CN115400033A

CN115400033A - Microcapsule shell material and microcapsule preparation method

Info

Publication number: CN115400033A
Application number: CN202211041828.2A
Authority: CN
Inventors: 袁彦洁; 李芸娇
Original assignee: Chongqing Xiaowan Biotechnology Co ltd
Current assignee: Chongqing Xiaowan Biotechnology Co ltd
Priority date: 2022-08-29
Filing date: 2022-08-29
Publication date: 2022-11-29
Also published as: WO2024045003A1

Abstract

The invention discloses a microcapsule shell material and a microcapsule preparation method. The microcapsule shell material comprises the following components in percentage by weight: 0-50% of higher fatty alcohol or polyethylene glycol, 10-60% of grease or wax, 0-20% of oil thickener and the balance of emulsifier. The melting point of the shell material of the microcapsule is higher than 50 ℃, and the shell material is solid at the temperature of different climates; it has no sign of melting, softening, separating out liquid oil and the like; can swell and soften by absorbing water in water, but does not dissolve or disintegrate in water. Under the action of pressure, the coating can be easily spread to release the coated substance, and the coated core material can be solid or liquid. The invention solves the problem that the microcapsule prepared by using a single melting shell material in the prior art can not simultaneously meet the special technical requirements of daily chemicals on melting point, hardness, high-temperature stability, release, skin feel and the like.

Description

Microcapsule shell material and microcapsule preparation method

Technical Field

The invention belongs to the technical field of daily chemical articles, and particularly relates to a wall material of a microcapsule and a method for preparing the microcapsule by using the wall material through a melting, dispersing and condensing method.

Background

In the field of cosmetics, many active substances having an effect on the skin cannot stably exist in an environment such as water, air, ultraviolet rays, etc., and many ingredients in cosmetics, such as water, oil, a surfactant, an acid-base regulator, a chelating agent, etc., are also liable to undergo a compatible reaction with the active substance to inactivate the active substance, and cannot produce a corresponding effect. It is therefore necessary to encapsulate these active ingredients in a manner that improves their stability during storage and yet allows them to be rapidly released on the skin at the time of use.

Microcapsules (microcapsules) refer to a micro-container or wrap having a polymeric or inorganic wall. Microencapsulation (Microencapsulation) is a technique in which an active substance in a solid, liquid or gaseous state is encapsulated by a material. The microcapsule technology can cover the bad taste and smell of the coated substance, control the release speed and mode of the active substance, improve the matching degree of the active substance and the environment, reduce incompatibility, isolate factors such as oxygen, water and the like which have influences on the stability of the active substance. Microcapsule technology has been used for many years in many industrial areas and by many methods such as pan coating processes, spray drying, spray freezing, fluidized bed, orifice methods, interfacial polymerization, in situ polymerization, and the like.

One of the microencapsulation techniques is the melt dispersion condensation method. The method utilizes a material which has a low softening point and can be melted, such as a wax-like substance, a polymer solution and the like, as a microcapsule shell material. When the substances are heated, the substances soften and become liquid, and the coated core materials are dispersed into the substances to form uniform dispersion liquid; when the system cools, a solid shell forms around the core. The melting dispersion condensation method is to realize microencapsulation by utilizing the unique properties of a hot melting material when being heated and condensed, and the method can be used for condensing microencapsulation in a liquid medium and also can be used for condensing microencapsulation in a gaseous medium. When the melting dispersion method is used for preparing the microcapsule, the microcapsule has the advantages of no solvent, effective light shielding, high wrapping speed and high efficiency, and has very high practical value.

The melting, dispersing and condensing method is used to prepare the microcapsule, and the used wrapping material usually adopts the inert substances with non-solvent property, high thermal stability and low reaction activity. Solid oil, wax, fatty acid, fatty alcohol and solid surfactant are all very common ingredients in cosmetics, and are also good hot-melt shell raw materials which can be used in a melting, dispersing and condensing method. However, the common hot-melt materials, such as grease, wax, fatty acid and fatty alcohol, have a problem of selecting a melting point. Generally, the melting point of a hot melt in daily chemicals is lower than 35 ℃ of the surface of skin so that the hot melt can be easily spread, but the hot melt material with the melting point lower than 50 ℃ is unstable and is easily melted to be liquid at high temperature in summer so that the microcapsules are damaged. Whereas hot melt materials with a melting point above 50 ℃ generally do not soften the skin, are too hard to spread by pressure and body surface temperature and therefore do not release the active.

Although there are also some hot melt materials with melting points above 50 c, such as polyethylene glycol with a degree of polymerization above 4000. However, polyethylene glycol 4000-6000 is readily soluble in water and dissolves in water as a wrapping material, resulting in disintegration of the microcapsules, and most cosmetics contain water. Polyethylene glycol with a polymerization degree higher than 6000 is not easy to dissolve in water, but has too high hardness to be smeared on the skin, and has the problem that active substances are difficult to release. Polyethylene glycol also presents skin safety issues and european legislation has limited the use of polyethylene glycol. In addition, liquid polyethylene glycols such as PEG-4 and PEG-100 are easily absorbed by the skin, have been shown to lower blood pressure, and components are not easily decomposed and easily accumulated in the liver, and the smaller the number, the more easily chemical components are absorbed by the skin, the more harmful the chemical components are. In addition, the by-product pollutants in the production of PEG comprise carcinogen 1,4-dioxane (1,4-dioxane), polycyclic aromatic compounds, heavy metals of lead, iron, cobalt, nickel, cadmium, arsenic and the like.

Disclosure of Invention

Aiming at the defects in the prior art, the invention aims to provide a microcapsule shell material, which solves the technical problem that the melting point, water solubility and hardness of the common microcapsule shell material in the prior art cannot simultaneously meet the requirement of a melting, dispersing and condensing method for preparing microcapsules.

Furthermore, the invention also provides a method for preparing the microcapsule by using the microcapsule shell material.

In order to solve the technical problems, the invention adopts the following technical scheme:

a microcapsule shell material, the shell material having a melting point above 50 ℃ and being solid at temperatures of different climates. Can absorb water to swell and soften in water, but does not dissolve or disintegrate in water; under the action of pressure, the coating can be easily spread to release the coated substance, and the coated core material can be solid or liquid.

Further, the microcapsule shell material comprises the following core components in percentage by weight: 0-50% of higher fatty alcohol or polyethylene glycol, 10-60% of grease or wax, 0-20% of oil thickening agent and the balance of emulsifier.

Further, the shell material also comprises 0-50% of fat-soluble pigment or inorganic color lake according to weight percentage. Wherein the pigment lakes are synthetic or natural organic pigments or organic lakes; the lake refers to inorganic lake.

Further, the emulsifier is a nonionic emulsifier, an anionic emulsifier, a cationic emulsifier or a zwitterionic emulsifier; nonionic emulsifiers are preferred.

Further, the oil or wax is any one of vegetable oil ester and vegetable wax, animal oil and fat, synthetic oil and synthetic wax, silicone oil and silicone wax.

Further, the higher aliphatic alcohol refers to a higher alcohol having a melting point of more than 30 degrees; higher alcohols with a carbon number greater than 14 are typically used.

Further, the polyethylene glycol { PEG } refers to solid polyethylene glycol with a molecular weight of more than 1000 and a freezing point of more than 25 ℃.

Further, the oil thickener is a polymer thickener or a solid powder thickener dissolved in oil.

Further, the emulsifier is preferably a solid emulsifier having a melting point higher than 30 ℃, and the HLB value of the emulsifier is between 3 and 13.

Further, the nonionic emulsifier comprises: alcohol nonionic emulsifiers, polyoxyethylene nonionic emulsifiers, nitrogen-containing nonionic emulsifiers, block polyether type and sterol-derived nonionic emulsifiers.

Further, the alcoholic nonionic emulsifier includes: one or more of glycol esters, glycerides, polyglycerol fatty acid esters, neopentyl polyol esters, sugar esters, sorbitol esters, and alkyl glycoside type nonionic emulsifiers.

Wherein the glycol ester is a nonionic emulsifier generated by the reaction of glycol and fatty acid. The glycerin fatty acid ester is a nonionic emulsifier which is generated by the reaction of glycerin and fatty acid and is monoglyceride, diester or triester. The polyglycerin fatty acid ester emulsifier is a polyhydroxy ester nonionic surfactant formed by polyglycerin and fatty acid. The neopentyl polyol lipid nonionic emulsifier is pentaerythritol fatty acid ester. The sugar ester emulsifier is nonionic emulsifier prepared by esterifying glucose with multiple hydroxyl groups, sucrose and fatty acid such as lauric acid, stearic acid, oleic acid, palmitic acid, etc.; sugar esters can be classified into monoesters, diesters, and triesters, depending on the degree of esterification. The sorbitol esters are partial fatty acid esters (Tween) of polyoxyethylene sorbitan and sorbitan fatty acid ester (span) emulsifiers. The alkyl glycoside is synthesized by glucose and fatty alcohol. The polyoxyethylene type nonionic emulsifier includes: one or more of fatty alcohol-polyoxyethylene ether, fatty acid-polyoxyethylene ester, alkylphenol ethoxylate and polyoxyethylene ammonium fatty acid. The fatty alcohol-polyoxyethylene ether is an ether nonionic emulsifier obtained by adding polyethylene glycol (PEG) and fatty alcohol through ethylene oxide, and the chemical general formula RO (CH 2CH 2O) nH is the most common emulsifier developed at most.

Further, the fatty acid polyoxyethylene ester is generated by the addition reaction of fatty acid and ethylene oxide, and the general formula of the fatty acid polyoxyethylene ester is RCOO (CH 2CH 2O) nH.

The invention also provides a preparation method of the microcapsule, which adopts the microcapsule shell material component and comprises the following preparation steps:

1) Heating the microcapsule shell material to be molten, and fully and uniformly stirring;

2) Adding the core material into the microcapsule shell material and uniformly stirring;

3) Cooling and molding the melted and dispersed liquid obtained in the step 2) in air to obtain the microcapsule with required size, specification and shape.

The cooling method comprises the step of injecting the melted and dispersed liquid into a mold or spreading the liquid on a plane for cooling to obtain the mold-shaped or sheet-shaped wrapper.

Further, the cooling method comprises the steps of dripping or spraying the melted and dispersed liquid into cold air, and cooling the air through a certain distance of drop height to obtain spherical coated microspheres with different specifications

Wherein the core material is water-soluble active substance, fat-soluble active substance or insoluble substance.

The water-soluble active substance is one or more of vitamin B1, B3, B5, B12, vitamin C and its derivatives, ethyl ascorbic acid, tea polyphenols, peptide, amino acid, and plant extract.

The fat-soluble active matter is one or more of vitamin E, vitamin E acetate, vitamin A palmitate, vitamin C palmitate, Q10, carotene, astaxanthin, lutein, ceramide, and phytosphingosine.

The fat-soluble active matter is plant extracted essential oil or essence.

The insoluble substance refers to active substances insoluble in both water and oil, including minerals, probiotics, plant and animal raw powder and/or protein, etc.

The invention also provides another preparation method of the microcapsule, which adopts the microcapsule shell material component and comprises the following steps:

2) And (4) coating the melted shell solution on the wrapped core material in a coil mode, and cooling to obtain the microcapsule.

Wherein the core material is a crystal or a solid particle.

Compared with the prior art, the invention has the following beneficial effects:

1. the melting point of the shell material is above 50 ℃, the shell material can keep a stable solid state in any season, can be softened in a water and oil containing daily chemical product, can not be completely dissolved in water or oil, can be easily spread on skin under the pressure of fingers, and releases the wrapped core material; solves the technical problem that the melting point, water solubility and hardness of the common microcapsule shell material in the prior art can not simultaneously meet the requirements of the melting, dispersing and condensing method for preparing the microcapsule in daily chemicals.

2. The microcapsule shell material of the invention is composed of emulsifier, fatty alcohol, grease or wax, and the like, and uses raw materials which are safely approved by cosmetics, foods and medicines, and the raw materials are nontoxic and environment-friendly and do not harm human health and cause environmental pollution. The microcapsule is a series of hot-melt raw materials, can be prepared by a melting, dispersing and condensing method, and can be kept in a solid state at room temperature without melting, softening and other signs; can absorb water and oil in water to swell and soften, and is insoluble or disintegrated in water and oil. The coated material can be easily spread and released under pressure, and the coated core material can be solid or liquid.

3. The microcapsule preparation method adopts a melting dispersion condensation method, and has the advantages of no solvent, effective light shielding, high packaging speed and high efficiency when the microcapsule is prepared by using the method, and has very high practical value.

4. The microcapsule shell material of the present invention is melted at high temperature, contains no water, has an antibacterial effect due to a large amount of emulsifier, and is stored in a solid state, so that a preservative is not required.

Detailed Description

In order to make those skilled in the art better understand the technical solution of the present invention, the present invention will be further described with reference to the following specific examples, but the embodiments of the present invention are not limited thereto.

The invention provides a microcapsule shell material, wherein the melting point of the shell material after mixing is higher than 50 ℃, and the shell material is solid at temperatures of different climates. The core components of the composite material comprise the following components in percentage by weight: 0-50% of higher fatty alcohol or polyethylene glycol, 10-60% of grease or wax, 0-20% of oil thickener and the balance of emulsifier.

The shell material further contains a fat-soluble pigment or an inorganic lake.

Wherein the emulsifier is a nonionic emulsifier. In fact, the emulsifier may be an anionic emulsifier, a cationic emulsifier, an amphoteric emulsifier, a non-ionic emulsifier or a mixture of several emulsifiers. The nonionic emulsifier is a surfactant which does not ionize ions in any form in an aqueous solution, is not dissociated in the aqueous solution, mainly comprises a certain number of oxygen-containing groups (generally ether groups or hydroxyl groups) on hydrophilic groups, and is dissolved by forming hydrogen bonds with water. The nonionic emulsifier has high stability and is not easily influenced by strong electrolyte, inorganic salt and acid and alkali; the compatibility with other surfactants is good; . Has the advantage of better solubility in both water and organic solvents. Considering the incompatibility with various systems, for example, the problem that anionic emulsifiers cannot be used in cationic hair conditioner systems and the like can generate flocculation and precipitation through electropolymerization reaction, nonionic emulsifiers are generally preferred, so that the emulsifiers have wider applicability.

The nonionic surfactant is an amphiphilic structure compound that does not dissociate into an ionic state in water. The hydrophilic group is mainly composed of polyethylene glycol group, i.e., polyoxyethylene group, and is based on polyhydric alcohol (e.g., glycerin, pentaerythritol, sucrose, glucose, sorbitol, etc.). In addition, the structure based on monoethanolamine and diethanolamine is also provided.

The non-ionic emulsifier comprises: alcohol nonionic emulsifiers, polyoxyethylene nonionic emulsifiers, nitrogen-containing nonionic emulsifiers, block polyether type and sterol-derived nonionic emulsifiers.

Wherein, the alcohol nonionic emulsifier is an ester generated by esterification reaction of polyhydric alcohol containing a plurality of hydroxyl groups and fatty acid; in addition, it also includes the compound with NH ₂ Or NH amino alcohol and saccharide with-CHO group react with fatty acid or ester to obtain non-ionic emulsifier.

The alcohol nonionic emulsifier comprises: one or more of glycol esters, glyceride nonionic emulsifier, polyglycerol fatty acid ester nonionic emulsifier, neopentyl polyol ester nonionic emulsifier, sugar ester nonionic emulsifier, sorbitol esters, and alkyl glycoside nonionic emulsifier.

Wherein, the glyceride nonionic emulsifier is one or more of monoester, diester or triester; the monoester comprises a monoglyceride fatty acid lipid; the monoglyceride fatty acid ester is monoglyceride stearate, monoglyceride palmitate, monoglyceride laurate, glyceryl monoisostearate or monoglyceride distearate.

Wherein, the polyglycerol fatty acid ester is prepared by the reaction of fatty acid and derivatives thereof and polyglycerol, the chemical structure and the physicochemical property of the polyglycerol fatty acid ester are related to the polymerization degree, the fatty acid type and the esterification degree of the polyglycerol, wherein: the degree of polymerization of polyglycerol is generally from 2 to 10; the carbon chain length of the fatty acid is generally 6 to 18, and the carbon chain can be saturated or unsaturated, and can also be straight chain or branched chain; in addition, the esterification degree of the hydroxyl can be monoester, diester, polyester and the like, so that a series of polyglyceryl fatty acid ester emulsifiers with various structures and different properties can be obtained.

The polyglycerol fatty acid ester nonionic emulsifier is one or more of polyglycerol ricinoleate, triglycerol distearate, triglycerol diisostearate, polyglycerol 10 palmitate, polyglycerol 10 myristate, polyglycerol-6 polyricinoleate and polyglycerol-2 dipolyhydroxystearate.

Wherein the neopentyl polyol lipid nonionic emulsifier is pentaerythritol fatty acid ester. The pentaerythritol fatty acid ester is a good cream excipient, can obviously improve the consistency and stability of the product by compounding with monoglyceride, is easy to emulsify, and does not affect the viscosity, foam and stability of the product. The cream containing pentaerythritol distearate is light in texture, easy to absorb and spread, and smooth and soft for skin.

The sugar ester non-ionic emulsifier is sucrose stearate. Glucose, sucrose, etc. all have multiple external hydroxyl groups, and can be esterified with lauric acid, palmitic acid, stearic acid, oleic acid, etc. to obtain sugar esters. Since the saccharide has more hydroxyl groups, it can be esterified into water-soluble products. Most sugar esters are tasteless and odorless, can be completely biodegraded completely, and have no toxicity or irritation to human bodies.

The polyethylene glycol type nonionic emulsifier is a product of addition reaction of ethylene oxide and a compound containing active hydrogen, and belongs to ethers; including higher alcohol ethylene oxide adducts, alkylphenol ethylene oxide adducts, fatty acid ethylene oxide adducts, and higher fatty amide ethylene oxide adducts. Many varieties and large yield, and is a non-ionic large class. The polyethylene glycol type nonionic emulsifier can be classified into long-chain fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, fatty acid polyoxyethylene ester, polyoxyethylene alkylamine, polyoxyethylene alkylamide, polyether and the like according to the type of the hydrophobic group. For example: peg-20 methyl glucose sesquistearate, peg-20 stearate, peg-100 stearate, ceteareth 6, 25, 2, 21 or cetearyl glucoside. .

The higher aliphatic alcohol refers to an aliphatic alcohol having a chain of 12 to 22 carbon atoms and containing twelve or more carbon atoms, and is a waxy solid saturated monohydric alcohol, which is also called a higher alkanol. The higher alkanol has stable property, is not easy to oxidize, is stable under illumination, is acid and alkali resistant, does not absorb moisture, and has good biodegradability and bioactivity; white waxy solid at normal temperature. The higher fatty alcohol moiety has amphiphilic properties, i.e., it has a hydrophobic group such as a hydrocarbon chain and a hydrophilic group such as a hydroxyl group in the molecule.

The fat-soluble pigment or inorganic lake is organic synthetic pigment or lake red 30, blue 1, yellow 5, yellow 6, green 6, etc., and the natural pigment is carotene, lutein, chlorophyll, astaxanthin, lycopene, arnebia oil, curcuma rhizome, gardenia yellow, etc. The inorganic lake is one or more of ultramarine, chromium green, manganese violet, titanium dioxide, mica, carbon black or iron oxide.

The emulsifier is solid and has a melting point above 40 ℃.

The HLB value of the emulsifier is between 3 and 13.

The oil or wax is one or more of hydrogenated vegetable oil, candelilla wax, rice bran wax, palm wax, ceresin, microcrystalline wax, myristyl myristate, lanolin and beeswax. These waxes or greases are generally solid or semi-solid at room temperature, have a melting point above 35 degrees, and the greases and waxes may be of natural origin or synthetic.

The oil thickener is a high molecular polymer dissolved in oil or a solid powder oil phase thickener insoluble in oil. The thickener is used to prevent the precipitation of low-melting oil. The high molecular material dissolved in oil for increasing oil viscosity is one or more of palmitic acid dextrin, castor oil IPDI copolymer, dibutyl ethyl hexanoyl glutamine, dibutyl lauroyl glutamine, hydrogenated styrene/butadiene copolymer, and silicon elastomer. The oil insoluble solid powder oil phase thickener is one or more of silica, hectorite, montmorillonite, bentonite, zeolite, clay, and plant cellulose.

The shell material of the invention can wrap fat-soluble active substances such as vitamin E, vitamin E acetate, vitamin A palmitate, vitamin C palmitate, Q10, carotene, astaxanthin, lutein, ceramide, phytosphingosine, salicylic acid and the like.

The shell material of the invention can wrap one or more of water-soluble active substances of vitamin B1, B3, B5, B12, vitamin C and derivatives thereof, ethyl ascorbic acid, tea polyphenol, peptide, amino acid and plant extract.

The shell material of the invention can wrap the raw powder of water and oil insoluble active substance protein, enzyme, probiotics, mineral substances, plant or animal tissues and the like.

1. The melting point of the microcapsule shell material is higher than 50 ℃, and the microcapsule shell material is solid at different climatic temperatures.

Examples 1 to 18, table 1, the ingredients in weight percent

TABLE 1 composition of microcapsule Shell Material

The melting point of the combined shell material is higher than 50 ℃, the combined shell material can keep solid state at room temperature under different climates, and the signs of melting, softening, separating out liquid oil and the like do not exist; can absorb water and absorb oil to swell and soften in water and oil, but is not dissolved or disintegrated in water and oil. Under the action of pressure, the coating can be easily spread to release the coated substance, and the coated core material can be solid or liquid. Solves the problem that the microcapsule prepared by using a single melting shell material in the prior art can not simultaneously meet the special technical requirements of daily chemicals on melting point, hardness, high-temperature stability, release, skin feel and the like. The raw materials used in the invention are hot-melt raw materials, and the microcapsules can be prepared by a melting, dispersing and condensing method.

2. Application of microcapsule shell material

Example 19

TABLE 1 orange microcapsules

The preparation method comprises the following steps:

1) Heating cetearyl alcohol and cetearyl glucoside, PEG100 monostearate in water bath to 70 deg.C for complete melting, and mixing;

2) Adding vitamin A, vitamin E and astaxanthin into the mixture obtained in the step 1) and uniformly mixing;

3) Dripping the mixture obtained in the step 2) after melting and dispersing into a cooling tower with the inlet air temperature of 10 ℃ and the height of 6 meters by using a 0.5 mm orifice;

4) The microcapsules were collected at the bottom of the cooling tower.

By the steps, the orange wax spherical microcapsules with the diameter of 0.2-0.8 mm can be collected at the bottom of the cooling tower by an operator, and the microcapsules can absorb water and oil in water, gel or cream at 25 ℃, swell and soften by 1-2 times and can be easily applied by fingers.

From the above combination, a molten composition having a melting point of greater than 50 degrees, about 55-65 degrees C, is obtained as a shell.

HLB value of

Vitamin A is a coenzyme for regulating glycoprotein synthesis, has a stabilizing effect on cell membranes of epithelial cells, and can cause epithelial tissue dry cell keratinization due to the maintenance of morphological integrity and functional vitamin A deficiency of the epithelial cells. Vitamin E and astaxanthin are antioxidant and antiaging active substances. However, all three actives are unstable to oxidation by light and heat. The encapsulated microcapsule is more stable against oxygen and air, is easy to add, and the microcapsule is easy to absorb water and swell in the formula to release the active ingredients

Example 20

Double-layer color-changing pigment microcapsule

TABLE 3 (formulation of inner pigment core)

TABLE 4 (outer pigment shell formula)

Composition (I)	Percentage of	Components
			Monoglyceride (I)	10％	Glyceride type emulsifier
Polyglycerol 10 palmitate	20％	Polyglycerol ester emulsifier
			1618 alcohol	25％	Higher fatty alcohols
Myristyl alcohol myristate	5％	Synthetic oil and fat
			Rice bran wax	5％	Natural wax
Titanium white powder	30％	Inorganic lake
			Palmitic acid vitamin C ester	5％	Fat-soluble active substance
Total up to	100％

A preparation method of color-changing pigment microcapsules comprises the following steps:

1) Heating monoglyceride, polyglycerol 10 palmitate and 1618 alcohol according to the proportion shown in the table 3 and the table 4 until the monoglyceride, the polyglycerol 10 palmitate and the 1618 alcohol are melted, and fully and uniformly stirring;

2) Respectively stirring the ferric oxide lake microcapsule shell materials and the titanium dioxide lake microcapsule shell materials uniformly;

3) Spraying the iron oxide brown molten dispersion liquid in the table 3 in the step 2 into cooling air to obtain spherical microcapsule cores with the diameter of 0.4-0.6 mm;

4) And (3) putting the brown microcapsule core obtained in the step (3) serving as a core into a tangential spraying fluidized bed, and spraying and cooling the titanium dioxide molten dispersion liquid in the step (2) shown in the table 4 onto the brown microcapsule core flowing in a rotating manner. The brown core is coated with a white shell. The sprayed weight of the white layer was 3 times the weight of the brown core. Finally, white direct microcapsules of 0.8-1.2 mm are obtained.

The melting microcapsule has a double-layer structure, wherein the inner core is brown, and the outer layer is white. The toner content is as high as 30%. It swells in the curry and cream and is white granule. But when pressure is applied, the inner brown and outer white mix to become a skin tone. Has good concealing effect. And the vitamin C palmitate as the active whitening component is also coated. The capsule has physical concealer and skin whitening effects. The melting point of the mixture is 55-65 deg.C, and HLB value is 6-9.

Example 21

TABLE 5A Heart type Capsule

Composition (I)	Percentage of	Class of component
			Polyglycerol 10 palmitate	15％	Polyglycerol emulsifiers
Polyglycerol-6 polyricinoleate	20％	Polyglycerol emulsifiers
			22 alcohol	10％	Higher fatty alcohols
1618 alcohol	10％	Higher fatty alcohols
			Hydrogenated jojoba oil	40％	Grease
Hydrolysed keratins	2％	Water soluble actives
			Polygonum multiflorum Thunb extract	2％	Plant extract active substance
Ginger essential oil	0.5％	Functional aromatic essential oil
			Litsea cubeba essential oil	0.5％	Functional aromatic essential oil
Lycopene	Proper amount of	Natural pigment
			Total up to	100％

The preparation method comprises the following steps:

1) Heating microcapsule shell materials of polyglycerol 10 palmitate, polyglycerol-6 polyricinoleate, 22 alcohol, 1618 alcohol and hydrogenated jojoba oil to melt, and stirring completely and uniformly;

2) Adding core material hydrolyzed keratin powder, polygoni Multiflori radix extract, rhizoma Zingiberis recens essential oil, litsea cubeba essential oil, and lycopene into microcapsule shell material, and stirring;

3) Quickly dripping the melt-dispersed liquid obtained in the step 2) into a heart-shaped mould. And (4) rapidly cooling and forming to obtain the wax block-shaped microcapsule with the required diameter of about 3 mm and the thickness of 0.5 mm.

The melting point of the formula is higher than 55 ℃, and the HLB value is between 4 and 9. Wherein the keratin has scalp caring effect. The ginger essential oil and the fleece-flower root extract have the effects of blackening and growing hair. The tablet capsule can be used in hair conditioner and hair treatment gel, and has beautiful appearance and practical effect. The hydrogenated jojoba oil is used for replacing the conditioning and smoothing functions of silicone oil. The raw materials of the formula are natural, and the production process has no water, solvent or preservative, thereby meeting the new trend of green chemistry of daily chemical industry.

3. Application method of microcapsule shell material

1. A method for preparing microcapsules comprises the following steps:

3) Cooling and molding the melted and dispersed liquid obtained in the step 2) in the air to obtain the microcapsule with the required size, specification and shape.

The cooling method comprises the step of injecting the melted and dispersed liquid into a mold or cooling the liquid on a plane to obtain a mold-shaped or sheet-shaped wrapper.

The cooling method comprises the steps of dripping or spraying molten and dispersed liquid into cold air, and obtaining spherical coated microspheres with different specifications through a certain distance of fall.

The core material is water-soluble active matter or fat-soluble active matter.

The water-soluble active substance is one or more of vitamins B1, B3, B5, B12, tea polyphenol, plant extract or plant powder.

The fat-soluble active matter is one or more of vitamin E, vitamin A, Q, carotene, astaxanthin, lutein, ceramide or phytosphingosine.

2. The invention also provides another application method of the microcapsule shell material, which comprises the following preparation steps:

2) And (3) coating the melted shell material solution on the coated core material in a disc mode, and cooling to obtain the microcapsule.

Wherein the core material is a crystal or a solid particle.

The melting point of the shell material of the microcapsule prepared by the method is higher than 50 ℃, and the microcapsule keeps a solid state at room temperature without the signs of melting, softening, separating out liquid oil and the like; in water, the water-soluble polymer can absorb water to swell and become soft, and is not dissolved or disintegrated in water. Under the action of pressure, the coated material can be easily dispersed and released, and the coated core material can be a solid or liquid material, so that the technical problem that the melting point, hardness, high-temperature stability and release conditions of the common microcapsule shell material in the prior art cannot simultaneously meet the requirements of a melting, dispersing and condensing method for preparing microcapsules for daily chemicals is solved.

Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the technical solutions, and those skilled in the art should understand that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all that should be covered by the claims of the present invention.

Claims

1. A microcapsule shell material, wherein the shell material has a melting point of greater than 50 ℃ and is solid at climatically different temperatures; can absorb water to swell and soften in water, but does not dissolve or disintegrate in water; under the action of pressure, the coating can be easily spread to release the coated substance, and the coated core material is solid or liquid.

2. The microcapsule shell according to claim 1, wherein the core component comprises, in weight percent: 0-50% of higher fatty alcohol or polyethylene glycol, 10-60% of grease or wax, 0-20% of oil thickener, 0-50% of fat-soluble pigment or inorganic lake and the balance of emulsifier.

3. The microcapsule shell according to claim 2, wherein the emulsifier is a nonionic emulsifier, an anionic emulsifier, a cationic emulsifier, or a zwitterionic emulsifier; nonionic emulsifiers are preferred.

4. A microcapsule shell according to claim 2, wherein the oil or wax is a vegetable oil ester or wax, an animal oil or fat, a synthetic oil or wax, a silicone oil or wax.

5. The microcapsule shell according to claim 2, wherein the higher aliphatic alcohol is a higher alcohol having a melting point of more than 30 degrees; higher alcohols with a carbon number greater than 14 are typically used.

6. The microcapsule shell according to claim 2, wherein the polyethylene glycol { PEG } is a solid polyethylene glycol having a molecular weight of more than 1000 and a solidification point of more than 25 ℃.

7. The microcapsule shell according to claim 2, wherein the oil thickener is a polymer thickener dissolved in oil or a solid powder thickener.

8. The microcapsule shell according to claim 2, wherein the pigment lake refers to a synthetic or natural organic pigment or organic lake.

9. The microcapsule shell material according to claim 2, wherein the lake is an inorganic lake.

10. A microcapsule shell according to claim 3, characterized in that the emulsifier is preferably a solid emulsifier with a melting point higher than 30 ℃.

11. A microcapsule shell according to claim 3, wherein the emulsifier has an HLB value of between 3 and 13.

12. The microcapsule shell according to claim 3, wherein the non-ionic emulsifier comprises: alcohol nonionic emulsifiers, polyoxyethylene nonionic emulsifiers, nitrogen-containing nonionic emulsifiers, block polyether type and sterol-derived nonionic emulsifiers.

13. The microcapsule shell according to claim 12, wherein the alcohol-based nonionic emulsifier comprises: one or more of glycol esters, glycerides, polyglycerol fatty acid esters, neopentyl polyol esters, sugar esters, sorbitol esters, and alkyl glycoside type nonionic emulsifiers.

14. The microcapsule shell according to claim 13, wherein the glycol ester is a nonionic emulsifier produced by a reaction between ethylene glycol and a fatty acid.

15. The microcapsule shell according to claim 13, wherein the glycerin fatty acid ester is a monoglyceride, a diester or a triester as a nonionic emulsifier produced by the reaction of glycerin with a fatty acid.

16. The microcapsule shell according to claim 13, wherein the polyglycerin fatty acid ester-based emulsifier is a polyhydroxy ester-based nonionic surfactant composed of a polyglycerin and a fatty acid.

17. The microcapsule shell according to claim 13, wherein the neopentyl polyol lipid nonionic emulsifier is pentaerythritol fatty acid ester.

18. The microcapsule shell according to claim 13, wherein the sugar ester-based emulsifier is a nonionic emulsifier obtained by esterifying glucose having a plurality of hydroxyl groups, sucrose and fatty acid such as lauric acid, stearic acid, oleic acid, palmitic acid, etc.; sugar esters can be classified into monoesters, diesters, and triesters, depending on the degree of esterification.

19. The microcapsule shell according to claim 13, wherein the sorbitol esters are partial fatty acid esters of polyoxyethylene sorbitan (tween) and sorbitan fatty acid ester (span) emulsifiers.

20. The microcapsule shell according to claim 13, wherein the alkylglycoside is an alkylglycoside synthesized from glucose and a fatty alcohol.

21. The microcapsule shell according to claim 13, wherein the polyoxyethylene-type nonionic emulsifier comprises: one or more of fatty alcohol-polyoxyethylene ether, fatty acid-polyoxyethylene ester, alkylphenol ethoxylate and polyoxyethylene ammonium fatty acid.

22. The microcapsule shell according to claim 21, wherein the fatty alcohol-polyoxyethylene ether is an ether nonionic emulsifier obtained by addition of polyethylene glycol (PEG) and a fatty alcohol via ethylene oxide, and has a chemical formula of RO (CH 2O) nH.

23. The microcapsule shell material of claim 21, wherein the fatty acid polyoxyethylene ester is formed by an addition reaction of a fatty acid and ethylene oxide and has a general formula of RCOO (CH 2O) nH.

24. A process for the preparation of microcapsules, characterized in that the microcapsule shell components of claims 2 to 23 are used, which comprises the steps of:

2) Adding the core material into the microcapsule shell material and uniformly stirring; the core material is a solid or liquid material;

25. The method for preparing a microcapsule according to claim 24, wherein the cooling step is carried out by pouring the molten and dispersed liquid into a mold or spreading the liquid on a flat surface to cool the liquid, thereby obtaining a mold-shaped or sheet-shaped coating.

26. The process for preparing microcapsules of claim 24, wherein the cooling is carried out by dropping or spraying the molten dispersion liquid into cold air, and cooling with air through a certain distance of drop to obtain coated microspheres with different sizes of spheres.

27. The method of claim 24, wherein the core material is a water-soluble active, a fat-soluble active, or an insoluble substance.

28. The method of claim 27, wherein the water soluble active is one or more of vitamin B1, B3, B5, B12, vitamin C and its derivatives, ethyl ascorbic acid, tea polyphenols, peptides, amino acids, plant extracts.

29. The method of claim 27, wherein the lipid soluble active is one or more of vitamin E, vitamin E acetate, vitamin a palmitate, vitamin C palmitate, Q10, carotene, astaxanthin, lutein, ceramide, phytosphingosine.

30. A process for the preparation of microcapsules according to claim 27, wherein said lipid soluble active is a plant derived essential oil or essence.

31. The method for preparing microcapsules of claim 27, wherein said insoluble substance is an active substance insoluble in both water and oil and includes minerals, probiotics, raw plant and animal powder, proteins, etc.

32. A process for the preparation of microcapsules, characterized in that a microcapsule shell component according to any one of claims 2 to 24 is used, which process comprises the steps of:

33. The method of claim 32, wherein the core material is a crystal or a solid particle.