CN111803387A

CN111803387A - Sustained-release moisturizing aerogel mask matrix and preparation method and application thereof

Info

Publication number: CN111803387A
Application number: CN202010561807.8A
Authority: CN
Inventors: 李圆; 张露; 陈骏佳; 谢东
Original assignee: Guangdong Institute of Bioengineering Guangzhou Cane Sugar Industry Research Institute
Current assignee: Guangdong Institute of Bioengineering Guangzhou Cane Sugar Industry Research Institute
Priority date: 2020-06-18
Filing date: 2020-06-18
Publication date: 2020-10-23
Anticipated expiration: 2040-06-18
Also published as: CN111803387B

Abstract

The invention discloses a slow-release moisturizing aerogel mask matrix and a preparation method and application thereof, wherein the aerogel mask matrix comprises 0.5-10% by mass of a matrix solution, a water-retaining agent, a coagulant and aerogel powder. The mask matrix disclosed by the invention realizes functionalization by selecting a specific water-retaining agent and a specific coagulator to adjust the flexibility and transparency of the mask matrix, and realizes slow release of effective functional components by regulating the addition amount and the type of aerogel micro powder, so that the obtained aerogel mask matrix can load different active functional substances, has the functions of heat preservation, moisture preservation and slow release and control, is strong in use comfort, simple in preparation method, green and environment-friendly in material source, and is suitable for the fields of beauty, medicine, health care and the like.

Description

Sustained-release moisturizing aerogel mask matrix and preparation method and application thereof

Technical Field

The invention relates to the technical field of gel preparation. More particularly, relates to a sustained-release moisturizing aerogel mask matrix and a preparation method and application thereof.

Background

The patch type facial mask is a common daily chemical product, is often used as a skin health-care product and is matched with other skin-care ingredients for use, has the functions of whitening, resisting aging, removing scars and the like, and is one of daily chemical products which are most popular with modern people. Compared with the common non-woven fabric facial mask, the hydrogel facial mask has many advantages, such as crystal clear surface, good glossiness, good skin-friendly feeling, ice-cold feeling, and strong water retention and moisture retention capacity, and common hydrogel facial mask base materials mainly comprise collagen, sodium alginate, chitosan, polyvinyl alcohol (PVA) and the like, are all natural polymers and artificially synthesized green polymer materials, are harmless to the body, and have no pollution to the environment after being used.

Patent CN201610096094.6 provides a hydrogel mask matrix and a preparation method thereof, and the obtained matrix material is uniform, good in glossiness and beautiful in jade texture; the hydrogel mask has the advantages that the surface viscosity and the mechanical strength are appropriate, the film-forming property and the stretchability meet requirements, the peeling integrity is good, the hydrogel mask is single in function, the temperature is too low when the hydrogel mask is used in winter, the heat preservation effect is insufficient, the irritation to the face is strong, the slow release performance is poor, the pursuit of people for face care, particularly for the functionality and the experience of the mask product is increased day by day, the common hydrogel mask cannot meet the requirements of the existing beauty market, and therefore, the development of a multifunctional high-strength mask substrate is urgently needed, and the functions of heat preservation, moisture preservation and slow and controlled release of effective components are realized.

Disclosure of Invention

The invention aims to provide a sustained-release moisturizing aerogel mask matrix and a preparation method and application thereof.

It is a primary object of the present invention to provide an aerogel film substrate.

Another object of the present invention is to provide a method for preparing the above aerogel facial film matrix.

It is a further object of the present invention to provide the use of the aerogel facings substrates described above.

In order to achieve the purpose, the invention is realized by the following scheme:

the invention provides an aerogel mask matrix which comprises the following components:

0.5-10% of matrix aqueous solution, a water-retaining agent, a coagulant and aerogel powder; wherein the matrix is polyvinyl alcohol, sodium alginate or chitosan; the water-retaining agent is carboxymethyl cellulose or hydroxypropylA base cellulose; the coagulant is one or more of konjac gum, carrageenan or gelatin; the aerogel powder is SiO₂、Al₂O₃Or TiO₂。

The raw materials adopted by the invention are green natural polymers or artificially synthesized inorganic materials, the raw materials are green and safe, the mask matrix has super-strong water retention capacity due to the introduction of a specific water retention agent, the mask matrix has super-strong load performance and heat preservation and moisture preservation performance due to the introduction of aerogel particles, meanwhile, the release of active ingredients is controlled through the structure and the addition of a porous aerogel material, the release speed can be controlled by the introduction of the specific water retention agent, the aerogel mask matrix achieves high skin-friendly feeling and high strength, the obtained aerogel mask matrix can be timely temperature-regulated according to the skin temperature of a human body, in addition, the flexibility and the transparency of the mask matrix are regulated through the addition of the water retention agent and a coagulating agent, and the obtained aerogel mask has the sustained and controlled release performance through the functionalization of an aerogel regulation and control wall material. The mask substrate greatly improves the user experience, widens the functions of the gel mask and has important application value.

The aerogel powder used in the invention is inorganic aerogel SiO₂，Al₂O₃，TiO₂The release of the loaded functional micromolecules can be effectively controlled by controlling the using amount of the aerogel powder, the heat preservation and moisture preservation effects are achieved, and the prepared mask matrix product can be repeatedly used.

Preferably, the mass ratio of the matrix solution to the water-retaining agent to the coagulant to the aerogel powder is 1: 0.001-0.2: 0.001-0.2: 0.01 to 0.2.

Further preferably, the mass ratio of the matrix solution to the water-retaining agent to the coagulant to the aerogel powder is 1: 0.005-0.1: 0.005-0.1: 0.1 to 0.2.

Further preferably, the mass ratio of the matrix solution to the water-retaining agent to the coagulant to the aerogel powder is 1: 0.01-0.1: 0.01-0.1: 0.1 to 0.2.

Most preferably, the mass ratio of the matrix solution to the water-retaining agent to the coagulant to the aerogel powder is 1: 0.07: 0.1: 0.2.

preferably, in the coagulant, the glucomannan content of the konjac glucomannan is 40-90%. The higher the glucomannan content in the coagulant is, the higher the viscosity is, the higher the gel strength after gel formation is, and otherwise, the smaller or no gel is formed, so that the coagulant is one of the key factors for preparing the hydrogel mask.

Preferably, the molecular weight of the carrageenan is greater than 20 ten thousand.

Preferably, the relative molecular mass of the water retaining agent is 90000-250000. The larger the relative molecular mass of the water-retaining agent is, the larger the viscosity is, and the longer the molecular chain is, so that the water absorption rate of the water-retaining agent is increased, and the water-retaining property of the gel mask matrix is ensured. Meanwhile, the viscosity determines the fluidity and uniformity of the original mask solution, and greatly influences the preparation process.

More preferably, the relative molecular mass of the water retaining agent is 150000-250000.

Preferably, the degree of substitution of the water retaining agent is 0.7-1.2. The substitution degree of the water-retaining agent determines the water solubility of the water-retaining agent, and the difficulty and the easiness of the preparation process of the hydrogel mask matrix can be influenced.

The invention also provides a preparation method of the aerogel surface film matrix, which specifically comprises the following steps:

s1, adding a water-retaining agent into a matrix water solution, and fully dispersing to prepare a mixed suspension;

s2, sieving the coagulant by a 40-120-mesh sieve, adding the coagulant into the mixed suspension obtained in the step S1, and fully dispersing to prepare a mixed solution;

s3, sieving the aerogel powder by a sieve of 40-120 meshes, adding the aerogel powder into the mixed solution obtained in the step S2, uniformly mixing, heating, cooling and forming a film to obtain the aerogel surface film matrix.

The aerogel mask matrix is prepared by adopting a method of heating, dissolving, mixing and then cooling and forming, different bio-based materials are used as matrix raw materials, water retention agents and coagulants are added, the granularity of the coagulants is controlled to enable the coagulants to have the optimal water solubility, the preparation process of the aerogel mask matrix is facilitated, aerogel powder is added after the coagulants are fully and uniformly mixed, microwave-assisted heating is carried out to a certain temperature, and then cooling is carried out to form a film, so that the obtained aerogel mask matrix has a crystal clear surface, good glossiness, and super-strong water retention capacity and heat-preservation controlled-release performance. Compared with the existing common hydrogel facial mask, the preparation method is quick and simple, does not adopt a repeated freezing and thawing method, and is prepared by one-time heating, dissolving, cooling and forming.

Preferably, the specific preparation method of the aqueous matrix solution may be: adding the matrix raw material into deionized water, and fully dispersing and dissolving the matrix raw material on a high-speed dispersion machine at room temperature to prepare transparent solution.

Preferably, the heating in step S3 is heating at 85-100 ℃ for 5-15 min.

Most preferably, the heating of step S3 is heating at 95 ℃ for 10 min.

Preferably, the cooling in step S3 is cooling at 15-30 ℃ for 2-10 min.

Most preferably, the cooling of step S3 is cooling at 25 ℃ for 2 min.

The invention also claims the application of the aerogel mask matrix in the preparation of a patch mask or a skin application product.

The skin application product can be wound repair, skin health products, such as eye patches, T-membranes, etc.

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

the preparation process is simple and convenient, the prepared raw materials are environment-friendly green materials, the mechanical property, the water retention property and the controlled slow release property of the mask matrix are regulated and controlled by controlling the types and the adding amounts of the water retention agent, the coagulating agent and the aerogel, the wet film strength of the obtained aerogel mask matrix is large (more than or equal to 0.2MPa), the water absorption multiplying power of a dry film is more than or equal to 20 times, and the aerogel mask matrix has the characteristics of super-strong load capacity, heat preservation and moisture retention properties, easiness in loading of functional substances, slow release of functional substances and wide application in the fields of beauty treatment, medicine, health care and the like.

Drawings

Fig. 1 is a flow chart of the preparation of an aerogel mask.

Fig. 2 is a diagram of the exhibition and use effects of the aerogel mask product.

Detailed Description

The invention is further described with reference to the drawings and the following detailed description, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.

Unless otherwise indicated, reagents and materials used in the following examples are commercially available.

EXAMPLES 1-11 preparation of aerogel facemask matrices

1. Material

Taking 100g of total aerogel surface film matrix raw material, wherein the component usage ratio of each aerogel surface film matrix is shown in table 1:

TABLE 1

In the table above, the degree of substitution of the water-retaining agent in examples 1 to 3 was 0.7; the degree of substitution of the water-retaining agent in examples 4 to 6 was 1; the degree of substitution of the water-retaining agent in examples 7 to 9 was 1.1; the degree of substitution of the water-retaining agent in examples 10 to 11 was 1.2.

The relative molecular mass of the water retention agent in examples 1 to 3 is less than 90000; the relative molecular mass of the water-retaining agent in examples 4 to 6 was 90000 to 150000; the water-retaining agent in examples 7 to 9 had a relative molecular mass of 150000 to 200000; in examples 10 to 11, the relative molecular mass of the water-retaining agent was 200000 to 250000.

The glucomannan content of the coagulant konjac glucomannan of examples 1 and 3 was 40%; the konjac glucomannan content of the konjac glucomannan of examples 5 to 9 was 60%; the glucomannan content of the coagulant konjac glucomannan of example 11 was 90%.

The matrix water solution is prepared by adding matrix raw materials into deionized water, and fully dispersing and dissolving the matrix raw materials on a high-speed dispersion machine at room temperature to prepare transparent solution. The mass fraction of the polyvinyl alcohol solution is 0.5 percent; the mass fraction of the sodium alginate solution is 5 percent; the mass fraction of the chitosan solution is 10 percent.

The molecular weight of the carrageenan used in the above examples was greater than 20 million.

2. The preparation method of gel facial mask matrix is shown in figure 1

s2, sieving the coagulant through a 120-mesh sieve for later use, adding the coagulant into the mixed suspension obtained in the step S1, and fully dispersing to obtain a mixed solution;

s3, sieving the aerogel powder with a 120-mesh sieve for later use, adding the aerogel powder into the mixed solution obtained in the step S2, uniformly mixing, heating to 95 ℃, keeping the temperature for 10min, cooling at 25 ℃ for 2min, and forming a film to obtain the aerogel surface film matrix.

Example 12 aerogel topcoat matrix Performance characterization

1. Experimental methods

(1) Water absorption and retention performance:

the water retention performance comprises water retention time and water absorption rate, the water retention time is the time when the weight loss rate of the tested mask exceeds 5 percent at normal temperature, and the water absorption rate calculation method comprises the following steps: putting the mask sample into an oven for drying overnight at 80 ℃ for later use, precisely weighing 0.2g of dry mask, putting the dry mask into a beaker containing deionized water, soaking for 1 hour, taking out, naturally hanging for 30 minutes, precisely weighing by a ten-thousand-position balance, calculating the water absorption rate and the side reaction water retention property by using the weight of the mask before and after water absorption, and calculating according to the following formula.

Q＝(G₂-G₁)/G₁

In the formula: q is the water absorption rate; g₂The mass of the film behind the water absorption; g₁The water absorption front film quality.

(2) Testing the slow release performance:

the drug slow-release performance of the mask adopts a simulation method, 5-Fluorouracil (5-Fluorouracil) is used as a target slow-release medicament, 8mg/mL of 5-Fluorouracil is added in the preparation process of the mask, and then the surface of the prepared mask is washed to remove more drugs. Weighing 1g of wet facial mask containing the medicine, adding the wet facial mask into 10ml of Phosphate Buffered Saline (PBS) with the pH value of 7.2, oscillating for 2 hours at room temperature, testing the absorption value of the solution at the position with the wavelength of 271nm by using an ultraviolet spectrophotometer, and calculating the concentration of 5-fluorouracil by using a standard curve, thereby calculating the slow release performance of the facial mask on the medicine.

(3) Testing the heat preservation effect:

the heat preservation effect test method comprises a direct test and an indirect test, wherein the direct test is to directly paste the mask on the skin, and the heat preservation performance of the sensory mask after being pasted is considered to be excellent, good and poor; the indirect testing method is to wrap the mask on the surface of a glass bottle filled with 37 ℃, and test the descending speed of the temperature of water in the glass bottle along with time by using a temperature measuring gun, so that the side surface reflects the heat preservation performance, and the grades are excellent, good and poor.

(4) Testing the wet film strength:

the prepared wet mask is cut into a dumbbell shape by a cutter, and the tensile strength of a mask sample is tested by an electronic stretching device, so that the numerical value of the wet film strength is obtained, wherein the unit is MPa.

2. Results of the experiment

The results of the performance tests for each sample are shown in table 2.

TABLE 2

The slow release performance test result is as follows: the ultraviolet spectrophotometer tests the absorption value of the solution at the position with the wavelength of 271nm and calculates the corresponding concentration, tests the slow release test result of the 5-fluorouracil by the facial mask matrix, and the slow release performance is ranked as follows in sequence: examples 8 > 9 > 10 > 7 > 5 > 3 > 11 > 6 > 2 > 4 > 1. Thus combining water absorption and retention properties, thermal insulation properties, wet film strength, and sustained release properties, example 8 is the best mask base component addition ratio, followed by examples 7, 9, and 10, followed by examples 1, 2, 3, 4, 5, 6, and 11.

Example 13 high Strength aerogel mask with sustained Release moisturizing

1. The composition of each aerogel facing film matrix was the same as in example 8, taking a total of 100g of aerogel facing film matrix starting material.

2. Adding a matrix material into water to prepare a matrix aqueous solution, adding a water-retaining agent into the matrix solution, and fully dispersing to prepare a mixed suspension; sieving the coagulant with a 120-mesh sieve, adding the coagulant into the mixed suspension liquid, and fully dispersing to prepare a mixed solution; sieving aerogel powder with a 120-mesh sieve, dropwise adding 0.1-5% of essence relative to the mass of the mask matrix raw material into the aerogel powder, stirring with a glass rod to uniformly mix the materials, adding the aerogel powder containing the essence into the mixed solution, uniformly mixing, heating to 95 ℃, keeping the temperature for 10min, cooling at room temperature for 2min, and forming a film to obtain the aerogel mask adsorbing the essence, wherein the obtained aerogel mask product is shown in figure 2.

2. Trial population

40 capital deep mask users are recruited as professional judgment groups to intensively, professionally and seriously experience each trial product and give objective opinions.

The age group distribution of the subjects at this time: 25% of 20-25 years old; 20% of 25-30 years old; 40% of 30-40 years old; age 40 to 15%.

3. Trial results

(1) 85% of the testers think that the facial mask has good water retention effect and strong smooth feeling, the facial temperature is kept at about 37 ℃ when the facial mask is used in winter, the comfort is high, and the facial mask does not have any skin pricking feeling when being applied and can also be suitable for sensitive skin.

(2) Compared with the common high-price brand hydrogel mask: 70% of the experimenters believe that compared with high-price brand products (a snail hydrogel mask, a Korean water acupuncture mask and a French cardamom essence mask), the aerogel mask provided by the invention has little or even better experience feeling.

Comparative examples 1 to 5

1. Experimental Material

The total amount of 100g of aerogel surface film matrix raw material was taken, and the components of each aerogel surface film matrix are shown in table 3:

TABLE 3

Wherein the degree of substitution of the water-retaining agent in comparative examples 1 to 2 is 0.6; the degree of substitution of the water-retaining agent in comparative examples 3 to 5 was 1.3.

In comparative examples 1-2, the konjac glucomannan content was 30%; in comparative examples 3 to 5, the konjac glucomannan content was 95%.

In comparative examples 1 to 2, the relative molecular mass of the hydroxypropylcellulose was 80000; the relative molecular mass of the hydroxypropyl cellulose in comparative examples 3 to 5 was 260000.

The preparation of the matrix solution is that the matrix raw material is added into deionized water, and fully dispersed and dissolved on a high-speed dispersion machine at room temperature to prepare transparent solution. The mass fraction of the prepared corn starch solution is 1 percent; the mass fraction of the chitosan solution is 1 percent.

2. The aerogel film substrates were prepared according to the same methods as in examples 1 to 11.

3. Performance testing

The test method is the same as examples 1 to 11, and the specific test results are shown in Table 4.

TABLE 4

The slow release performance test result is as follows: comparative examples 1 to 5 have inferior results of the sustained-release test of 5-fluorouracil to those of examples 1 to 11, because the strength of the wet membrane and the water retention time are relatively poor and the membrane loading capacity is relatively poor in the comparative examples, the amount of 5-fluorouracil sustained-released into the buffer solution is small, most of the 5-fluorouracil has been washed away, and the obtained sustained-release effect is biased.

Comparative example 6

1. Experimental Material

The composition of each aerogel facing film matrix was the same as in example 8, taking a total of 100g of aerogel facing film matrix starting material.

2. Preparation method

S1, adding a base material, a water-retaining agent and a coagulant into water to prepare a mixed solution;

s2, adding aerogel powder into the mixed suspension obtained in the step S1 to prepare a mixed solution;

and S3, heating to 95 ℃, quickly pouring into a mold, and cooling to form a film, thus obtaining the aerogel mask matrix.

3. Results of the experiment

According to the aerogel mask matrix prepared by the method, firstly, a matrix material is insufficient in dissolving solution, insoluble particles are generated, especially PVA and a water-retaining agent are easy to form wrapping particles, so that the mask is opaque, and meanwhile, aerogel powder is not sieved, so that the touch feeling of the mask is influenced due to overlarge particles, the wet film strength, the aerogel powder falling and the like are caused.

The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims

1. An aerogel mask substrate, wherein the mask substrate comprises the following components: 0.5-10% of matrix aqueous solution, a water-retaining agent, a coagulant and aerogel powder by mass;

wherein the matrix is polyvinyl alcohol, sodium alginate or chitosan; the water-retaining agent is carboxymethyl cellulose and/or hydroxypropyl cellulose; the coagulant is one or more of konjac gum, carrageenan or gelatin(ii) a The aerogel powder is SiO₂、Al₂O₃Or TiO₂。

2. The aerogel facefilm substrate of claim 1, wherein the mass ratio of the substrate solution, water retention agent, coagulant, and aerogel powder is 1: 0.001-0.2: 0.001-0.2: 0.01 to 0.2.

3. The aerogel facefilm substrate of claim 2, wherein the mass ratio of the substrate solution, water retention agent, coagulant, and aerogel powder is 1: 0.005-0.1: 0.005-0.1: 0.1 to 0.2.

4. The aerogel mask matrix of claim 1, wherein the konjac glucomannan content of the konjac gum is 40-90%.

5. The aerogel facial film matrix according to any of claims 1 to 4, wherein the relative molecular mass of the water retaining agent is 90000 to 250000.

6. The aerogel facial film substrate according to any of claims 1 to 4, wherein the degree of substitution of the water retaining agent is 0.7 to 1.2.

7. The aerogel facefilm matrix of any of claims 1-6, prepared by a process comprising the steps of:

s1, adding a water-retaining agent into a matrix solution, and fully dispersing to prepare a mixed suspension;

8. The aerogel mask matrix of claim 7, wherein the heating of step S3 is performed at 85-100 ℃ for 5-15 min.

9. The aerogel mask matrix of claim 7, wherein the cooling in step S3 is performed at 15-30 ℃ for 2-10 min.

10. Use of the aerogel mask matrix of any of claims 1-9 in the preparation of a patch mask or skin application product.