anti-hair loss and oil control silicone-free shampoo is characterized by comprising the following components in percentage by weight: 12-25% of surfactant, 5-10% of amino acid compound, 0.2-3.5% of conditioner, 0.01-0.2% of chelating agent, 0.1-11% of plant extract and derivatives thereof, 0.05-2% of emulsifier, 0.02-4% of zinc compound, 0.01-0.2% of pH regulator, 0.001-0.01% of preservative and the balance of water to 100%.
2. The anti-hair loss and oil control silicone-free shampoo as defined in claim 1, wherein the surfactant comprises one or more of an ionic surfactant, a nonionic surfactant, an amphoteric surfactant and a built surfactant.
3. The shampoo according to claim 2, wherein the ionic surfactant is one or two of an anionic surfactant and a cationic surfactant.
4. The anti-hair loss and oil control silicone-free shampoo as defined in claim 2, wherein the amphoteric surfactant is one or more of an amino acid amphoteric surfactant and a betaine amphoteric surfactant.
5. The anti-hair loss and oil control silicone-free shampoo according to claim 4, wherein the amino acid compound is one or more of sarcosine, glycine, glutamic acid, methyl taurine and alanine.
6. The anti-hair loss and oil control silicone-free shampoo as defined in claim 4 or 5, wherein the betaine amphoteric surfactant is one or more of dodecyl dimethyl hydroxypropyl sulfobetaine, cocamidopropyl hydroxysulfobetaine, tetradecylamidopropyl hydroxypropyl sulfobetaine, cocamidopropyl betaine, lauryl betaine, dodecyl ethoxy sulfobetaine and dodecyl dimethyl sulfopropyl betaine.
7. The anti-hair loss and oil control silicone-free shampoo according to any one of claims 1-6, wherein the conditioner is one or more of hydroxypropyl guar hydroxypropyl trimonium chloride, polyquaternium-47, polyquaternium-10, polyquaternium-39 and polyquaternium-7.
8. The shampoo with hair loss prevention and oil control and no silicone oil as claimed in claim 7, wherein the plant extract and the derivatives thereof are one or more of cacumen biotae extract, ginger root oil, polygonum multiflorum extract, angelica sinensis root extract, scutellaria baicalensis root extract and gleditsia sinensis root extract.
9. The anti-hair loss and oil control silicone-free shampoo according to claim 8, wherein the zinc compound is one or more of zinc pyrrolidone carboxylate, zinc lactate, zinc chloride, zinc pyrithione and zinc gluconate.
10. The preparation method of the anti-hair loss and oil control silicone-free shampoo according to any one of claims 1 to 9, characterized by comprising the following steps of:
mixing the raw materials uniformly to obtain the product.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210828320.0A CN115487127A (en) | 2022-07-13 | 2022-07-13 | Anti-hair loss oil-control silicone-oil-free shampoo and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210828320.0A CN115487127A (en) | 2022-07-13 | 2022-07-13 | Anti-hair loss oil-control silicone-oil-free shampoo and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN115487127A true CN115487127A (en) | 2022-12-20 |
Family
ID=84467419
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202210828320.0A Pending CN115487127A (en) | 2022-07-13 | 2022-07-13 | Anti-hair loss oil-control silicone-oil-free shampoo and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN115487127A (en) |
Citations (18)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10354116A1 (en) * | 2003-11-19 | 2005-06-23 | Beiersdorf Ag | Silicone-free formulation, used for cleaning keratin structures, especially human hair; contains lauryl ether sulfate, cocamidopropyl betaine and 2 nonionic surfactants with different specified hydrophilic lipophilic balance values |
JP2007001889A (en) * | 2005-06-22 | 2007-01-11 | Mandom Corp | Shampoo composition |
CN101947195A (en) * | 2010-10-13 | 2011-01-19 | 广州温雅日用化妆品有限公司 | Foaming agent shampoo |
CN105748376A (en) * | 2016-04-26 | 2016-07-13 | 成都彦宁科技有限公司 | Oil-control anti-hair-loss liquid shampoo |
CN105796415A (en) * | 2016-03-22 | 2016-07-27 | 广东嘉丹婷日用品有限公司 | Hair care composition with oil control and dandruff removal effects |
CN105796407A (en) * | 2016-03-16 | 2016-07-27 | 千草万木(北京)科技有限公司 | Plant extract composition, application of plant extract composition in cosmetics, shampoo composition and preparing method of shampoo composition |
CN106619277A (en) * | 2016-11-15 | 2017-05-10 | 东莞自然衡健康科技有限公司 | Silicone oil-free grease control anti-hair loss shampoo |
CN107737039A (en) * | 2017-11-15 | 2018-02-27 | 广州无与伦比企业集团有限公司 | Containing ginger without silicone oil without sulfate health-care shampoo and its preparation technology |
CN107854331A (en) * | 2017-11-21 | 2018-03-30 | 彭钦龙 | One kind is without silicone oil shampoo |
CN107913228A (en) * | 2017-11-15 | 2018-04-17 | 广州无与伦比企业集团有限公司 | Containing ginger without silicone oil health-care shampoo and its preparation process |
CN109498494A (en) * | 2018-12-26 | 2019-03-22 | 广州蜜妆生物科技有限公司 | A kind of salubrious oil-control is without silicone oil shampoo and preparation method thereof |
CN109793681A (en) * | 2018-12-26 | 2019-05-24 | 拉芳家化股份有限公司 | It is a kind of containing educating the shampoo composite for sending out hair loss composite reactive Essence anti- |
CN111012730A (en) * | 2019-12-02 | 2020-04-17 | 广州妮趣化妆品有限公司 | Composition for regulating scalp microecology |
CN112402275A (en) * | 2020-12-04 | 2021-02-26 | 上海怡宝化妆品集团有限公司 | Organic zinc compound oil-control anti-dandruff shampoo and preparation method thereof |
CN113908095A (en) * | 2021-11-09 | 2022-01-11 | 上海蜂花日用品有限公司 | Oil-control moisturizing hair composition containing double proteins |
CN114146012A (en) * | 2021-07-30 | 2022-03-08 | 广东嘉丹婷日用品有限公司 | Antibacterial and anti-dandruff shampoo and preparation method thereof |
CN114159330A (en) * | 2021-07-30 | 2022-03-11 | 广东嘉丹婷日用品有限公司 | Oil-control and dandruff-removing hair care composition and preparation method thereof |
CN114376957A (en) * | 2022-01-13 | 2022-04-22 | 广东星芮生物科技有限公司 | Scalp-maintaining, tough and anti-hair-loss double-repairing shampoo and preparation method thereof |
-
2022
- 2022-07-13 CN CN202210828320.0A patent/CN115487127A/en active Pending
Patent Citations (18)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10354116A1 (en) * | 2003-11-19 | 2005-06-23 | Beiersdorf Ag | Silicone-free formulation, used for cleaning keratin structures, especially human hair; contains lauryl ether sulfate, cocamidopropyl betaine and 2 nonionic surfactants with different specified hydrophilic lipophilic balance values |
JP2007001889A (en) * | 2005-06-22 | 2007-01-11 | Mandom Corp | Shampoo composition |
CN101947195A (en) * | 2010-10-13 | 2011-01-19 | 广州温雅日用化妆品有限公司 | Foaming agent shampoo |
CN105796407A (en) * | 2016-03-16 | 2016-07-27 | 千草万木(北京)科技有限公司 | Plant extract composition, application of plant extract composition in cosmetics, shampoo composition and preparing method of shampoo composition |
CN105796415A (en) * | 2016-03-22 | 2016-07-27 | 广东嘉丹婷日用品有限公司 | Hair care composition with oil control and dandruff removal effects |
CN105748376A (en) * | 2016-04-26 | 2016-07-13 | 成都彦宁科技有限公司 | Oil-control anti-hair-loss liquid shampoo |
CN106619277A (en) * | 2016-11-15 | 2017-05-10 | 东莞自然衡健康科技有限公司 | Silicone oil-free grease control anti-hair loss shampoo |
CN107913228A (en) * | 2017-11-15 | 2018-04-17 | 广州无与伦比企业集团有限公司 | Containing ginger without silicone oil health-care shampoo and its preparation process |
CN107737039A (en) * | 2017-11-15 | 2018-02-27 | 广州无与伦比企业集团有限公司 | Containing ginger without silicone oil without sulfate health-care shampoo and its preparation technology |
CN107854331A (en) * | 2017-11-21 | 2018-03-30 | 彭钦龙 | One kind is without silicone oil shampoo |
CN109498494A (en) * | 2018-12-26 | 2019-03-22 | 广州蜜妆生物科技有限公司 | A kind of salubrious oil-control is without silicone oil shampoo and preparation method thereof |
CN109793681A (en) * | 2018-12-26 | 2019-05-24 | 拉芳家化股份有限公司 | It is a kind of containing educating the shampoo composite for sending out hair loss composite reactive Essence anti- |
CN111012730A (en) * | 2019-12-02 | 2020-04-17 | 广州妮趣化妆品有限公司 | Composition for regulating scalp microecology |
CN112402275A (en) * | 2020-12-04 | 2021-02-26 | 上海怡宝化妆品集团有限公司 | Organic zinc compound oil-control anti-dandruff shampoo and preparation method thereof |
CN114146012A (en) * | 2021-07-30 | 2022-03-08 | 广东嘉丹婷日用品有限公司 | Antibacterial and anti-dandruff shampoo and preparation method thereof |
CN114159330A (en) * | 2021-07-30 | 2022-03-11 | 广东嘉丹婷日用品有限公司 | Oil-control and dandruff-removing hair care composition and preparation method thereof |
CN113908095A (en) * | 2021-11-09 | 2022-01-11 | 上海蜂花日用品有限公司 | Oil-control moisturizing hair composition containing double proteins |
CN114376957A (en) * | 2022-01-13 | 2022-04-22 | 广东星芮生物科技有限公司 | Scalp-maintaining, tough and anti-hair-loss double-repairing shampoo and preparation method thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
EP3403642B1 (en) | Cosmetic | |
US7977290B1 (en) | Body cleansing composition | |
CN107496317B (en) | Repairing and nursing shampoo containing periplaneta americana active ingredient | |
CN113332191A (en) | Shampoo and preparation method thereof | |
RU2116065C1 (en) | Cosmetic detergent composition for hair | |
US10420962B2 (en) | Organic hair formulation and treatment | |
CN108771645B (en) | Quinoa shampoo and preparation method thereof | |
WO2016139125A1 (en) | Cosmetic agent with bioactive substance and a dipeptide | |
KR100834891B1 (en) | Hair treatment composition including ink extracts of cephalopoda | |
CN108158921B (en) | Plant composition containing tea bran and rosemary as well as preparation method and application of plant composition | |
EP0662815A1 (en) | Hair-care agent. | |
CN115444766B (en) | Bi-component shampoo with scalp nourishing effect and preparation method thereof | |
CN115487127A (en) | Anti-hair loss oil-control silicone-oil-free shampoo and preparation method thereof | |
CN117083051A (en) | Novel topical compositions free of sulphate-derived surfactants | |
CN113648261A (en) | Ginger shampoo with scalp care effect and preparation method thereof | |
CN114306197A (en) | Bubble hair conditioner | |
CN108524343B (en) | Composition for nourishing scalp and caring hair, and preparation method and application thereof | |
KR20150146011A (en) | Cosmetic composition for preventing hair damage | |
CN114159327A (en) | Mild hair-care type infant shampoo and preparation method thereof | |
CN113633597A (en) | Shampoo with plant fermentation extracted components and preparation method thereof | |
JPS62289509A (en) | Hair cosmetic | |
CN117898968B (en) | Collagen shampoo with sun-screening, anti-dandruff and repairing functions and preparation method thereof | |
CN114767575B (en) | Fluffy shampoo composition | |
KR102399544B1 (en) | Composition for cleaning hair and scalp enhancing scrub function through salt | |
KR102569171B1 (en) | Hair tone up shampoo composition, Hair tone up shampoo using the same and Manufacturing method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |