CN109431821B

CN109431821B - Nano-fiber mask containing opal shale and preparation method thereof

Info

Publication number: CN109431821B
Application number: CN201811603339.5A
Authority: CN
Inventors: 张显华; 于宾; 娄辉清; 冯向伟; 何闯; 胡卓; 李佳欣; 宗佩佩
Original assignee: Henan Institute of Engineering
Current assignee: Hangzhou Yasheng Biological Technology Co ltd; Yami Technology Guangzhou Co ltd
Priority date: 2018-12-26
Filing date: 2018-12-26
Publication date: 2021-07-16
Anticipated expiration: 2038-12-26
Also published as: CN109431821A

Abstract

The invention discloses an opal shale-containing nanofiber mask which is prepared from the following raw materials in parts by mass: 2-14% of polyvinyl alcohol, 1-10% of polyethylene glycol, 1-40% of sericin, 0.01-1% of opal shale and the balance of deionized water. Uniformly dispersing opal shale in a polyvinyl alcohol, polyethylene glycol and sericin blended solution by an ultrasonic generator, and preparing the nano-fiber facial mask containing the opal shale by using a non-woven fabric substrate for the facial mask as a receiving screen through an electrostatic spinning technology. The nanofiber facial mask provided by the invention has the advantages of high specific surface area and super strong adsorption capacity, can thoroughly remove dirt and grease in the deep layer of the skin, has the effect of keeping the skin in a fully clean state, can whiten the skin, and greatly improves the convenience in use and the comfort level compared with the existing cleaning facial mask.

Description

Nano-fiber mask containing opal shale and preparation method thereof

Technical Field

The invention relates to the technical field of facial masks, and particularly relates to a nano-fiber facial mask containing opal shale and a preparation method thereof.

Background

With the increasing living standard and the increasing health pursuit of people, and the rapid development of dermatology, more and more people begin to care skin and pay attention to the quality and functionality of cosmetics. The facial mask is a cosmetic for caring facial skin, and can be applied to face by user, and kept on face for a long time to obtain good skin caring effect.

The existing cleaning facial mask mainly comprises a peel-off type facial mask, a smearing type facial mask and a patch type facial mask. The peel-off cleansing facial mask is not suitable for frequent use because it causes large irritation and damage to the skin during peeling, and tends to cause large pores and loose skin. The smearing type cleaning facial mask mainly takes curry jelly and paste as main materials, has strong cleaning force, is easy to crack and difficult to clean in the cleaning process, needs to continuously rub and pull the face, and is easy to cause the phenomena of irritation, intolerance to skin, reddish dryness of the face and the like after long-term use. The patch type cleaning facial mask mainly adopts a black facial mask, bamboo charcoal components with adsorbability are attached to woven cloth and are attached to the face to permeate the skin for a period of time, so that the adsorption function and the skin care process in a short time are achieved, the skin irritation is small, but because the pore structure of the bamboo charcoal is in a grid shape, the fiber porosity is low in the process of preparing the facial mask, the capability of adsorbing dirt in pores is poor, and the cleaning force is weak.

Disclosure of Invention

Aiming at the problems of insufficient cleaning force, large skin irritation, poor use experience and inconvenient cleaning of the existing cleaning facial mask, the invention aims to provide the nanofiber facial mask which can thoroughly clean deep dirt and grease of the skin, is mild, does not irritate and is convenient to use.

The invention is realized by the following technical scheme:

the nano-fiber mask containing the opal shale is prepared from the following raw materials in parts by mass: 2-14% of polyvinyl alcohol, 1-10% of polyethylene glycol, 1-40% of sericin, 0.01-1% of opal shale and the balance of deionized water.

Further, the polyvinyl alcohol is PVA1797 type, and the alcoholysis degree is 96.0-98.0%.

Further, the molecular weight of the polyethylene glycol is 2000-10000.

A preparation method of a nanofiber mask containing opal shale comprises the following steps:

step one, preparing a polyvinyl alcohol, polyethylene glycol and sericin blending solution: respectively dissolving polyvinyl alcohol and polyethylene glycol in distilled water, magnetically stirring at 80 + -5 deg.C for more than 8 hr to obtain solution, mixing the two solutions at a certain proportion, cooling, adding sericin, dissolving in 50-60 deg.C water bath for 4 hr, and cooling to obtain polyvinyl alcohol, polyethylene glycol, and sericin blended solution;

step two, preparing electrostatic spinning solution: starting an ultrasonic generator, adding opal shale into the polyvinyl alcohol, polyethylene glycol and sericin blending solution, performing ultrasonic treatment at the power of 220-;

step three, preparing the nano-fiber mask containing the opal shale: and (3) preparing the nano-fiber mask containing the opal shale by using a non-woven fabric substrate for the mask as a receiving screen through an electrostatic spinning technology.

Furthermore, the electrostatic spinning process conditions are that the electrostatic high voltage is 5-40kV, the distance is 5-25cm, and the speed is 0.15ml/h-1.5 ml/h.

The opal shale is rich in various benthic biological components and mineral substances, is necessary for human skin, has a special nano-pore structure, has extraordinary adsorption capacity, can thoroughly remove dirt and grease in deep layers of the skin, and keeps the skin in a fully clean state so as to further absorb other nutritional skin-care components.

Polyvinyl alcohol is a water-soluble high-molecular polymer with wide application, has good water solubility, film-forming property, adhesive force, excellent oil resistance, solvent resistance and other properties, is nontoxic and tasteless, has no irritation to skin, and does not cause skin allergy.

The main component of sericin is serine, and in addition, aspartic acid, glutamic acid, alanine, and glycine. As a natural protein, the biocompatibility and affinity of sericin have been recognized. The sericin has biological characteristics of moisture preservation, antibiosis, antioxidation, anticoagulation, promotion of cell adhesion and proliferation and the like, and has good effect of promoting cell growth at burn or wound. Moreover, sericin has hydrophilicity and degradability, and is an ideal biomedical material.

Polyethylene glycol (PEG) is non-toxic and non-irritant, has good water solubility and good intermiscibility with a plurality of organic matter components, can obtain larger phase change enthalpy through the transformation from an amorphous state to a crystalline state at normal temperature, and can be absorbed, stored and released in a latent heat form to be used as a phase change energy storage functional group.

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

(1) according to the nano-fiber mask containing the opal shale, the nano-fibers obtained through electrostatic spinning have extremely high specific surface area and high porosity, meanwhile, the opal shale is uniformly distributed on the surface and inside of the fibers, aggregation does not occur, the nano-fiber mask is firmly combined with the nano-fibers, the nano-fibers are not easy to lose in the preparation and use processes, and the adsorption capacity is ultra-strong;

(2) according to the nano-fiber mask containing the opal shale, the added sericin has excellent effects of humidifying, moisturizing, biocompatibility and oxidation resistance, and can promote cell adhesion and proliferation, and has a natural antibacterial effect, so that the nano-fiber mask containing the opal shale can play the roles of diminishing inflammation and resisting allergy while being deeply cleaned, has the effects of humidifying and moisturizing, can prevent skin dryness and pruritus, can inhibit skin melanin formation, and plays a role in whitening, amino acid in sericin can be absorbed by skin, can supplement nutrition, can shrink pores, and can keep the skin white, soft, smooth and elastic;

(3) the nano-fiber mask containing the opal shale is prepared by adopting an electrostatic spinning technology, the fine structure of fibers can be effectively regulated, and both the opal shale and sericin have natural antibacterial effects, so that no preservative is required to be added, the cost is low, the nano-fiber mask is mild and non-irritating, and only after skin is cleaned in use, clear water is used for spraying the nano-fiber mask on the face to directly apply the nano-fiber mask on the face.

Drawings

Fig. 1 is a scanning electron microscope image of the nano-fiber mask containing opal shale prepared in example 2.

Detailed Description

To further illustrate the technical means and effects of the present invention, the following detailed description is given with reference to the accompanying drawings and specific embodiments.

Example 1

The nano-fiber mask containing the opal shale is prepared from the following raw materials in parts by mass: 12% of polyvinyl alcohol, 1% of polyethylene glycol, 25% of sericin, 0.02% of opal shale and the balance of deionized water.

Further, the molecular weight of the polyethylene glycol is 10000.

step two, preparing electrostatic spinning solution: starting an ultrasonic generator, adding opal shale into the polyvinyl alcohol, polyethylene glycol and sericin blended solution, performing ultrasonic treatment at the power of 220W for 1h to uniformly disperse the opal shale to obtain an electrostatic spinning solution;

Example 2

The nano-fiber mask containing the opal shale is prepared from the following raw materials in parts by mass: 8% of polyvinyl alcohol, 2% of polyethylene glycol, 30% of sericin, 0.06% of opal shale and the balance of deionized water.

Further, the molecular weight of the polyethylene glycol is 4000.

step two, preparing electrostatic spinning solution: starting an ultrasonic generator, adding opal shale into the polyvinyl alcohol, polyethylene glycol and sericin blended solution, performing ultrasonic treatment at the power of 240W for 0.7h to uniformly disperse the opal shale to obtain electrostatic spinning solution;

Example 3

The nano-fiber mask containing the opal shale is prepared from the following raw materials in parts by mass: 4% of polyvinyl alcohol, 10% of polyethylene glycol, 13% of sericin, 0.8% of opal shale and the balance of deionized water.

Further, the molecular weight of the polyethylene glycol is 2000.

step two, preparing electrostatic spinning solution: starting an ultrasonic generator, adding opal shale into the polyvinyl alcohol, polyethylene glycol and sericin blended solution, performing ultrasonic treatment at the power of 260W for 0.5h to uniformly disperse the opal shale to obtain electrostatic spinning solution;

Fig. 1 is a scanning electron microscope image of the nano fiber mask containing opal shale obtained in example 2, and it can be seen that opal shale nano particles are uniformly distributed on and in the fiber surface, the fiber surface is relatively smooth, no beading phenomenon exists, and the diameter distribution is also uniform.

Comparative example 1

The same procedure as in example 2 was repeated, except that the opal shale was not contained.

Comparative example 2

The procedure is as in example 2 except that polyethylene glycol is not included.

Comparative example 3

The procedure of example 2 was repeated except that sericin was not contained.

Clinical trial

1 object and method

1.1 study subjects: inclusion criteria were: firstly, a female subject with the phenomena of oil generation, pigmentation, dark complexion and the like on the facial skin of 18-35 years old is tested; second, voluntarily participate in the study and sign informed consent. Exclusion criteria: firstly, patients with allergic history of any component in the product; ② pregnant or lactating women; (iii) those who have recently used (orally or externally) steroid drugs or antihistamine drugs; patients with systemic diseases or skin diseases; the product can not be used according to requirements; sixthly, the patients can not follow up on time.

1.2 methods of investigation

1.2.1 sources and types of skin care products: the bamboo carbon black mask with a cleaning function is sold in the market; the nanofiber mask containing the opal shale is prepared in embodiments 1-3 of the invention; and (3) preparing the nanofiber mask according to comparative examples 1-3.

1.2.2 subject grouping method: all the subjects are randomly divided into 7 groups according to a random number table, namely a control group, test groups 1-3 and comparison groups 1-3. The number of control groups was 30, the number of test groups was 29, the number of test groups was 2, the number of test groups was 3, the number of control groups was 1 was 32, the number of control groups was 2, the number of control groups was 28, the forehead rich in sebaceous glands was selected as the site to be tested, three groups of subjects were each coated with a corresponding facial mask before sleeping and after cleaning the forehead every day, the control groups used commercially available bamboo black facial masks having a cleaning function, the test groups used the opal shale-containing nanofiber facial masks prepared in examples 1 to 3 of the present invention, and the control groups used the nanofiber facial masks prepared in comparative examples 1 to 3. The entire study lasted 12 weeks during which no other cleansing and whitening products were used on the forehead.

1.2.3 cleanliness testing and photo taking: the moisture content, oil content, fineness, smoothness and harmful bacteria content of the forehead skin of the subject were measured before the test (W0), after 2 weeks (W2), after 4 weeks (W4), after 8 weeks (W8) and after 12 weeks (W12), and the results were compared with each group of the test results before the test (W0), and the results were compared with each other, and the results were increased by "+", decreased by "-", and no significant change was observed by 0 ", and the positive forehead image of the subject was taken with a digital camera (Coolpix 5700, Nikon, japan) before each test.

1.2.4 skin whitening assessment

The degree of improvement of the forehead skin color of the subject was evaluated by a dermatologist who did not participate in the test on the basis of the photographs in W2, W4, W8 and W12, and was classified into four grades of marked improvement, moderate improvement, mild improvement and no improvement.

3 results

3.2 skin cleanliness test results are shown in Table 1.

TABLE 1 statistics of frontal skin test results for three groups of subjects

3.3 skin lightening assessment results are shown in Table 2.

TABLE 2 statistics of forehead skin tone improvement effect of three groups of subjects

The test finds that statistics of skin test results and color improvement effects of a test group and a control group are statistically different (P is less than 0.05), and the skin of a tester using the test groups 1-3 of the application is improved to different degrees, which shows that the nanofiber facial mask containing opal shale can thoroughly clean the skin, reduce grease secretion, have the effects of moisturizing, whitening and resisting bacteria, and the skin fineness and smoothness are improved along with the prolonging of the using time.

As can be seen from the data in the skin test results table 1 and the skin color improvement effect table 2 of the test groups 1 to 3 and the comparison groups 1 to 3, each test result and the skin color improvement effect of the test groups 1 to 3 are superior to those of the comparison group, the comparison group 1 does not contain opal shale, the cleaning effect of the mask is greatly reduced, the antibacterial property is weakened, and the skin absorbs less nutrition from sericin and has a poor color improvement effect due to incomplete cleaning; the comparative group 2 does not contain polyethylene glycol, so that the compatibility of the mask is reduced, pores are not easy to open when the mask is used, and the effects of cleaning, moisturizing and color improvement are poor; the comparative group 3 did not contain sericin, and the cleaning efficacy was not significantly reduced, but the antibacterial effect was poor, and the moisturizing and whitening effects could not be achieved.

The above description is only for the specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and other modifications or equivalent substitutions made by the technical solution of the present invention by the ordinary skilled in the art should be covered within the scope of the claims of the present invention without departing from the spirit and scope of the technical solution of the present invention.

Claims

1. The nanofiber mask containing opal shale is characterized by being prepared from the following raw materials in percentage by mass: 2-14% of polyvinyl alcohol, 1-10% of polyethylene glycol, 1-40% of sericin, 0.01-1% of opal shale and the balance of deionized water;

the polyvinyl alcohol is PVA1797 type, and the alcoholysis degree is 96.0-98.0%; the molecular weight of the polyethylene glycol is 2000-10000;

the preparation method of the nano-fiber mask containing the opal shale comprises the following steps:

step one, preparing a polyvinyl alcohol, polyethylene glycol and sericin blending solution: respectively dissolving polyvinyl alcohol and polyethylene glycol in deionized water, magnetically stirring at 80 +/-5 ℃ for more than 8 hours to prepare solutions, mixing the two solutions in proportion, cooling, adding sericin, dissolving in a water bath at 50-60 ℃ for 4 hours, and cooling to obtain a polyvinyl alcohol, polyethylene glycol and sericin blending solution;

2. The preparation method of the nano-fiber mask containing the opal shale according to claim 1, which is characterized by comprising the following steps:

3. The method for preparing the nano fiber mask containing the opal shale according to claim 2, wherein the electrostatic spinning process conditions are electrostatic voltage of 5-40kV, distance of 5-25cm and speed of 0.15mL/h-1.5 mL/h.