CN114481441A - Nano-fiber mask base cloth containing fibroin, functional mask and preparation method of functional mask - Google Patents

Abstract

The invention discloses a nanofiber mask base cloth containing fibroin, a functional mask and a preparation method of the functional mask, and belongs to the technical field of skin care products. The silk peptide and polyvinyl alcohol are mixed to obtain spinning solution containing fibroin, and then a relatively mature and stable electrostatic spinning technology is adopted to produce the nano-fiber mask base cloth containing the fibroin, so that fibers with nano-grade diameters can be obtained; the nano-scale silk peptide contained in the facial mask is very easy to be fully absorbed and utilized by the face in the using process of the facial mask and has good biocompatibility; the added functional substances can be confined in the nano-fibers and released after meeting water, thereby playing a nursing role. The raw materials are green and natural, and the prepared mask base cloth has excellent performance parameters and good face fitting performance; the prepared functional facial mask can well protect and protect functional components in a solid state, and release the functional components after meeting water, so that the functional facial mask is easy to store, convenient to use and capable of realizing batch production.

Description

A kind of nanofiber facial mask base cloth containing silk protein, functional facial mask and preparation method thereof

technical field

The invention belongs to the technical field of skin care products, and in particular relates to a nanofiber facial mask base cloth containing silk protein, a functional facial mask and a preparation method thereof.

Background technique

The traditional mask is composed of two parts: the mask base layer and the mask essence. The common mask base fabric layer on the market is mainly non-woven fabrics. The fibers of non-woven fabrics are generally thicker, about a dozen microns, and the size of the facial skin grooves is between 50 and 60 nm, so the non-woven mask is skin-friendly and soft. Poor sex and poor fit with the face. Mask essence is easily contaminated during packaging and use, some active substances are easily oxidized and deteriorated in liquid state, and excess essence that cannot be absorbed by the skin also causes a waste of resources.

SUMMARY OF THE INVENTION

In order to solve the above problems, the present invention provides a nanofiber facial mask base cloth containing silk protein, a functional facial mask and a preparation method thereof. The raw materials are green and natural, the obtained facial mask base cloth has excellent performance parameters and good facial fit; The functional mask can well protect the functional components in a solid state, and release them after encountering water, which is easy to store and use, and can be mass-produced.

The present invention is achieved through the following technical solutions:

The invention discloses a preparation method of a nanofiber facial mask base cloth containing silk protein, comprising the following steps:

Step 1: dissolve the polyvinyl alcohol in deionized water to prepare a polyvinyl alcohol solution with a mass fraction of 10% to 12%; then add the silk peptide into the prepared polyvinyl alcohol solution to obtain a mixed solution, and the silk peptide in the mixed solution The quality of the polyvinyl alcohol is 10% to 20% of the quality of the polyvinyl alcohol;

Step 2: fully stir the mixed solution prepared in step 1 at a constant temperature until a uniform and transparent solution is formed, stand at room temperature and then defoam for standby to obtain a spinning solution;

Step 3: Electrospin the spinning solution, and the product is dried to obtain a nanofiber mask base cloth containing fibroin.

Preferably, the polyvinyl alcohol in step 1 is 1788 type, the molecular weight is 44.05, and the alcoholysis degree is 87.0%-89.0%.

Preferably, in step 2, the stirring is performed at 50-70° C. for 4-6 h.

Preferably, in step 2, the standing time is 2-3 hours.

Preferably, in step 3, the parameters of electrospinning include: the voltage is 14-20 kV, the flow rate is 0.4-1.0 mL/h, the receiving distance is 14-20 cm, the rotational speed of the roller is 100-700 r/min, and the ambient humidity is 30 %～40%, the temperature is 15～25℃; the drying conditions of the product are drying at 70～90℃ for 1～2h.

Further preferably, the electrospinning is performed simultaneously by using double needles, and the distance between the needles is 5-10 cm.

The fibroin-containing nanofiber facial mask base cloth disclosed by the invention has a gram weight of 10.91-12.73 g/m ² and a specific surface area of 2.68-6.29 m ² /g.

A preparation method of a functional nanofiber facial mask containing silk protein disclosed in the invention comprises the following steps:

Step 1: dissolve the polyvinyl alcohol in deionized water to prepare a polyvinyl alcohol solution with a mass fraction of 10% to 12%; then add the silk peptide into the prepared polyvinyl alcohol solution to obtain a mixed solution, and the silk peptide in the mixed solution The quality of the polyvinyl alcohol is 10% to 20% of the quality of the polyvinyl alcohol;

Step 2: Stir the mixed solution prepared in step 1 at 50-70° C. for 4-6 hours until a uniform and transparent solution is formed, stand for 2-3 hours at room temperature, and then deaerate for use to obtain a spinning solution; Add water-soluble functional substances to the silk liquid. The mass of the functional substances is 10% to 20% of the mass of the polyvinyl alcohol. After fully stirring at room temperature for 2 to 4 hours, let stand for 2 to 3 hours at room temperature and then defoamed for use. , to obtain functional spinning solution;

Step 3: Electrospin the functional spinning solution, and obtain a functional nanofiber mask containing silk protein after the product is dried, cut, shaped and sterilized.

Preferably, the functional substance is one or more of sodium hyaluronate, niacinamide, dipotassium glycyrrhizinate, kojic acid, anthocyanin and honeysuckle extract.

The functional nanofiber facial mask containing silk fibroin disclosed by the invention according to the above preparation method has a gram weight of 12.71-14.55 g/m ² , and can be completely dissolved and absorbed by the skin within 12-24 s after encountering water.

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

The invention discloses a preparation method of a nanofiber facial mask base cloth containing silk protein, which adopts polyvinyl alcohol solution, which has good biocompatibility and fibrillation film-forming properties, does not produce cytotoxicity, and is non-irritating to human skin. And a large number of hydroxyl groups of polyvinyl alcohol make it have good hydrophilicity; the spinning solution obtained by mixing silk peptide and polyvinyl alcohol contains silk protein, and then relatively mature and stable electrospinning technology is used to carry out nanofibers containing silk protein. In the production of mask base fabric, fibers with nanometer diameter can be obtained, which has better adhesion than the micrometer fiber base fabric produced by traditional spunlace method.

Further, the polyvinyl alcohol used in step 1 is 1788 type, the molecular weight is 44.05, and the alcoholysis degree is 87.0% to 89.0%. The alcoholysis degree and molecular weight of polyvinyl alcohol will directly affect the dissolution rate of the nanofiber mask base cloth, 1788 The nanofiber mask base cloth made of 100% polyvinyl alcohol can be quickly and completely dissolved in water, releasing nutrients, and users can enjoy the ultimate and rapid skin care experience.

Further, the stirring is performed at 50-70° C. for 4-6 hours. Since polyvinyl alcohol is insoluble in water at room temperature, increasing the temperature and prolonging the stirring time is conducive to the rapid formation of a homogeneous and stable polyvinyl alcohol solution.

Further, the voltage of electrospinning is 14-20kV, the flow rate is 0.4-1.0mL/h, the receiving distance is 14-20cm, the rotating speed of the roller is 100-700r/min, the ambient humidity is 30%-40%, and the temperature is 15～25℃. The electrospinning process is affected by the synergy of many factors, and the increase of the voltage is conducive to the electric field force to overcome the intermolecular force and surface tension of the spinning solution, and obtain fine and uniform fibers; when the flow rate increases, the spinning solution cannot be obtained in the high voltage electric field Sufficient stretching is not conducive to the formation of fibers with good morphology; too long receiving distance will cause the fibers to float around and affect the spinning efficiency; the surface of the roller will add a kind of winding drafting force, and the increase of the roller speed is beneficial to Form finer fibers; temperature and humidity mainly affect the spinning process by affecting the fluidity and volatilization of the solvent. It is necessary to optimize the spinning process parameters and explore the optimal spinning conditions for the formation of nanofibers.

Furthermore, using double needles for electrospinning at the same time can improve production efficiency; the distance between needles is 5 to 10 cm, and if the distance between needles is too close, the spinning jets will interfere with each other, affecting the distribution of nanofibers and nanofibers. Homogeneity of the fibrous membrane.

^The nanofiber facial mask base cloth containing fibroin prepared by the method disclosed in the present invention is light in weight and good in softness. The specific surface area of the mask is increased, and the specific surface area of the nanofiber mask base fabric is 2.68-6.29 m ² /g.

In the preparation method of the functional nanofiber facial mask containing silk protein disclosed in the invention, the added functional components are all water-soluble substances, which can be uniformly and stably dispersed in the mixed spinning solution, and after electrospinning, the functional substances are imprisoned In the nanofiber, it is released after contact with water, acting on the skin and playing a nursing role.

Further, the functional substance is one or more of sodium hyaluronate, nicotinamide, dipotassium glycyrrhizinate, kojic acid, anthocyanin and honeysuckle extract, which can be added according to actual needs to play a role in the corresponding skin. Nursing effect.

The functional nanofiber facial mask containing silk protein disclosed by the present invention by the above-mentioned method truly contains silk components, the nano-level silk peptide contained in the mask can be easily fully absorbed and utilized by the face during the use of the mask, and the silk protein has good The biocompatibility can promote metabolism while supplementing nutrients for the skin, making the skin moist, soft and shiny. Nanofibers have excellent characteristics such as large specific surface area and small porosity, and have excellent skin adhesion and good air permeability. The prepared nanofiber mask is solid, spray water, toner or essence water on the face before use, and then stick the nanofiber mask on the face, and the mask dissolves and releases the essence, which solves the waste of the mask essence to a certain extent. The problem is that the active ingredients and trace elements in the essence are effectively protected in the solid state and are not easy to be oxidized and deteriorated. The mask is non-toxic, non-irritating, natural and environmentally friendly, easy to store and easy to use. The gram weight is between 12.71 and 14.55g/m ² , which is light in weight and convenient for transportation and carrying. The larger porosity enables the mask to have a larger specific surface area, and it can load more functional substances under the same weight, thus showing better performance. hydrating, moisturizing, whitening and antioxidant properties. Functional substances are not easy to be oxidized and fail in solid state. After the mask meets water, it can be quickly dissolved within 12 to 24 seconds. The facial skin can quickly and efficiently absorb the released nano-level nutrients. The unique design of nanofiber mask with different functions is suitable for a wide range of applications.

Description of drawings

Fig. 1 is the physical map of the functional nanofiber facial mask containing silk protein obtained by the present invention;

Fig. 2 is the scanning electron microscope image of the functional nanofiber facial mask containing silk protein obtained in Example 1;

Fig. 3 is the scanning electron microscope image of the functional nanofiber facial mask containing silk protein obtained in Example 2;

Fig. 4 is the scanning electron microscope image of the functional nanofiber facial mask containing silk protein obtained in Example 3;

Fig. 5 is the scanning electron microscope image of the functional nanofiber facial mask containing silk protein obtained in Example 4;

FIG. 6 is a time chart of the dissolution of the functional nanofiber facial mask containing fibroin prepared by the present invention in water.

Detailed ways

Below in conjunction with embodiment, the present invention is described in further detail:

Silk, as the "Queen of Fibers", is widely used in the field of cosmetics. Due to its good biocompatibility and medical properties, it has a good development prospect in the mask industry. However, in fact, silk masks have always been wrongly defined. Many mask companies rely on silk. The concept of mask is falsely marketed, so that more than 80% of silk mask experiencers buy fake masks, and they have not experienced the real effect of silk mask. The survey shows that there are mainly three types of fake silk masks on the market: one is that the base cloth of the mask is made of silk and other fibers, and there is no silk protein in the mask essence; A small amount of silk protein is added to it, and it is packaged into a 100% silk mask; the third is a mask base cloth produced by imitating the structure of silk fiber mesh, and its material is generally cupro fiber.

The invention aims to develop a functional nanofiber facial mask that really contains silk protein.

The preparation method of the nanofiber facial mask base cloth containing silk protein comprises the following steps:

Step 1: dissolve the polyvinyl alcohol in deionized water to prepare a polyvinyl alcohol solution with a mass fraction of 10% to 12%; then add the silk peptide into the prepared polyvinyl alcohol solution to obtain a mixed solution, and the silk peptide in the mixed solution The quality of the polyvinyl alcohol is 10% to 20% of the mass of the polyvinyl alcohol; the polyvinyl alcohol is 1788 type, the molecular weight is 44.05, and the alcoholysis degree is 87.0% to 89.0%;

Step 2: fully stir the mixed solution prepared in step 1 at 50 to 70° C. for 4 to 6 hours to form a uniform and transparent solution, stand at room temperature for 2 to 3 hours, and then defoam for later use to obtain a spinning solution;

Step 3: electrospin the spinning solution, and the parameters of electrospinning include: the voltage is 14-20 kV, the flow rate is 0.4-1.0 mL/h, the receiving distance is 14-20 cm, and the rotational speed of the roller is 100-700 r/min , the ambient humidity is 30% to 40%, and the temperature is 15 to 25° C. The product is dried to obtain a nanofiber mask base cloth containing silk protein.

The preparation method of the functional nanofiber facial mask containing silk protein comprises the following steps:

Step 1: dissolve the polyvinyl alcohol in deionized water to prepare a polyvinyl alcohol solution with a mass fraction of 10% to 12%; then add the silk peptide into the prepared polyvinyl alcohol solution to obtain a mixed solution, and the silk peptide in the mixed solution The quality of the polyvinyl alcohol is 10% to 20% of the mass of the polyvinyl alcohol; the polyvinyl alcohol is 1788 type, the molecular weight is 44.05, and the alcoholysis degree is 87.0% to 89.0%;

Step 2: Stir the mixed solution prepared in step 1 at 50-70° C. for 4-6 hours until a uniform and transparent solution is formed, stand for 2-3 hours at room temperature, and then deaerate for use to obtain a spinning solution; Add functional substances to the silk liquid, and the mass of the functional substances is 10% to 20% of the mass of polyvinyl alcohol. After fully stirring at room temperature for 2 to 4 hours, let stand for 2 to 3 hours at room temperature and then defoam for use. Sex spinning solution;

Step 3: Electrospin the functional spinning solution. The parameters of the electrospinning include: the voltage is 14-20kV, the flow rate is 0.4-1.0mL/h, the receiving distance is 14-20cm, and the rotation speed of the roller is 100-700r /min, the ambient humidity is 30% to 40%, and the temperature is 15 to 25°C; it is preferable to use double needles for simultaneous electrospinning, and the distance between the needles is 5 to 10 cm; the product is dried to obtain functional fibroin containing fibroin. Nanofiber mask.

Example 1

Accurately weigh 0.6g of polyvinyl alcohol with an electronic balance and add it to 4.4g of deionized water to obtain a polyvinyl alcohol solution with a mass fraction of 12%, then weigh 0.06g of silk peptide and add it to the polyvinyl alcohol solution. Put it in a constant temperature magnetic stirrer and stir at 50°C for 6 hours until a homogeneous and transparent solution is formed, so that the silk peptide is fully dissolved in the polyvinyl alcohol solution, and the spinning solution is taken out and left at room temperature for 2 hours for defoaming. Add 0.06 g of nicotinamide to the spinning solution prepared in the first step, place the solution on a magnetic stirrer, stir at room temperature for 3 hours, and stand at room temperature for 2 hours for defoaming. Electrospinning was carried out on an electrospinning machine with a spinning voltage of 14kV, a flow rate of 0.4mL/h, a receiving distance of 14cm, a roller speed of 700r/min, an ambient humidity of 30%, a temperature of 25°C, and a distance between needles. 5 cm, the product was dried at 70 °C for 2 h, and the scanning electron microscope picture of the prepared nanofiber mask is shown in Figure 2.

Example 2

Accurately weigh 0.6g of polyvinyl alcohol with an electronic balance and add it to 4.4g of deionized water to obtain a polyvinyl alcohol solution with a mass fraction of 12%, then weigh 0.1g of silk peptide and add it to the polyvinyl alcohol solution. Place it in a constant temperature magnetic stirrer and stir at 60°C for 5 hours until a uniform and transparent solution is formed, so that the silk peptide is fully dissolved in the polyvinyl alcohol solution. Add 0.1 g of hyaluronic acid to the spinning solution prepared in the first step, place the solution on a magnetic stirrer, stir at room temperature for 2 hours, and stand at room temperature for 2 hours for defoaming. Electrospinning was carried out on an electrospinning machine with a spinning voltage of 20kV, a flow rate of 0.4mL/h, a receiving distance of 18cm, a roller speed of 300r/min, an ambient humidity of 40%, a temperature of 25°C, and a distance between needles. 10 cm, and the product was dried at 85 °C for 1.5 h. The SEM image of the prepared nanofiber mask is shown in Figure 3.

Example 3

Accurately weigh 0.55g of polyvinyl alcohol with an electronic balance and add it to 4.45g of deionized water to obtain a polyvinyl alcohol solution with a mass fraction of 11%, and then weigh 0.08g of silk peptide and add it to the polyvinyl alcohol solution. Put it in a constant temperature magnetic stirrer and stir at 70°C for 4 hours until a homogeneous and transparent solution is formed, so that the silk peptide is fully dissolved in the polyvinyl alcohol solution. Add 0.04g kojic acid and 0.04g dipotassium glycyrrhizinate to the spinning solution prepared in the first step, place the solution on a magnetic stirrer, stir at room temperature for 3 hours, and let stand for 3 hours at room temperature for defoaming. Electrospinning was carried out on an electrospinning machine, the spinning voltage was 16kV, the flow rate was 0.6mL/h, the receiving distance was 20cm, the roller speed was 300r/min, the ambient humidity was 35%, the temperature was 20°C, and the distance between the needles was 8 cm, and the product was dried at 90 °C for 1 h. The SEM picture of the prepared nanofiber mask is shown in Figure 4.

Example 4

Accurately weigh 0.5g of polyvinyl alcohol with an electronic balance and add it to 4.5g of deionized water to obtain a polyvinyl alcohol solution with a mass fraction of 10%, then weigh 0.1g of silk peptide and add it to the polyvinyl alcohol solution. Put it in a constant temperature magnetic stirrer and stir at 60°C for 5 hours until a uniform and transparent solution is formed, so that the silk peptide is fully dissolved in the polyvinyl alcohol solution. Add 0.1 g of honeysuckle extract to the spinning solution prepared in the first step, place the solution on a magnetic stirrer, stir at room temperature for 3 hours, and let stand for 2 hours at room temperature for defoaming. Electrospinning was carried out on an electrospinning machine, the spinning voltage was 20kV, the flow rate was 1.0mL/h, the receiving distance was 20cm, the roller speed was 100r/min, the ambient humidity was 30%, and the temperature was 15°C. Dry at 80°C for 1.5h. The SEM image of the prepared nanofiber mask is shown in Figure 5.

After testing, the base cloth weight of the prepared nanofiber facial mask containing fibroin is 10.91-12.73 g/m ² , and the specific surface area is 2.68-6.29 m ² /g.

The prepared functional nanofiber facial mask containing silk protein has a gram weight of 12.71-14.55 g/m ² .

Fig. 1 is a real photo of the functional nanofiber facial mask containing fibroin obtained by the present invention. As can be seen from the figure, the nanofiber facial mask is solid, has no obvious defects in appearance, is dense and uniform in thickness, and has good flexibility.

It can be seen from Figure 2 to Figure 5 that the functional nanofiber mask containing fibroin has a good microscopic appearance, no beads and spindles appear, the surface of the nanofibers is smooth and the diameter distribution is uniform, and the size is about 300nm, which is better than traditional non-woven fabrics. The mask has good adhesion, and the inside of the mask presents a three-dimensional network structure, which endows the nanofiber mask with certain strength and toughness. effect.

It can be seen from Figure 6 that the prepared functional nanofiber mask containing silk protein has good water solubility. In the picture, deionized water is evenly sprayed on the inside of the arm. The applied functional nanofiber mask is completely dissolved in 12s, releasing nano-level nutrients. Gently tap and massage until the skin is completely absorbed. The skin is obviously not dry and tight. Hydration. The skin moisture content was detected with a skin smart tester. It was found that before the mask was applied, the normal skin moisture content was about 25%. At the initial stage of applying the mask, the skin was infiltrated with deionized water and effective nutrients, and the skin moisture content instantly increased to 60%. % to 80%, with the extension of time, part of the deionized water volatilizes, and part of the deionized water and effective nutrients are absorbed by the skin. After the mask is applied for 15 minutes, the skin moisture content can still be maintained at about 40%.

Claims (10)

1. a preparation method of the nanofiber facial mask base cloth containing silk protein, is characterized in that, comprises the following steps: Step 1: dissolve the polyvinyl alcohol in deionized water to prepare a polyvinyl alcohol solution with a mass fraction of 10% to 12%; then add the silk peptide into the prepared polyvinyl alcohol solution to obtain a mixed solution, and the silk peptide in the mixed solution The quality of the polyvinyl alcohol is 10% to 20% of the quality of the polyvinyl alcohol; Step 2: fully stir the mixed solution prepared in step 1 at a constant temperature until a uniform and transparent solution is formed, stand at room temperature and then defoam for standby to obtain a spinning solution; Step 3: Electrospin the spinning solution, and the product is dried to obtain a nanofiber mask base cloth containing fibroin. 2. the preparation method of the nanofiber facial mask base cloth containing silk protein according to claim 1, is characterized in that, the polyvinyl alcohol in step 1 is 1788 type, molecular weight is 44.05, and alcoholysis degree is 87.0%～89.0% . 3 . The method for preparing a fibroin-containing nanofiber facial mask base cloth according to claim 1 , wherein, in step 2, the stirring is at 50-70° C. for 4-6 h. 4 . 4 . The method for preparing a fibroin-containing nanofiber facial mask base cloth according to claim 1 , wherein in step 2, the standing time is 2 to 3 hours. 5 . 5. The preparation method of the fibroin-containing nanofiber facial mask base cloth according to claim 1, wherein in step 3, the parameters of electrospinning include: the voltage is 14-20kV, and the flow rate is 0.4-1.0mL/ h, the receiving distance is 14~20cm, the roller speed is 100~700r/min, the ambient humidity is 30%~40%, and the temperature is 15~25℃; the drying conditions of the product are 70~90℃ for 1~2h. 6 . The method for preparing a fibroin-containing nanofiber facial mask base cloth according to claim 5 , wherein electrospinning is performed simultaneously by using double needles, and the distance between the needles is 5-10 cm. 7 . 7. The nanofiber facial mask base cloth containing fibroin prepared by the preparation method according to any one of claims 1 to 6, characterized in that the gram weight is 10.91-12.73 g/m ² and the specific surface area is 2.68-6.29 m ² /g. 8. a preparation method of the functional nanofiber facial mask containing silk protein, is characterized in that, comprises the following steps: Step 1: dissolve the polyvinyl alcohol in deionized water to prepare a polyvinyl alcohol solution with a mass fraction of 10% to 12%; then add the silk peptide into the prepared polyvinyl alcohol solution to obtain a mixed solution, and the silk peptide in the mixed solution The quality of the polyvinyl alcohol is 10% to 20% of the quality of the polyvinyl alcohol; Step 2: Stir the mixed solution prepared in step 1 at 50-70° C. for 4-6 hours until a uniform and transparent solution is formed, stand for 2-3 hours at room temperature, and then deaerate for use to obtain a spinning solution; Add water-soluble functional substances to the silk liquid. The mass of the functional substances is 10% to 20% of the mass of the polyvinyl alcohol. After fully stirring at room temperature for 2 to 4 hours, let stand for 2 to 3 hours at room temperature and then defoamed for use. , to obtain functional spinning solution; Step 3: Electrospin the functional spinning solution, and obtain a functional nanofiber mask containing silk protein after the product is dried, cut, shaped and sterilized. 9. The preparation method of the functional nanofiber facial mask containing silk protein according to claim 8, wherein the functional substances are sodium hyaluronate, niacinamide, dipotassium glycyrrhizinate, kojic acid, anthocyanin and One or more of honeysuckle extracts. 10 . The functional nanofiber facial mask containing fibroin prepared by the preparation method according to claim 8 or 9 , wherein the gram weight is 12.71-14.55 g/m ² , and it can be used within 12-24 s after encountering water. 11 . Completely dissolves and is absorbed by the skin.

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