WO2020093192A1

WO2020093192A1 - Water-soluble active particle, preparation method therefor and use thereof

Info

Publication number: WO2020093192A1
Application number: PCT/CN2018/113940
Authority: WO
Inventors: 袁彦洁; 蒋伺江; 杜森垚; 罗敏
Original assignee: 重庆小丸科贸有限公司
Priority date: 2018-11-05
Filing date: 2018-11-05
Publication date: 2020-05-14
Also published as: CN112930166A

Abstract

A water-soluble active particle which can be quickly dissolved when added into cosmetics, a preparation method therefor and use thereof. The water-soluble active particle comprises the following components by weight percentage: 0.1-15% of a binder, 1-80% of a filler, 0.1-5% of a disintegrant, and an appropriate amount, i.e. 0-1%, of a pigment, with the balance being water-soluble active powder. The particle is made from pharmaceutical, edible or cosmetic raw materials.

Description

Water-soluble active material particle, preparation method and application thereof

Technical field

The invention relates to the technical field of cosmetics, in particular to a water-soluble active substance particle and a preparation method and application thereof.

Background technique

There are many water-soluble active substances that have whitening, moisturizing, anti-aging, anti-allergy, and anti-acne effects on the skin. However, there are quite a lot of water-soluble actives in water that cannot maintain long-term stability. However, most cosmetics contain water, which leads to the direct addition of these water-soluble actives in aqueous cosmetics can not be stable during shelf life or use period . Therefore, the application of these active substances is greatly limited. For example, vitamin C is an active substance that is easily soluble in water but extremely unstable in water. Vitamin C is a natural antioxidant, anti-oxidant to prevent cancer. It can inhibit the synthesis of melanin and reduce the produced melanin to colorless reduced melanin. It also has the effect of promoting collagen synthesis and has strong physiological functions in the skin, such as whitening, anti-aging, and acne. It can also remove free radicals, which can delay the rate of body degradation, prevent skin aging, help repair damaged and dull skin, shrink pores, and make skin firm. Therefore, vitamin C has been used in skin care products as a safe and effective whitening ingredient for a long time. However, vitamin C powder has a large surface area, which is easy to absorb moisture and oxidize. It oxidizes faster in water-containing products, which means that vitamin C is directly added to water-containing cosmetic formulas and it is impossible to be stable for 2-3 years according to shelf life. existing. Therefore, the acidity and extremely oxidizable nature of vitamin C limit the application of vitamin C directly in cosmetics.

At present, vitamin C derivatives are mainly used in skin care products to replace vitamin C such as vitamin C ethyl ether, vitamin C palmitate, vitamin C glucoside, and vitamin C phosphate, although the above derivatives will be decomposed by the enzyme system inside the skin And reduced to vitamin C, but its physiological activity is much lower than vitamin C itself. In addition, because vitamin C powder itself has no fluidity, dust, and strong moisture absorption, it is difficult to canned. Therefore, how to achieve the stability and fluidity of vitamin C in skin care formulations is an urgent problem to be solved, and it has also been paid more and more attention by researchers at home and abroad.

Summary of the invention

In view of the above-mentioned shortcomings of the prior art, the object of the present invention is to provide a water-soluble active material particle, which solves the problem that the water-soluble active material is easy to oxidize and absorb moisture during storage, and the particles are easy to dust, fluff and The problem of poor fluidity; such water-soluble active particles are usually used in cosmetics where the particles and the base are packaged separately. When used, the particles are mixed into the cosmetic base, and the particles are quickly dispersed and dissolved to release the water-soluble active substance. Immediate fresh use avoids the problem of instability caused by direct addition of active substances.

The invention provides a preparation method of the particles. The invention also provides the application of water-soluble active substance particles in cosmetics.

In order to solve the above technical problems, the present invention adopts the following technical solution: a water-soluble active substance particle, characterized in that the water-soluble active substance powder is wrapped in an instant shell to form fine particles; wherein, the water-soluble active substance The mass percentage of the powder and the instant shell is 20-99: 80-1; the instant shell includes a binder, an instant filler and a disintegrant. The content of the instant soluble shell including particles of water-soluble active matter can be as high as 99%, and the content ratio of water-soluble active matter can also be reduced by adding an instant filler according to application requirements.

Further, the instant shell further includes a pigment, which accounts for 0% to 1% of the particles of the water-soluble active substance.

Further, the water-soluble active substance is a water-soluble active substance having effects of moisturizing, whitening, anti-aging or anti-allergy in cosmetics. Among them, the water solubility of the active substance is defined as a 1% by mass aqueous solution of the active substance, which is a uniform and clear aqueous solution or a uniform dispersion liquid at 25 ° C.

The instant shell includes binders, instant fillers, disintegrants, pigments, etc., all of which are easily soluble in water to ensure that there are no residues after the particles are dissolved.

The bulk density of the water-soluble active material particles is 0.4 g / mL to 1.2 g / ml, the more common bulk density range is 0.6 g / mL to 1.0 g / ml, and the high bulk density water-soluble active material particles have good fluidity and volume Small for canning.

The particle size of the water-soluble active material particles is 100-2000n micrometers, on the one hand, the specific surface area of the water-soluble active material powder is reduced, thereby reducing the surface area of the water-soluble active material powder in contact with air; on the other hand, on the surface of the water-soluble active material Form a layer of instant shell to delay the rate of oxidation.

Further, the binder is sucrose, various cellulose derivatives, or includes carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose, methyl cellulose, crospovidone, One or more of polyvinyl alcohol, sodium alginate, xanthan gum and agar are easily soluble in water polymer materials. The instant filler is an edible soluble material including glucose, mannitol, sorbitol, fructose, or lactose. Disintegrants include water-swellable materials such as sodium carboxymethyl cellulose, sodium carboxymethyl starch, acrylic starch or agar.

The polymer material includes carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose, methyl cellulose, crospovidone, polyvinyl alcohol, sodium alginate, xanthan gum, keratin One or more water-soluble polymer materials in carrageenan or agar.

Among them, sucrose can be dissolved into syrup as a binder in the ingredients, and the water-soluble active powder can also be diluted with sucrose powder as a filler to achieve the required content of water-soluble active. The sucrose solution itself has a viscosity and can be used as a binder in the process. The sucrose dissolves quickly and does not affect the dissolution rate of water-soluble active substances. If other water-soluble polymer materials are used, according to different content requirements, appropriate amounts of water-soluble fillers such as sucrose, glucose, mannitol, sorbitol, lactose, etc. can be added. Generally, when water-soluble polymer materials are used as binders, the dissolution time of water-soluble active material particles will be prolonged and the purpose of high-speed dissolution cannot be achieved. Therefore, when granulating with water-soluble polymer materials, it is necessary to appropriately add disintegrants, usually some The highly swellable water-soluble colloid allows the particles to quickly disintegrate into powder, so that the water-soluble active substance dissolves quickly in water. Disintegrants include carboxymethyl cellulose, carboxymethyl starch, modified starch, or agar, which have both binding power and high swelling. The granules made by swelling rapidly with water, allowing the granules to disintegrate into powder instantly. Colloids act as both binders and disintegrants. When other water-soluble colloids with relatively low swelling properties are used as binders, such as povidone, polyvinyl alcohol, sodium alginate, xanthan gum, carrageenan, etc., the above disintegrating colloids can be appropriately added to accelerate the dissolution rate. In addition, in the granulation process, the binder liquid covers the water-soluble active substance with a film shell, and the water-soluble active substance powder is bound into strong particles, which greatly reduces the contact area between the water-soluble active substance and oxygen in the air. Reduce the oxidation rate to make it easier to store.

The present invention also provides a method for preparing instant water-soluble active substance particles, including the following steps:

1) According to the composition of the water-soluble active material particles;

2) Dissolve the binder in water to obtain a binder solution;

3) Put the water-soluble active material powder into a tangential spray rotary fluidized bed to make granules.

The working principle of the tangential spray rotating fluidized bed: the bottom of the raw material container of the fluidized bed is a high-speed rotating turntable, and there is a very small (0.5-5 mm) gap between the turntable and the side wall of the container. High-speed rise in the gap. The water-soluble active substance rotates at a high speed in the container due to the rotation of the turntable. The centrifugal force throws the water-soluble active substance towards the outer wall of the container. Therefore, the water-soluble active substance performs a high-speed rotation motion of a twisted rope suspension tumble along the edge of the turntable under the action of three external forces. The nozzle is immersed in the rotating water-soluble active substance, and the sprayed adhesive is completely applied to the high-speed flow The above water-soluble active substance particles completely avoid the loss of sprayed liquid. The hot air flowing upward penetrates the layer of flowing water-soluble active particles, so that the adhesive is dried in time. The granules made by this method make the powder easy to stick, compact and have a high packing density due to the centrifugal force. At the same time, the binder is sprayed on the water-soluble active powder rotating at high speed, which ensures the uniformity and consistency of the shell. In addition, due to the rolling friction of the circular motion of the particles, the particles have no sharp acute angles, and the particles are rounded, ensuring their excellent fluidity.

Further, usually due to the slow swelling speed of the water-soluble polymer binder, the particles prepared with the addition amount higher than 5% should be harder and affect the dissolution rate; the amount of the water-soluble polymer binder is too small, less than 0.1%, preparation The particles obtained should be loose, brittle, and irregular. Therefore, when the binder is sucrose which is easily dissolved in water, the percentage of sucrose is 8.0-15.0%. When the binder is a polymer material easily dissolved in water, the concentration is 0.1-5.0%.

Further, the linear velocity of the rotating speed of the fluidized bed is 100-2000 m / min. In this way, the high-speed centrifugal force of the fluidized bed turntable allows the particles to roll strong, not loose, and does not lose powder, ensuring its high bulk density. When large particles (particle size of 1000-2000um) are required, the linear velocity of rotation of the fluidized bed is controlled to be 100-1000 meters / minute. When small particles (particle size less than 1000um) are required, the linear velocity of rotation of the fluidized bed is controlled to be 1000-2000 meters / minute.

The water-soluble active material of the present invention is a water-soluble active material having the functions of moisturizing, whitening, anti-aging, anti-allergy and the like in cosmetics, and the water-soluble active material is unstable in water. Further, the water-soluble active substance is a water-soluble vitamin, such as vitamin C, vitamin B family (B1, B2, B5, B6, B12) niacin, folic acid, pantothenic acid, and lipid derivatives of these vitamins. Among them, vitamin C is a typical active substance with extremely high water solubility, whitening effect, but very unstable in water.

The water solubility of the active substance is defined as a 1% by mass aqueous solution of the active substance, which is a uniform and clear aqueous solution at 25 ° C. Further, such water-soluble active substance particles are generally used in cosmetics in which the particles and the base material are packaged separately. When used, the particles are mixed into the cosmetic base material, and the particles are rapidly dispersed and dissolved to release the water-soluble active substance. Timely fresh use avoids the problem of instability of active substance added directly.

The application of the above water-soluble active substance particles in cosmetics separates the water-soluble active substance particles and the base material through the packaging of skin care products. When in use, the water-soluble active substance particles are mixed into the base material of the skin care product. The water-soluble active substance particles are usually quickly dissolved in the base material within 10 to 30 seconds and no more than 1 minute in the base material, and can be used immediately Fresh, useless, water-soluble actives that are oxidatively deteriorated.

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

1. The innovation of the present invention is that the water-soluble active material powder is wrapped in an instant shell to form micro particles, which solves the problem that the water-soluble active material is easy to oxidize and absorb moisture during storage, and the particles are easy to raise dust and fluff during the canning process. The problem of poor fluidity; the instant shell includes fillers, binders, disintegrants, pigments, etc., which are raw materials that are easily soluble in water to ensure that there are no residues after the particles are dissolved. Among them, the mass percentage of the water-soluble active material powder and the instant shell is 20 to 99: 80 to 1.

2. The water-soluble active material particles of the present invention have high bulk density, good fluidity, dust-free to avoid inhalation of high-concentration water-soluble active materials during worker operation and cause physical discomfort, small volume is convenient for canning, the particles can quickly be used in cosmetic formulations containing water It dissolves rapidly in the medium, usually no more than 1min between 10 and 30 seconds, and at the same time reduces the specific surface area of the water-soluble active powder, thereby reducing the surface area in contact with air, followed by forming a thin film shell on the surface of the water-soluble active, The speed of oxidation is delayed, so that the water-soluble active material powder retains a high physiological activity, and solves the defects of poor stability and no fluidity of the water-soluble active material powder.

3. The preparation method of the invention is simple and fast, with simple raw materials and low cost, and can control the speed of the turntable, the size of the airflow, and the concentration spray speed of the adhesive to prepare regular and uniform size particles, which is convenient for quality control. control.

4. The water-soluble active material particles of the present invention are convenient to use. Since most cosmetics contain water, the invention is suitable for any water-soluble actives, especially suitable for the application of water-soluble actives unstable in water in cosmetics. In particular, cosmetics that package active materials and base materials separately have good application prospects. The water-soluble active substance particles can be immediately mixed into the base material, quickly dissolved and used immediately. Avoid adding water-insoluble actives that are unstable to water to water-based cosmetics when they are unstable for a long period of time.

When in use, it is only necessary to mix the water-soluble active material particles with the skin care product base material, so that the water-soluble active material particles quickly dissolve in the skin care product base material to form a uniform liquid. The particles are quickly soluble and completely soluble. The test is made according to this method. The granules are made into a 10% aqueous solution, that is, 10 grams of granules are stirred and dissolved to 90 grams of room temperature pure water. The complete dissolution rate is no more than 60 seconds, usually the dissolution time is 10-30 seconds, basically the dissolution rate of the water-soluble active substance powder Consistent. It has the characteristics of convenient use, so that the water-soluble active substance powder retains high physiological activity and has good application prospects.

BRIEF DESCRIPTION

Figure 1 is a schematic diagram of the structure of water-soluble active material particles.

2 is a schematic diagram of the process of the present invention.

In Fig. 1, 1 is a water-soluble active substance and an instant filler, and 2 is a mixture of a binder and a disintegrant.

In Fig. 2, 3 is a raw material container (fluidized bed), 4 is a rotating turntable, and 5 is upward hot air generated by spraying.

detailed description

The present invention will be further described in detail below in conjunction with examples.

1. A water-soluble active particle formula (dry parts)

2. A method for preparing instant vitamin C granules / instant vitamin B granules

Example 1

1) The ingredients are blended according to Example 1 in proportion;

2) Dissolve the binder sodium carboxymethyl cellulose in water to obtain a 3% binder solution;

3) Put the vitamin C powder into the tangential spray rotary fluidized bed and set at 1500rpm / min (turntable radius is about 0.2m, linear speed is 1884m / min to rotate, then start the spraying device, and the bond prepared in step 2) The agent solution is sprayed into the vitamin C powder rotating at a high speed from the tangential direction, so that the vitamin C powder is adhered by the binder until the resulting particles reach the desired size and the spraying is stopped, and then the particles are dried to obtain instant vitamin C particles.

Example 2

1) The ingredients are blended according to Example 2 in proportion;

2) Dissolve the sucrose binder in water to obtain a 30% binder solution;

3) Put the vitamin C powder into the tangential spray rotary fluidized bed and set 600rpm / min (turntable radius about 0.2m, linear speed 750m / min to rotate, and then start the spraying device, the step 2) is obtained The agent solution is sprayed into the vitamin C powder rotating at a high speed from the tangential direction, so that the vitamin C powder is adhered by the binder until the obtained particles reach the desired size to stop spraying, and then the particles are dried to obtain instant vitamin C particles.

Example 3

1) The ingredients are blended according to Example 3 in proportion;

2) Dissolve the sodium carboxymethyl cellulose binder in water to obtain a 3% binder solution;

3) Mix vitamin C powder and sucrose powder in proportion to the tangential spray rotary fluidized bed and set 750rpm / min (turntable radius about 0.2m, linear speed 940m / min to rotate, then start the spray device, step 2 ) The prepared binder solution is sprayed into the vitamin C powder rotating at a high speed from the tangential direction, so that the vitamin C powder is adhered by the binder until the resulting particles reach the desired size, stop spraying, and then dry the particles, that is Instant vitamin C granules are obtained.

Example 4

1) The ingredients are blended according to Example 4 in proportion;

2) Dissolve the hydroxyethyl cellulose binder in water to obtain a 3% binder solution;

3) Mix vitamin B1, B5 and B6 powders evenly with mannitol powder and sodium carboxymethyl starch. Proportionally mix into the tangential spray rotary fluidized bed and set 1500rpm / min (turntable radius about 0.2m, linear speed about 1900m / min to rotate, and then start the spray device, the adhesive solution prepared in step 2) from Spraying into the mixed powder rotating at high speed in the tangential direction, the vitamin B powder is adhered by the binder until the resulting particles reach the desired size and the spraying is stopped, and then the particles are dried to obtain instant vitamin B particles.

Example 5

1) According to the proportion of each component according to the implementation of 5 ingredients;

2) Dissolve the povidone binder in water to obtain a 5% binder solution;

3) Mix vitamin B5 powder with xylitol and mannitol powder in proportion to the tangential spray rotary fluidized bed and set 800rpm / min (turntable radius about 0.2m, linear speed 1100m / min for rotation, and then start the spray Device, spraying the binder solution prepared in step 2) into the vitamin B5 powder rotating at high speed from the tangential direction, so that the mixed powder is adhered by the binder until the resulting particles reach the desired size to stop spraying, and then the The granules are dried to obtain instant vitamin B5 granules.

As can be seen from the above table, the water-soluble active particles prepared by the present invention have high bulk density, good fluidity, and small volume for easy canning. The particles can quickly dissolve in water-containing cosmetic formulations, usually between 10 and 30 In seconds, the vitamin granules retain a high physiological activity, ensuring that the vitamin granules can be stable in skin care products for 2 to 3 years according to shelf life.

3. Application of Instant Vitamin C Granules

3.1. The instant vitamin C / B particles prepared in Examples 1 to 5 are used in a facial mask.

When packaging, divide the mask bag into 3 small bags (3 chambers), and the 3 chambers are respectively filled with film cloth, essence and VC / VB particles. When using, pour the VC / VB particles into the essence and dissolve quickly, then add the essence containing VC / VB to the membrane cloth, immerse the membrane cloth, and immediately apply the face.

3.2 Instant Vitamin C particles are used in cosmetics.

1) The instant vitamin C granules prepared in Examples 1 to 3/6 to 8 are used in the essence

Packed in a double-chamber vacuum package containing two chambers, the main chamber of water-based essence packaging, VC particles are installed in the smaller chamber inside, unscrew the VC particle chamber switch when first used, VC particles are mixed Into the essence, shake to dissolve the VC particles, then use the essence mixed with VC

2) The instant vitamin C particles prepared in Examples 1 to 6 are used in whitening creams

VC granules are packed separately in aluminum foil light-proof plastic bags, poured into the whitening cream base before use, stirred and dissolved to mix. Then use.

3.3 The instant mixed vitamin B particles prepared in Examples 4 to 5 were used in anti-aging sleep mask

The packaging bottle of the mask contains two parts. The bottle is filled with a lotion, and there is a cavity inside the lid (with instant vitamin B mixed granules. Pour the granules into the emulsion and mix them evenly after the first use. The granules are added to later products It needs to be used within 30 days to ensure the activity of the active substance.

4. Principles and methods based on the water-soluble active material particles of Examples 1 to 8, wherein the water-soluble active material uses vitamin B family (B1, B2, B5, B6, B12) niacin, folic acid, pantothenic acid or fats of these vitamins All derivatives can achieve the purpose of the present invention, and will not be exhaustive here.

The above are only the preferred embodiments of the present invention and are not limited by the present invention. Any modification, equivalent replacement and improvement made within the spirit and principle of the present invention should be included in the present invention. Within the scope of protection.

Claims

A water-soluble active substance particle, characterized in that the water-soluble active substance powder is wrapped in an instant shell to form fine particles; wherein, the mass percentage of the water-soluble active substance powder and the instant shell is 20-99: 80- 1; The instant shell includes binder, instant filler and disintegrant.
The water-soluble active substance particle according to claim 1, wherein the instant shell further comprises a pigment, and the percentage of the water-soluble active substance particle is 0 to 1%.
The water-soluble active substance particles according to claim 1 or 2, wherein the water-soluble active substance is a water active substance having moisturizing, whitening, anti-aging or anti-allergy effects in cosmetics.
The water-soluble active material particle according to claim 1 or 2, wherein the binder is sucrose easily soluble in water or a polymer material easily soluble in water.
The water-soluble active substance particle according to claim 1 or 2, wherein the instant filler is a powder containing sucrose, glucose, mannitol, sorbitol, fructose or lactose, an edible and soluble material.
The instant water-soluble active substance granule according to claim 1 or 2, characterized in that the disintegrant is a high swelling material comprising sodium carboxymethyl cellulose, sodium carboxymethyl starch, acrylic acid starch or agar in water.
The water-soluble active material particle according to claim 1 or 2, wherein the bulk density of the water-soluble active material particle is 0.4 to 1.2 g / ml.
The water-soluble active substance particle according to claim 1 or 2, wherein the particle size of the water-soluble active substance particle is 100-2000 microns.
The water-soluble active substance particles according to claim 1 or 2, characterized in that the weight percentage components are: binder 0.1 to 15%, instant filler 1 to 80%, disintegrant 0.1 to 5%, more than The amount is a water-soluble active substance.
The water-soluble active substance particles according to claim 3, characterized in that the water-soluble active substance is a water active substance that has moisturizing, whitening, anti-aging, anti-allergy and other effects in cosmetics but is unstable in water.
The water-soluble active substance particles according to claim 3, characterized in that the water-soluble active substance is a water-soluble vitamin, including vitamin C, vitamin B family (B1, B2, B5, B6 or B12) niacin, folic acid, Pantothenic acid and lipid derivatives of these vitamins.
The water-soluble active material particle according to claim 4, wherein the polymer material includes carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose, methyl cellulose, cross-linked polymer One or more water-soluble high-molecular-weight materials in ketone, polyvinyl alcohol, sodium alginate, xanthan gum, carrageenan or agar.
The water-soluble active material particle according to claim 7, wherein the bulk density of the water-soluble active material particle is 0.6 to 1.0 g / ml.
A method for preparing water-soluble active substance particles, characterized in that it includes the following steps:

1) Ingredients according to any one of claims 1 to 2;

2) Dissolve the binder and disintegrant in water to obtain a binder solution;

3) Put the mixture of water-soluble active material powder and filler powder into the tangential spray rotary fluidized bed and rotate at high speed, then start the spray device, and spray the adhesive solution prepared in step 2) from the tangential direction into high-speed rotation The water-soluble active material powder and the instant filler are mixed with powder to make them adhered by the binder to form granules, and then dried to obtain water-soluble active material particles.
The method for preparing water-soluble active material particles according to claim 14, wherein the concentration of the binder solution is 0.1-15.0%.
The method for preparing water-soluble active material particles according to claim 14, wherein the linear velocity of rotation of the fluidized bed is 100-2000 m / min.
The method for preparing water-soluble active material particles according to claim 14, wherein when the binder and sucrose which are easily soluble in water, the percentage of the binder in the particles is 8.0-15.0%.
The method for preparing water-soluble active material particles according to claim 14, wherein when the binder is a polymer material easily soluble in water, the percentage of the binder in the particles is 0.1-5.0% .
The method for preparing water-soluble active material particles according to claim 16, wherein the linear velocity of the fluidized bed rotation is 100-1000 meters / minute at low and medium times, and the resulting particle size is 1000-2000um.
The method for preparing water-soluble active material particles according to claim 16, characterized in that the linear velocity of rotation of the fluidized bed is relatively high from 1000 to 2000 meters per minute, and the particle size of the resulting particles is less than 1000 um.