WO2023184621A1 - Oil microcapsule capable of self-dispersing in water and preparation method therefor - Google Patents

Abstract

An oil microcapsule capable of self-dispersing in water, which oil microcapsule comprises the following components in percentages by mass: 35-70% of a porous raw material, 20-40% of an oil, 1-20% of an active substance, and 1-40% of an emulsifier. A preparation method for the oil microcapsule capable of self-dispersing in water comprises the following steps: 1) dissolving an oil and an oil-soluble active substance, and mixing same until uniform; 2) mixing an emulsifier and a polyol until uniform; (3) mixing the products obtained in steps (1) and (2) until uniform; and 4) spraying the product obtained in step 3) into a flowing powdery porous raw material, and cooling same to obtain a self-dispersing oil microcapsule. Water is not needed in the production process; moreover, by compounding the oil microcapsule with an emulsifier, a soluble filler, a thickener, etc., oil particles can be quickly dispersed in water to release oil, and a stable emulsion, cream or paste is obtained; and a product of the oil microcapsule can be used independently or in a compounded manner.

Description

A self-dispersing oil microcapsule in water and its preparation method Technical field

The present invention relates to the technical fields of personal care products and health care products, and in particular to a self-dispersing oil microcapsule in water and a preparation method thereof.

Background technique

Oils and fat-soluble active substances are important additives for daily chemicals, food, health products and medicines. For example, but not limited to the following common basic vegetable oils: olive oil, flaxseed oil, grapeseed oil, jojoba oil, argan oil, shea butter, avocado oil, almond oil, sunflower oil, castor oil, etc. , these natural oils are not only used in food and health products, but also widely used in cosmetics and personal care products. In addition, many synthetic oils and fatty acid esters are also used in daily chemicals, such as but not limited to squalane, squalene, caprylic acid triglyceride, myristyl myristate, mineral oil, alkanes, silicone oil, polyvalent Alcohols are also widely used in personal care products and cosmetics. In short, oil is an indispensable and important component of personal care products, food, and health care products.

Many fat-soluble functional active ingredients dissolve in fats and oils and work. For example: essential oils, fat-soluble vitamin A and its derivatives, vitamin E and its derivatives, vitamin K and its derivatives, coenzyme Q10, carotene, astaxanthin, lutein, lycopene, anti-aging agents, nerve Amides, phytosphingosine, idebenone, lipoic acid, tea oil, various essential oils, various volatile oils, various flavors, etc.

Many water-soluble active substances such as but not limited to vitamin C, curcumin, tea polyphenols, etc. are easily oxidized in water and air. Oil is a good wrapping material because it is hydrophobic and blocks oxygen. For example, vitamin C is wrapped in waxy oil. Will delay oxidation in the future.

Personal care products and cosmetics often have very complex ingredients, contain large amounts of water and oil, and have shelf lives of several years. The most common way oils are presented in cosmetics is in the form of lotions or creams. Many active substances cannot remain active for a long time in complex water-containing environments. Even ordinary vegetable oils are prone to oxidative rancidity. Many oils and fat-soluble active substances used in food, daily chemicals and pharmaceuticals are unstable and difficult to add in air, water, and complex compatibility environments. Stored in the form of encapsulated solid microcapsules or added to products, it is more stable than adding oil directly to products.

Some innovative daily chemical products will store the solid active ingredients separately from water and base materials through packaging, and then mix them after use for immediate use or one-time use to avoid compatibility issues and stability issues. Then it is necessary to make the oil and fat-soluble active substances into particles or powders that are easily dispersible and soluble in water.

In the existing technology, most of the oil powders are obtained by directly adsorbing oil and fat through porous raw materials. For example, silica, porous dextrin, cellulose, etc. can directly absorb oil and fat-soluble active substances to obtain powdered oil. However, powder particles that directly absorb grease or fat-soluble active substances cannot be uniformly dispersed into emulsions when floating in water. The grease will seep out from the pores and water and oil will separate.

Contents of the invention

In view of the above-mentioned deficiencies in the prior art, the purpose of the present invention is to provide a self-dispersing oil microcapsule in water to solve the problem that the powder particles of existing oils and fat-soluble active substances float in water and cannot be uniformly dispersed into emulsions.

Furthermore, the present invention also provides a method for preparing the self-dispersing oil microcapsules in water.

In order to solve the above technical problems, the present invention adopts the following technical solutions:

A self-dispersing oil microcapsule in water, including the following mass percentage ingredients:

Porous raw materials 35% to 70%, grease 20% to 40%, active substances 1% to 20%, emulsifier 1% to 40%.

Furthermore, it also includes polyols, accounting for 1-40% of the emulsifier mass; the polyols are glycerol, diglycerin, propylene glycol, ethylene glycol, butylene glycol, pentanediol, hexylene glycol, and polyethylene glycol 200 - One or more of 600, 16-alcohol, 18-alcohol or sugar alcohols; the sugar alcohols include sorbitol, mannitol, lactitol, and xylitol. It can adjust the HLB value of the emulsifier and form smaller emulsion droplets to assist emulsification. Polyols are hydrophilic and can make oil microcapsules self-emulsifying and dispersed in water.

Furthermore, it also includes solid soluble auxiliary materials, accounting for 0-30% of the mass of the oil; the solid soluble auxiliary materials are one or more of fructose, glucose, sucrose, maltose, lactose, ascorbic acid, xylitol, mannitol or sorbitol. Various. Adding solid soluble excipients can increase the penetration of water into the particles and accelerate disintegration and dissolution.

Furthermore, it also includes water-soluble polymers, which are used to change the viscosity and skin feel of the oil microcapsules after they are dispersed in water, accounting for 0%-10% of the oil quality; the water-soluble polymers are xanthan gum, carrageenan, and seaweed. Acid, gellan gum, guar gum and its derivatives, acrylic acid/C10-30 alkyl acrylic acid polymer, carbomer, konjac gum, chitosan, pullulan, polyvinyl alcohol, polyvinylpyrrolidine Ketones, mixture of sodium carboxymethyl cellulose and microcrystalline cellulose, sodium carboxymethyl starch, methyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose or polyacrylic acid branched starch, polyethylene glycol One or more of -240/HDI copolymer bis-decyltetradecanol-20, sodium polyacrylate, starch and its derivatives, dextrin and its derivatives. Adding water-soluble thickeners can assist emulsification, increase the stability of the emulsion after the particle oil is dispersed in water, and obtain emulsions with different thicknesses and viscosities.

The plant sources of the starch and its derivatives, dextrin and its derivatives include potatoes, corn, beans, sweet potatoes, cassava, taro, rice, barley, wheat and fruits such as water chestnuts, lotus root and kudzu root.

The plant sources of cellulose and microcrystalline cellulose include wood pulp and cotton pulp.

Further, the porous raw materials include inorganic porous raw materials and organic porous raw materials;

The inorganic porous raw materials include one or more of silica and its derivatives, bentonite, montmorillonite, activated carbon, kaolin, zeolite, molecular sieve, and graphene;

The organic porous raw materials include starch and its derivatives, dextrin and its derivatives, cellulose and microcrystalline cellulose and its derivatives, cyclodextrin and its derivatives, ultrafinely pulverized plant powder, porous starch and its derivatives. one or more derivatives.

Further, the emulsifier is an oil-in-water emulsifier, and its HLB is greater than 8.

A method for preparing self-dispersing oil microcapsules in water, which is prepared according to the above components. The specific steps include:

1) Dissolve the oil and active substances and mix them evenly;

2) Add emulsifier and mix evenly;

3) If the product obtained in step 2) is solidified at room temperature, heat it until it melts. The heating temperature is 40-60°C. Then spray the product obtained in step 2) into the flowing powdery porous raw material and cool it to obtain a self-dispersing oil. Microcapsules;

If the product obtained in step 2) is still in the form of a paste with high viscosity after being heated at room temperature or 40-60°C and cannot be sprayed, pass the product through a ball mill and a three-roller mixer successively, and squeeze and adsorb it into the powdery porous raw material. , and then cooled to obtain self-dispersing oil microcapsules.

A method for preparing self-dispersing oil microcapsules in water. The specific steps include:

1) Dissolve the oil and active substances and mix them evenly;

2) Add polyol, solid soluble excipients and/or water-soluble polymer to the emulsifier, and mix evenly;

3) Mix the products obtained in steps 1) and 2) evenly;

4) If the product obtained in step 3) is solidified at room temperature, heat it until it melts. The heating temperature is 40-60°C. Then spray the product obtained in step 3) into the flowing powdery porous raw material and cool it to obtain a self-dispersing oil. Microcapsules;

If the product obtained in step 3) is still in the form of a paste with high viscosity after being heated at room temperature or 40-60°C and cannot be sprayed, pass the product through a ball mill and a three-roller mixer successively, and squeeze and adsorb it into the powdery porous raw material. , and then cooled to obtain self-dispersing oil microcapsules.

Furthermore, the dissolving and mixing temperature of the oil and active matter in step 1) is 40-80°C.

Further, the flowing powdery porous raw material is prepared using a stirrer, ball mill, trough mixing, three-roller mixer, wet granulator or fluidized bed.

When using a fluidized bed to prepare flowing powdery porous raw materials, boil and flow at a temperature about 5-10°C lower than the mixture.

An application of self-dispersing oil microcapsules, using the above oil microcapsules for food, health care products, medicines, personal care products or cosmetics.

Compared with the existing technology, the present invention has the following advantages:

1. The oil microcapsules of the present invention solve the problem of oil particles floating in water and unable to be uniformly dispersed into emulsions by adjusting and compounding other auxiliary materials such as emulsifiers, thickeners, etc., and the oil particles of the present invention can be quickly dissolved in water. Disperse and release oil, and obtain stable emulsions, creams or pastes for use alone or in combination.

2. The preparation method of the present invention does not require the addition of water as a solvent, which solves the problem that many active substances cannot maintain activity for a long time in complex water-containing environments and are easily oxidized and acidified.

3. The preparation method of the present invention uses porous raw materials to adsorb and wrap the oil mixture to prepare powdered oil. There is no need to use organic solvents, the process is water-free, and there is no need to carry out complex processing such as emulsification, homogenization, and drying of the oil. It does not affect the flavor of the oil and will not Because high temperature drying and moisture have an adverse effect on the active ingredients of oils, it can be more easily added to oral products; the solid powder granular oils for oral use are natural, safe, and non-toxic, the dosage is not limited, and the production process does not require organic solvents. porous material carrier. The process is simple and the cost is low.

4. The oil particles prepared by the present invention are widely used and can be used in the fields of food, health care products, medicines, personal care products, cosmetics and other fields. The selection of adsorbent raw materials is natural, safe, non-toxic, and listed in the standards of medicines, foods, and cosmetics.

Detailed ways

In order to enable those skilled in the art to better understand the technical solutions of the present invention, the present invention will be further described below with reference to specific examples, but the implementation of the present invention is not limited thereto.

Porous starch definition: The hydrolyzate obtained by the degradation of various starches by enzymes with hydrolytic activity of raw starch below the gelatinization temperature.

HLB (Hydrophile Lipophilic Balance): Hydrophile-lipophilic balance value.

Example 1

Porous maltodextrin encapsulates vitamin E, vitamin A, and astaxanthin. The percentage of each raw material is shown in Table 1.

Table 1

raw material	percentage	Remark
porous maltodextrin	50	Adsorption raw materials
sunflower oil	31	grease
Vitamin E	1	active substance
Vitamin A	1	active substance
Astaxanthin	0.5	active substance
glycerin	15	emulsifier solubilizer
sodium subtilisin	1.5	emulsifier
total	100	​

The preparation steps are as follows:

1) Dissolve sodium subtilisin and 10 parts of glycerol in a water bath at 50°C, then mix evenly with the remaining glycerin;

2) Dissolve vitamins E, A and astaxanthin into sunflower oil;

3) Mix and homogenize 1) and 2) to obtain a glycerol-in-oil oil phase mixture;

4) Stir 3) into the porous maltodextrin.

Step 3) The obtained glycerol-in-oil mixture has a certain viscosity at room temperature. Preheat it to about 40 degrees to soften it. Add porous maltodextrin to the wet granulator, turn on the large slow mixer below, and set the speed to 50 -500r/min, make the dextrin flow in a vortex, and then add the oil phase mixture. Turn on the high-speed shearing paddle, and part of the softened oil phase is absorbed and bonded by the micropores of porous maltodextrin; part of it is sheared into very small particles, and the outside of the particles is wrapped by free excess porous starch, forming a powder-encapsulated oil particle. capsule.

Sodium subtilisin is a naturally fermented high-performance emulsifier. The production process of this granular capsule does not require heating, does not contain water, and does not require drying. The granular capsules quickly disperse into a uniform emulsion when exposed to cold water. All three active ingredients have skin repair, antioxidant and anti-aging effects. The granular capsules can be added to the facial mask powder, and mixed with water when used, which fully ensures the activity of the active ingredients. During the production process, it does not come into contact with water, does not heat, and is stored in solid form.

The content of active substances can be increased to 20% as needed, and all raw materials are food raw materials. Therefore, this product can also be used as a food and health product additive.

Example 2

It is an easily dispersible mud mask powder that contains fat and vitamin C. The percentage of each raw material is shown in Table 2.

Table 2

raw material	percentage	Remark
Bentonite	14	adsorbent
kaolin	50	adsorbent
sodium carboxymethyl starch	1	thickener, disintegrant
caprylic triglyceride	5	grease
Myristic acid myristin	5	grease
shea butter	10	grease
monoglyceride	10	emulsifier
Vitamin C	5	active agent
total	100	​

The preparation steps are as follows:

1) Heat the monoglyceride and three kinds of fats to 60 degrees to fully melt them, and mix them evenly;

2) Add vitamin C powder and stir continuously;

3) Use fluidized bed top spray equipment to turn bentonite and kaolin into a flowing boiling state under the blowing of the incoming air, and the incoming air does not need to be heated;

4) The melted grease containing vitamin C powder is atomized into small oil mist through a spray gun and sprayed into the flowing powder;

5) The oil mist is absorbed and wrapped by the powder, forming a powder-encapsulated oil droplet structure.

This production process does not contain water. Since the oil phase is in a solid state at room temperature, the use of spray cooling not only allows the oil to be fully absorbed, but is also wrapped in powder to form a powder-encased oil droplet structure. In addition, vitamin C is sensitive to light and heat. , very sensitive to water and air, easily oxidized, and can hardly be added to any water-containing cosmetics. Vitamin C is wrapped in oil to isolate light and oxygen, improving storage stability. When the film powder is mixed with water, it is easily dissolved.

Example 3

Carotene granules and the percentages of each raw material are shown in Table 3.

table 3

The preparation steps are as follows:

1) Heat the sucrose fat and sweet almond oil to 40 degrees, mix thoroughly and dissolve, then cool;

2) Dissolve and mix carotene into 1);

3) Spray the mixture obtained in step 2) into the porous maltodextrin to allow the porous maltodextrin to fully absorb the oil;

4) The product obtained in step 3) is extruded into particles through an extruder, and then rounded into spherical particles using a shot blasting machine.

While rolling, the dextrinized octenylsuccinic anhydride-modified starch is thrown onto the particles formed by dextrin and oil to obtain a microcapsule wrapped in a dextrinized octenylsuccinic anhydride-modified starch powder shell. The diameter of the microcapsule is between 0.1-2 mm, and ideally, the diameter is between 0.5-1.5 mm.

This granule is easily dispersed in cold water. The dextrinized octenyl succinic anhydride modified starch plays an emulsifying and stabilizing role. All ingredients are edible ingredients and are a good food additive.

Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit the technical solutions. Those of ordinary skill in the art should understand that those technical solutions of the present invention can be modified or equivalently substituted without departing from the present technology. The purpose and scope of the solution should be covered by the claims of the present invention.

Claims (11)

1. A self-dispersing oil microcapsule in water, characterized by including the following mass percentage ingredients:

   Porous raw materials 35% to 70%, grease 20% to 40%, active substances 1% to 20%, emulsifier 1% to 40%.
2. The self-dispersing oil microcapsule in water according to claim 1 is characterized in that it also includes a polyol, accounting for 1-40% of the quality of the emulsifier; the polyol is glycerin, diglycerol, propylene glycol, ethylene glycol, butylene glycol. Alcohol, pentanediol, hexylene glycol, polyethylene glycol 200-600 or one or more sugar alcohols; the sugar alcohols include sorbitol, mannitol, lactitol, and xylitol.
3. The self-dispersing oil microcapsule in water according to claim 1 is characterized in that it also includes solid soluble auxiliary materials, accounting for 0-30% of the quality of the oil; the solid soluble auxiliary materials are fructose, glucose, sucrose, maltose, lactose, One or more of ascorbic acid, xylitol, mannitol or sorbitol.
4. The self-dispersing oil microcapsule in water according to claim 1, characterized in that it also includes a water-soluble polymer for changing the viscosity and skin feel of the oil microcapsule after being dispersed in water, accounting for 0%-10% of the oil quality; The water-soluble polymers are xanthan gum, carrageenan, alginic acid, gellan gum, guar gum and its derivatives, acrylic acid/C10-30 alkyl acrylic acid polymer, carbomer, konjac gum, and chitosan , pullulan, polyvinyl alcohol, polyvinylpyrrolidone, sodium carboxymethylcellulose and microcrystalline cellulose mixture, sodium carboxymethyl starch, methylcellulose, hydroxyethylcellulose, hydroxypropyl Methylcellulose, polyacrylic acid branched starch, polyethylene glycol-240/HDI copolymer bis-decyltetradecanol-20, sodium polyacrylate, starch and its derivatives or dextrin and its derivatives of one or more.
5. The self-dispersing oil microcapsules in water according to claim 1, wherein the porous raw materials include inorganic porous raw materials and organic porous raw materials;

   The inorganic porous raw materials include one or more of silica and its derivatives, bentonite, montmorillonite, activated carbon, kaolin, zeolite, molecular sieve, and graphene;

   The organic porous raw materials include starch and its derivatives, dextrin and its derivatives, cellulose and microcrystalline cellulose and its derivatives, cyclodextrin and its derivatives, ultrafinely pulverized plant powder, porous starch and its derivatives. one or more derivatives.
6. The self-dispersing oil microcapsule in water according to claim 1, characterized in that the emulsifier is an oil-in-water emulsifier and its HLB is greater than 8.
7. A method for preparing self-dispersing oil microcapsules in water, which is characterized in that it is prepared according to the components of 1, and the specific steps include:

   1) Dissolve the oil and active substances and mix them evenly;

   2) Add emulsifier and mix evenly;

   3) If the product obtained in step 2) is solidified at room temperature, heat it until it melts. The heating temperature is 40-60°C. Then spray the product obtained in step 2) into the flowing powdery porous raw material and cool it to obtain a self-dispersing oil. Microcapsules;

   If the product obtained in step 2) is still in the form of a paste with high viscosity after being heated at room temperature or 40-60°C and cannot be sprayed, pass the product through a ball mill and a three-roller mixer successively, and squeeze and adsorb it into the powdery porous raw material. , and then cooled to obtain self-dispersing oil microcapsules.
8. A method for preparing self-dispersing oil microcapsules in water, which is characterized in that it is prepared according to components 2, 3 or 4, and the specific steps include:

   1) Dissolve the oil and active substances and mix them evenly;

   2) Add polyol, solid soluble excipients and/or water-soluble polymer to the emulsifier, and mix evenly;

   3) Mix the products obtained in steps 1) and 2) evenly;

   4) If the product obtained in step 3) is solidified at room temperature, heat it until it melts. The heating temperature is 40-60°C. Then spray the product obtained in step 3) into the flowing powdery porous raw material and cool it to obtain a self-dispersing oil. Microcapsules;

   If the product obtained in step 3) is still in the form of a paste with high viscosity after being heated at room temperature or 40-60°C and cannot be sprayed, pass the product through a ball mill and a three-roller mixer successively, and squeeze and adsorb it into the powdery porous raw material. , and then cooled to obtain self-dispersing oil microcapsules.
9. The method for preparing self-dispersing oil microcapsules in water according to claim 7 or 8, characterized in that the dissolving and mixing temperature of the oil and active substance in step 1) is 40 to 80°C.
10. The method for preparing self-dispersing oil microcapsules in water according to claim 7 or 8, characterized in that the flowing porous powdery raw material adopts a stirrer, a ball mill, a trough mixing, a three-roller mixer, and a wet granulator. or fluidized bed preparation.
11. An application of self-dispersing oil microcapsules, which is characterized in that microcapsules according to any one of claims 1 to 6 are used for food, health care products, medicines, personal care products or cosmetics.