阅读说明：本技术 一种类微胶囊前驱体及其制备方法 (Microcapsule-like precursor and preparation method thereof ) 是由 暴跃 许晋荣 李�东 闫惠丽 于 2020-11-28 设计创作，主要内容包括：本申请涉及化妆品的技术领域,具体公开了一种类微胶囊前驱体及其制备方法和一种类微胶囊的制备方法。类微胶囊前驱体包括溶剂、增稠剂、皮肤调理剂、抗氧化剂和防腐剂；其制备方法为：将原料加热直至完全溶解、均质后进行冷却即可得到类微胶囊前驱体,类微胶囊前驱体的5(wt%)的水分散体即为类微胶囊。本申请打破了常规微胶囊结构,创造了无壁结构的类微胶囊前驱体缓释体；实现了具有可长期维持,并在使用中可快速释放核心成分活性的类微胶囊前驱体的制备,且制备工艺简单,易于放大生产。(The application relates to the technical field of cosmetics, and particularly discloses a microcapsule-like precursor, a preparation method of the microcapsule-like precursor and a preparation method of a microcapsule-like precursor. The microcapsule-like precursor comprises a solvent, a thickening agent, a skin conditioning agent, an antioxidant and a preservative; the preparation method comprises the following steps: heating the raw materials until the raw materials are completely dissolved, homogenizing, and then cooling to obtain a microcapsule-like precursor, wherein 5 wt% of water dispersion of the microcapsule-like precursor is the microcapsule-like precursor. The application breaks through the conventional microcapsule structure and creates a microcapsule-like precursor slow-release body without a wall structure; realizes the preparation of the microcapsule-like precursor which can be maintained for a long time and can quickly release the activity of the core component in use, and has simple preparation process and easy scale-up production.)

1. A microcapsule-like precursor characterized by: the feed comprises the following raw materials: the skin conditioner comprises a solvent, a thickening agent and a skin conditioning agent, wherein the weight ratio of the solvent to the thickening agent to the skin conditioning agent is 1: 0.3-0.8: 0.5 to 2;

the solvent is one or more of polydimethylsiloxane and derivatives thereof, PEG derivatives, polysiloxane and derivatives, rosa damascena flower oil and jojoba seed oil;

the thickening agent is one or more of cetostearyl alcohol, ozokerite and beeswax;

the skin conditioner is one or more of hydrogenated C6-14 alkene polymers, hydrogenated lecithin, caprylic/capric triglyceride, pentaerythritol tetra (ethyl hexanoate), bisabolol and rose oil.

2. The microcapsule-like precursor according to claim 1, wherein: also comprises an antioxidant and a preservative,

the antioxidant is one or more of tocopherol and derivatives thereof, butylated hydroxytoluene, ascorbic acid and derivatives thereof, astaxanthin and chamomile oil;

the antiseptic is one or more of phenoxyethanol, methyl hydroxybenzoate, chlorphenesin, sodium benzoate, caprylyl hydroximic acid, sorbic acid and methylisothiazolinone.

3. The microcapsule-like precursor according to claim 1, wherein: the weight ratio of the solvent to the thickener to the skin conditioner to the antioxidant to the preservative is 1: 0.3-0.8: 0.5-2: 0.05-0.3: 0.0001 to 0.005.

4. A microcapsule-like precursor according to claim 2, wherein: the weight ratio of the solvent to the thickener to the skin conditioner to the antioxidant to the preservative is 1:0.5:1:0.1: 0.001.

5. A method of preparing a microcapsule precursor of any one of claims 1 to 4, comprising the steps of:

a. heating, dissolving and homogenizing: respectively putting the raw materials into a heating container, heating until the raw materials are completely dissolved, and homogenizing to obtain a mixed solution;

b. and (3) cooling: and stirring and cooling the obtained mixed solution to obtain the microcapsule-like precursor.

6. The method of claim 5, wherein the microcapsule precursor is prepared by: in the heating, dissolving and homogenizing process, the heating temperature is 60-90 ℃, the homogenizing rotation speed is 300-1000r/min, and the homogenizing time is 3-10 min.

7. The method of claim 5, wherein the microcapsule precursor is prepared by: in the cooling process, the temperature is cooled to 33-35 ℃, and the stirring speed is 100-.

8. A preparation method of microcapsules is characterized in that:

a. obtaining a constant-temperature capsule precursor: taking 5-15 parts of microcapsule-like precursor, and keeping the temperature to 50-80 ℃ for later use;

b. obtaining a constant temperature water phase: taking 85-95 parts of deionized water as a dispersed water phase at a constant temperature of 40-50 ℃, and continuously stirring;

c. and (3) preparing a finished product: slowly adding the capsule-like precursor with constant temperature into the dispersed water phase, and stirring until the mixed solution is whitened to finish the preparation.

Technical Field

The application relates to the technical field of cosmetic preparation, in particular to a microcapsule precursor and a preparation method thereof.

Background

How to improve the high efficacy, stability and reduce the low irritation of cosmetics is a common problem in the development process of cosmetics. At home and abroad, a great deal of complaints about the irritation of cosmetics and no corresponding effect of cosmetics exist every year.

Microencapsulation of cosmetics is currently a relatively efficient method for preparing cosmetics that combines high efficacy with low irritation. The microcapsule technology is a micro-encapsulation technology, wherein active substance core materials are wrapped by polymers to form micro-particles, and the size of the microcapsules is different from 10 to 1000 mu m. The main purpose of microcapsule technology is to encapsulate the active substance (core material) to ensure that the core material is not affected by the environment of the area of use, the active substance (core material) can be solid, gas or liquid, and the permeability of the shell can control the release of the core material to achieve long-term release of the active ingredient in the environment, release in another medium or no release at all. The microcapsule product has the characteristics of reducing skin irritation, covering raw material odor, improving raw material compatibility, improving efficacy and the like.

In cosmetics, the granulation method of the microcapsule mainly prepares a core material into a water-soluble substance, and then adds the water-soluble substance into a high molecular polymer solution to ensure that the surface of the core material is coated with the high molecular polymer to form a thin wall. The wall materials used by the microcapsules can be divided into three categories: (1) the fully synthetic high polymer material is not easy to degrade, and the name of part of wall materials is consistent with that of Plastic microbeads (Plastic microbeads), so that the consumer is easy to panic; (2) the semisynthetic polymer material is easy to hydrolyze and not resistant to high temperature, has large limitation on raw materials, needs temporary preparation, is easy to cause poor quality of cosmetics and reduces the efficacy; (3) the natural polymer material has poor physical and chemical stability, few types of available stable wall materials, certain limitation, high difficulty in amplification production, and great change in appearance and use feeling caused by the fact that the prepared product is easily influenced by storage environment. At present, people start to use the microcapsules in cosmetics, so that the problems that the raw material limitation, the physicochemical stability and the efficacy of the cosmetics adopting the microcapsule technology are reduced, the amplification production difficulty is high and the like become hot points and difficulties in the field of cosmetics are solved.

Most microcapsule products in the current market have problems

1. The coated microcapsule is not easy to break, and is mainly caused by the structure of the wall-containing microcapsule;

2. the state of 2019 stipulates that the plastic microbead products are forbidden, although the microcapsule wall material does not belong to the plastic microbead in a strict sense, the possibility of coincidence exists in the whole cosmetic components (cosmetic packaging component information), and panic is easily caused.

Disclosure of Invention

Based on the problems of the existing cosmetic microcapsule products, the research and development of the wall-free microcapsule precursor are carried out.

In order to replace the traditional microcapsule technology to prepare a low-irritation skin care product with high efficacy and no thin-wall capsule, the application provides a microcapsule-like precursor, a preparation method thereof and a preparation method of a microcapsule-like product.

In a first aspect, the present application provides a microcapsule-like precursor, which adopts the following technical scheme:

a microcapsule-like precursor comprises the following raw materials: the skin conditioner comprises a solvent, a thickening agent and a skin conditioning agent, wherein the weight ratio of the solvent to the thickening agent to the skin conditioning agent is 1: 0.3-0.8: 0.5 to 2;

the solvent is one or more of polydimethylsiloxane and derivatives thereof, PEG derivatives, polysiloxane and derivatives, rosa damascena flower oil and jojoba seed oil;

the thickening agent is one or more of cetostearyl alcohol, ozokerite and beeswax;

the skin conditioning agent is: hydrogenated C6-14 alkene polymers, hydrogenated lecithin, caprylic/capric triglyceride, pentaerythritol tetra (ethyl hexanoate), bisabolol, and rose oil.

Based on the problems of limitation, physicochemical stability, reduced efficacy, high difficulty in scale-up production and the like in the prior art of microcapsule preparation, a novel high-efficacy particle which is not limited by raw materials becomes a new exploration direction. The inventor finds that no relevant report exists in the aspect of wall-free microcapsules (microcapsules-like) so far. The microcapsule precursor (namely, the raw material formula of the microcapsule product which is not embedded yet) is prepared into a wall-free microcapsule structure, and the microcapsule precursor can replace the traditional microcapsule to become one of the methods for preparing the high-efficacy and low-irritation cosmetics. Therefore, the development of the sustained-release preparation (microcapsule-like precursor) which is not limited by raw materials, can maintain the efficacy of the core raw materials for a long time, has good compatibility of the formula and simple operation, and is easy to be produced in an enlarged manner has important theoretical and practical significance.

The inventors found in many experiments that a functional raw material product like a microcapsule product without a wall can be formed by preparing the microcapsule-like precursor into an oil-soluble wax-like substance and adding the oil-soluble wax-like substance into an aqueous dispersion phase.

By adopting the technical scheme, the raw materials such as the solvent, the thickening agent, the skin conditioner and the like are oil-soluble substances, and a good dissolving effect exists among the raw materials. The product prepared by matching dimethyl silicone polymer and derivatives thereof, PEG derivatives, polysiloxane and derivatives, rosa damascena flower oil, jojoba seed oil and other solvents with a thickening agent and a skin conditioner has better use feeling when used, pushes away smoothness and enhances the absorption of the skin;

when the microcapsule-like product is prepared by matching and selecting hydrogenated C6-14 alkene polymers, hydrogenated lecithin, caprylic/capric triglyceride and pentaerythritol tetra (ethyl hexanoate) as skin conditioners, the stability of the skin is maintained, and the water content of the skin is improved; when the selected bisabolol, rose oil and the like are matched as the skin conditioner, the skin conditioner has certain whitening and brightening effects while the water content of the skin is improved.

The microcapsule-like precursor mainly comprises a solvent, a thickening agent and a skin conditioner, and the weight ratio of the microcapsule-like precursor to the skin conditioner is 1: 0.3-0.8: 0.5 to 2. Since the three raw materials in the above ratio are mixed to form an oil-soluble wax-like substance, a functional raw material product like a microcapsule product without a wall can be formed in an aqueous dispersion system. Compared with microcapsule products used in the current market, the capsule-like precursor prepared by the method has wide raw material sources and simple preparation process, and can realize large-scale production; and the product is converted into a capsule-like product, so that the capsule-like product has better stability and low irritation under the condition of keeping the effective components to play a role stably. The application breaks through the conventional microcapsule structure and creates a microcapsule-like precursor slow-release body without a wall structure; realizes the preparation of the microcapsule-like precursor which can be maintained for a long time and can quickly release the activity of the core components in use.

Preferably, the antioxidant and the preservative are also included, and the antioxidant is one or more of tocopherol and derivatives thereof, butylated hydroxytoluene, ascorbic acid and derivatives thereof, astaxanthin and chamomile oil; the antiseptic is one or more of phenoxyethanol, methyl hydroxybenzoate, chlorphenesin, sodium benzoate, caprylyl hydroximic acid, sorbic acid and methylisothiazolinone.

By adopting the technical scheme, the preservative and the antioxidant are added, so that the stability of the microcapsule-like precursor is improved on one hand, and the functional effect on the skin is also increased on the other hand. The antioxidant and the preservative are compounded, and the antioxidant, the thickener and the skin conditioner are good in compatibility, low in sensitization and good in antioxidant effect.

Preferably, the weight ratio of the solvent to the thickener to the skin conditioner to the antioxidant to the preservative is 1: 0.3-0.8: 0.5-2: 0.05-0.3: 0.0001 to 0.005.

By adopting the technical scheme, the ratio of the solvent, the thickening agent, the skin conditioner, the antioxidant and the preservative in parts by weight is 1: 0.3-0.8: 0.5-2: 0.05-0.3: 0.0001 to 0.005, the formula has good compatibility, and the microcapsule-like product prepared from the microcapsule-like precursor has better skin conditioning effect.

Preferably, the weight ratio of the solvent, the thickening agent, the skin conditioning agent, the antioxidant and the preservative is 1:0.5:1:0.1: 0.001.

By adopting the technical scheme, the test result shows that the weight part ratio of the raw materials is 1:0.5:1:0.1:0.001, and the prepared microcapsule-like product has high stability and optimal conditioning effect and functional effect on skin.

In a second aspect, the present application provides a method for preparing a microcapsule precursor, comprising:

heating, dissolving and homogenizing: respectively putting the raw materials into a heating container, heating until the raw materials are completely dissolved, and homogenizing to obtain a mixed solution;

and (3) cooling: and slowly stirring and cooling the obtained mixed solution to obtain the microcapsule-like precursor.

By adopting the technical scheme, the preparation of the microcapsule-like precursor can be completed only by assisting heating equipment and stirring equipment, the preparation method is simple, and the large-scale production of the microcapsule-like precursor is facilitated.

Preferably, in the heating, dissolving and homogenizing process, the heating temperature is 60-90 ℃, the homogenizing rotation speed is 300-1000r/min, and the homogenizing time is 3-10 min.

Preferably, in the cooling process, the temperature is cooled to 33-35 ℃, and the stirring speed is 100-300 r/min.

By adopting the technical scheme, the heating temperature of 60-90 ℃ in the heating, dissolving and homogenizing process is favorable for fully dissolving various components in the raw materials, and the temperature beyond the range is easy to cause uneven dispersion of various components of the microcapsule, thereby causing the reduction of efficacy and use feeling; the homogenizing rotating speed is 300-; in the cooling process, the homogenizing time is 3-10min, so that each component in the capsule-like precursor raw material system is micronized, homogenized and fully dispersed, and the functions of reducing the size of a dispersion and improving the distribution uniformity of the dispersion are achieved; in the cooling process, substances in the mixed solution are fully dispersed, the stirring is performed to enable the internal cooling speed of the mixed solution to be consistent, the phenomenon that the physicochemical properties in the mixed solution are not uniform due to inconsistent cooling speeds is reduced, especially when the stirring speed is too high, the local temperature difference of the solution can be caused, the solidification of the microcapsule-like precursor is not uniform, the process difficulty is enlarged, the precursor is lost, and the yield is reduced.

In a third aspect, the application provides a preparation method of microcapsules, which adopts the following technical scheme:

a. obtaining a constant-temperature capsule precursor: taking 5-15 parts of microcapsule-like precursor, and keeping the temperature to 50-80 ℃ for later use;

b. obtaining a constant temperature water phase: taking 85-95 parts of deionized water as a dispersed water phase at a constant temperature of 40-50 ℃, and continuously stirring;

C. and (3) preparing a finished product: slowly adding the capsule-like precursor with constant temperature into the dispersed water phase, and stirring until the mixed solution is whitened to finish the preparation.

By adopting the technical scheme, the prepared capsule-like product is not limited by raw materials, can maintain the efficacy of core raw materials for a long time, and has good compatibility of the formula; and forming the microcapsule-like particles by heating to 50-80 ℃. Temperatures outside this range do not form microcapsule-like particles. The steps are simple to operate, mixing can be achieved, the scale-up production is easy, and a reliable technical route and a theoretical basis are provided for preparing cosmetics with high efficacy, low irritation and stable change over time.

In summary, the present application has the following beneficial effects:

1. the application breaks through the conventional microcapsule structure and creates a microcapsule-like precursor slow-release body without a wall structure; the preparation of the microcapsule-like precursor which can be maintained for a long time and can quickly release the activity of the core components in use is realized;

2. the application provides a preparation method of the microcapsule-like precursor, which is simple to operate and convenient to implement, and realizes the preparation of the microcapsule-like precursor which can be maintained for a long time and can quickly release the activity of core components in use;

3. the application also provides a preparation method of the microcapsule-like structure, the microcapsule-like structure has no wall structure, the problems that the microcapsule is difficult to quickly release and absorbed by skin or the microcapsule wall is dissolved and damaged, so that the core functional components are lost, the efficacy is reduced due to quality change and the like are solved, the optimal activity and the service life of the core functional components are maintained, the release rate of the core functional components is improved, and the microcapsule-like structure is beneficial to research, development and amplification production of high-efficacy and low-irritation cosmetics.

Drawings

FIG. 1 is a comparison of the skin condition before and after use of a capsule-like product;

fig. 2 is a comparison of the facial stain detection and the area of the stain magnified before and after use of the capsule-like product by the test person 10.

Detailed Description

The present application is described in further detail below with reference to figures 1-2 and examples.

Some raw material sources in the examples of the present application are shown in table 1:

table 1 source of raw materials table:

example 1

A microcapsule-like precursor comprises the following raw materials: the skin care product comprises a solvent, a thickening agent and a skin conditioning agent, wherein in the embodiment, the solvent is 20g of jojoba seed oil and 20g of rosa damascena flower oil, the thickening agent is 12g of beeswax, and the skin conditioning agent is 80g of caprylic acid/capric acid triglyceride, wherein the weight ratio of the solvent to the thickening agent to the skin conditioning agent is 1: 0.3: 2.

specifically, heating, dissolving and homogenizing: respectively putting 20g of jojoba seed oil, 20g of rosa damascena flower oil, 12g of beeswax, 80g of caprylic/capric triglyceride and 0.0004g of coloring agent into a heating tank, heating to 60 ℃, completely dissolving, homogenizing at the rotation speed of 300r/min for 10min, and obtaining a mixed solution;

and (3) cooling: and slowly stirring the mixed solution prepared in the heating, dissolving and homogenizing process at the stirring speed of 300r/min, and cooling to 30 ℃ to obtain the microcapsule-like precursor.

Example 2

A microcapsule-like precursor comprises the following raw materials: the skin care product comprises a solvent, a thickening agent and a skin conditioning agent, wherein in the embodiment, the solvent is 38.5g of polydimethylsiloxane, the thickening agent is 19.07g of cetearyl alcohol, and the skin conditioning agent is 38.5g of pentaerythritol tetra (ethyl hexanoate), wherein the weight ratio of the solvent to the thickening agent to the skin conditioning agent is 1:0.5: 1.

specifically, heating, dissolving and homogenizing: respectively putting 38.5g of polydimethylsiloxane, 19.07g of cetearyl alcohol, 38.5g of pentaerythritol tetra (ethyl hexanoate) and 0.04g of colorant into a heating tank, heating to 75 ℃, completely dissolving, homogenizing at a rotation speed of 500r/min for 8min to obtain a mixed solution;

and (3) cooling: and slowly stirring the microcapsule precursor solution A prepared in the heating, dissolving and homogenizing process at the stirring speed of 200r/min, and cooling to 30 ℃ to obtain the microcapsule-like precursor.

Example 3

A microcapsule-like precursor comprises the following raw materials: the skin care product comprises a solvent, a thickening agent and a skin conditioning agent, wherein in the embodiment, the solvent is 42.5g of dimeric siloxane and derivatives, the thickening agent is 34g of ozokerite, and the skin conditioning agent is 21.25g of hydrogenated lecithin, wherein the weight ratio of the solvent to the thickening agent to the skin conditioning agent is 1: 0.8: 0.5.

heating, dissolving and homogenizing: respectively putting 42.5g of dimeric siloxane and derivatives, 34g of ozokerite, 21.25g of hydrogenated lecithin and 0.13g of colorant into a heating tank, heating to 90 ℃, completely dissolving, homogenizing at the rotation speed of 1000r/min for 3min to obtain a mixed solution;

and (3) cooling: and slowly stirring the mixed solution obtained in the heating, dissolving and homogenizing process at the stirring speed of 100r/min, and cooling to 30 ℃ to obtain the microcapsule-like precursor.

Example 4

The difference from example 2 is that 38.5g of pentaerythritol tetrakis (ethyl hexanoate) was replaced with 19.25g of bisabolol and 19.25g of rose oil as the selected skin conditioner.

Example 5

The difference from example 2 is that an antioxidant and a preservative are further included in the step of heating, dissolving and homogenizing. In this example, 3.85g tocopherol (vitamin E) was used as the antioxidant, methyl hydroxybenzoate, phenoxyethanol, chlorphenesin, sodium benzoate, caprylhydroxamic acid, sorbic acid, methylisothiazolinone was used as the preservative, and 0.04g phenoxyethanol was used in this example, wherein the ratio of the solvent, thickener, skin conditioner, antioxidant and preservative was 1:0.5:1: 0.1:0.001.

Example 6

The difference from example 5 is that the ratio of solvent, thickener, skin conditioner, antioxidant and preservative in parts by weight is 1: 0.3: 0.5: 0.05: 0.0001; specifically, 38.5g of polydimethylsiloxane, 11.55g of cetearyl alcohol, 19.25g of pentaerythritol tetra (ethyl hexanoate), 0.385g of tocopherol (vitamin E) and 0.0385g of phenoxyethanol.

Example 7

The difference from example 5 is that the ratio of solvent, thickener, skin conditioner, antioxidant and preservative in parts by weight is 1: 0.8: 2: 0.3: 0.005; specifically, 38.5g of polydimethylsiloxane, 30.8g of cetearyl alcohol, 77g of pentaerythritol tetra (ethyl hexanoate), 11.55g of tocopherol (vitamin E) and 0.1925g of phenoxyethanol.

Example 8

The difference from example 5 is that 3.85g of tocopherol (vitamin E) antioxidant was replaced with 2.57g astaxanthin, 1.28g chamomile oil.

Example 9

The difference from the embodiment 5 is that the heating temperature is 100 ℃, the homogenizing speed is 200r/min, the homogenizing time is 10min, and the stirring speed is 50r/min in the cooling process.

Example 10

The difference from the embodiment 5 is that the heating temperature is 50 ℃, the homogenizing speed is 200r/min, the homogenizing time is 10min, and the stirring speed is 400r/min in the cooling process.

Comparative example 1

A commercially available microcapsule product purchased from tianmao flagship store official website, product name: jia xi emperor bee pose gold reconstituted honey (promotion package 5ml), and national makeup preparation advanced character J20175509. The physical state of the product is as follows: a transparent liquid with particles.

Comparative example 2

The difference from example 5 is that: the weight ratio of the solvent to the thickener to the skin conditioner to the antioxidant to the preservative is 1: 0.2: 0.3: 0.4: 0.005; specifically, 38.5g of polydimethylsiloxane, 7.7g of cetearyl alcohol, 11.55g of pentaerythritol tetra (ethyl hexanoate), 15.4g of tocopherol (vitamin E) and 0.1925g of phenoxyethanol.

Comparative example 3

The difference from example 5 is that: the weight ratio of the solvent to the thickener to the skin conditioner to the antioxidant to the preservative is 1: 0.9: 2.1: 0.01: 0.005; specifically, 38.5g of polydimethylsiloxane, 34.65g of cetearyl alcohol, 80.85g of pentaerythritol tetra (ethyl hexanoate), 0.385g of tocopherol (vitamin E) and 0.1925g of phenoxyethanol.

Examples 11 to 20

The examples 1 to 10 and the comparative examples 2 to 3 are respectively prepared into microcapsules, which are the examples 10 to 20 of the application, and the specific steps are as follows:

obtaining a capsule-like precursor solution: heating the quasi-microcapsule precursor to 75 ℃ to obtain a quasi-microcapsule precursor solution;

obtaining a constant temperature water phase: keeping deionized water at constant temperature of 45 deg.C as dispersed water phase, and continuously stirring in IKA stirrer (model: YJ0030) at stirring speed of 50-100 r/min;

and (3) preparing a finished product: slowly adding the prepared capsule-like precursor solution into the constant-temperature dispersed water phase, and slowly stirring until the microcapsule-like particles in the mixed solution whiten, thus completing the preparation.

The specific composition parameters are as follows in table 2:

table 2 feed parameters for preparative examples 11-20:

example 21

The difference from the embodiment 15 is that in the step of obtaining the capsule-like precursor solution, the temperature of the microcapsule-like precursor is raised to 50 ℃, and in the process of obtaining the constant temperature water phase, the constant temperature of the deionized water is 40 ℃.

Example 22

The difference from the embodiment 15 is that in the step of obtaining the capsule-like precursor solution, the temperature of the microcapsule-like precursor is raised to 80 ℃, and in the process of obtaining the constant temperature water phase, the constant temperature of the deionized water is 50 ℃.

Example 23

The difference from the embodiment 15 is that in the step of obtaining the quasi-microcapsule precursor solution, the temperature of the quasi-microcapsule precursor is raised to 90 ℃, and in the process of obtaining the constant temperature water phase, the constant temperature of the deionized water is 35 ℃.

Example 24

The microcapsule-like body is taken as a main characteristic functional raw material, and can be added into skin care products such as hand cream, face cream, facial mask, essence/essence, sun cream, eye cream, body lotion, toner, emulsion and the like, wherein the dosage of the microcapsule-like body in the skin care products is 2% -8%, and in the embodiment, the dosage is preferably 5%.

Comparative examples 4 to 5

Comparative examples 2 to 3 were prepared as microcapsules, respectively, and the preparation methods of examples 11 to 20, comparative examples 4 to 5 of the present application, were specifically prepared.

Product performance detection test

After the microcapsules prepared in examples 11 to 23 and comparative examples 4 to 5 were put into practice, stability tests and irritation tests were carried out together with comparative example 1.

And (3) stability test:

the stability test is a high-temperature and low-temperature storage stability test: equal amount of the quasi-capsule samples were taken as sample 1, sample 2 and sample 3. Sample 1 was used to perform a high temperature heat resistance test at a high temperature of 50 ℃ for one month; sample 2 was used for a cold resistance test at-18 ℃ for 3 months; sample 3 was left at room temperature and served as a reference for samples 1 and 2. Comparing physical properties such as appearance, viscosity, smell, pH value and the like of the sample 1 and the sample 3 which are subjected to the high-temperature test; the physical properties such as appearance, viscosity, odor, and pH were compared between sample 2 and sample 3 after the low temperature test, and the stability test results are shown in table 3.

Table 3 stability test results

Table 3 the test data show:

combining examples 11-23 and comparative example 1, it can be seen that the commercially available skin care products using microcapsule technology have changed physical properties to different degrees under high temperature and low temperature conditions, whereas the capsule-like products prepared from the capsule-like precursors of the present application have good stability under high temperature and low temperature conditions, and appearance phase and odor changes, viscosity, pH value and the like do not change, indicating that the capsule-like products of the present application have good stability.

In addition, in the preparation raw materials of examples 15 to 17, the weight ratio of the solvent, the thickener, the skin conditioner, the antioxidant and the preservative is 1:0.3 to 0.8: 0.5-2: 0.05-0.3: 0.0001 to 0.005, and in the preparation experiment process, the preparation raw materials of the comparative examples 4 to 5 are not in the range, the prepared microcapsule-like product has the condition of physical property change in different degrees under the conditions of high temperature and low temperature, the stability is poor, and the weight ratio of each component in the raw materials of the application is determined.

The test data of example 15, examples 20 to 22 and example 23 show that the mixing temperature of the microcapsule-like precursor and the dispersed aqueous phase affects the stability of the capsule-like product during the preparation of the capsule-like product from the capsule-like precursor, and the results show that the stability of the prepared capsule-like product is better when the temperature of the microcapsule-like precursor is 50 to 80 ℃ and the temperature of the dispersed aqueous phase is 40 to 50 ℃.

Irritation test

The irritation test of the application adopts a skin patch test, and the patch test is a dermatology routine test and is mainly used for skin allergy and irritation tests.

The detection method comprises the following steps: smearing the microcapsule-like product on a spot tester, then pasting the microcapsule-like product on the inner side of the upper arm of a tester, continuously pasting for 48 hours, removing the spot tester for 0.5 hour, and then carrying out first interpretation; the second interpretation was performed 24 hours after the plaque removal tester.

The testers of the test select 5 cosmetic workers with 1 year or more of working experience to carry out the test, and the testers carry out subjective and objective evaluation:

1) subjective evaluation: description of tingling, itching and burning sensations experienced by the test person when using the sample;

2) objective evaluation: erythema, papules, and blister states presented by the skin of the test subjects.

The test results are shown in tables 4 and 5:

table 4 objective evaluation results of irritation test:

table 4 description of detection markers:

-as negative reaction;

is there a + indicated the presence of suspicious responses (only mild erythema);

+ indicates a weak yang response (erythema, infiltration, possibly with a small number of papules);

+ indicates a strong yang response (erythema, infiltration, papules, blisters);

+ + + indicated a very strong response (erythema, marked infiltration, papules, blister blistering).

Table 5 subjective evaluation results of irritation test:

the detection result shows that: no irritation reaction exists; slight is no obvious irritant reaction.

The experimental data of tables 4-5 show that:

in combination with examples 11-20, it was found that the capsule-like products prepared from the capsule-like precursor of the present application are less irritating to human skin during use. The reason why the test person 3 had a certain sensation of warmth immediately after applying the capsule-like product of example 11 was presumed to be: the skin of the test person 3 was dry or the raw material of example 11 was not added with an antioxidant or preservative, which slightly affected the feeling of use of the product.

Combining with the example 15 and the examples 21 to 23, it can be seen that the mixing temperature of the microcapsule-like precursor and the dispersed water phase in the process of preparing the capsule-like product affects the irritation of the capsule-like product in the use process, and the results show that the irritation of the prepared capsule-like product is low or none when the temperature of the microcapsule-like precursor is 50 to 80 ℃ and the temperature of the dispersed water phase is 40 to 50 ℃ in the mixing process.

Product function detection test

This test uses examples 11-20 of the present application as functional test specimens for capsule-like products.

A detection instrument: skin hair tester innovation skin & hair analysis system (model: ASW-100);

the detection method comprises the following steps: before the product is used, a skin hair tester is adopted to detect the skin state; after the face is cleaned in each use, the quasi-capsule product is tested and smeared on the face skin of a tester, and is used for 30 days continuously in the morning and at night; the moisture content of the skin was measured by a skin moisture test pen at 10 am on day 30 after the product was used, and the skin condition was measured using a skin-hair tester.

The test testers selected 10 women in the same office with 1 year and over experience of cosmetics work and the age of 25-30 years for test (wherein, 10 face of the testers have color spots), and the testers perform subjective and objective evaluation, and the evaluation results are listed in Table 6.

Table 6 microcapsule function test results:

the skin condition of the skin was checked by the skin-hair tester 11, and the results are shown in fig. 1.

The experimental data in table 6 and figure 1 show that:

in conjunction with examples 11-20, it was found that the skin moisture content was increased to varying degrees in all subjects after 30 days of use. Due to the addition of the antioxidant and the preservative in the raw materials of the examples 15 to 18, the test result shows that the skin moisture content of the testers 10 to 13 is obviously improved; the weight ratio of solvent, thickener, skin conditioner, antioxidant and preservative for the microcapsule-like samples of example 15 was the optimum ratio for the materials of the present application, with the highest increase in moisture content exhibited by the panelist 10 during the test.

With reference to fig. 1, before the quasi-capsule product is used, the skin of a tester 11 is in a scaly shape, the texture of the skin is obvious, and the phenomenon of water shortage exists; after the product is used for 30 days, the skin lines are light and have a glossy feeling.

Combining the data of examples 19-20 and the evaluation of examples 19-20 by the testers 14 and 15, the increase of skin moisture content is lower, and the example 20 has sticky using feeling, because the preparation parameters range from 60 ℃ to 90 ℃, the homogenizing rotating speed is 300-1000r/min and the homogenizing time is 3-10min in the process of heating, dissolving and homogenizing when the microcapsule-like precursor is prepared; in the cooling process, the stirring speed is beyond 100-300 r/min'. Meanwhile, the preparation process of the precursor-like body can influence the functions and the use feeling of the subsequent capsule-like products.

The skin of the test subject 10 was subjected to the detection of facial spots, and the detection of facial spots was carried out before, after 2 weeks (14 days) and after 4 weeks (28 days) of the capsule samples of the type of example 15, respectively, and the spots were enlarged.

A detection instrument: the facial image analyzer, melanin and heme tester SSA (model: Mexameter MX 18).

With reference to fig. 2, as the using time increases, the area of the color spot on the face of the tester gradually decreases, which shows that the capsule-like product prepared by the method also has the effect of reducing the color spot.

The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.