CN110735326B - Silver mask cloth and preparation method thereof - Google Patents
Silver mask cloth and preparation method thereof Download PDFInfo
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- CN110735326B CN110735326B CN201911066180.2A CN201911066180A CN110735326B CN 110735326 B CN110735326 B CN 110735326B CN 201911066180 A CN201911066180 A CN 201911066180A CN 110735326 B CN110735326 B CN 110735326B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
- D06M16/003—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic with enzymes or microorganisms
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0212—Face masks
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/144—Alcohols; Metal alcoholates
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/38—Polyurethanes
Abstract
The invention discloses a silver mask cloth and a preparation method thereof, belonging to the technical field of cosmetics, wherein the preparation method comprises the following steps of (1) preprocessing blended cloth: treating the blended fabric nylon/spandex mask fabric with a lipase solution; (2) pretreating chitosan: modifying chitosan with glacial acetic acid; (3) preparing a nano silver dispersion liquid: mixing AgNO3Dispersing the solution in the modified chitosan solution to obtain nano-silver dispersion liquid; (4) preparing silver-plated chinlon/spandex face mask cloth: dipping the pretreated blended fabric obtained in the step (1) in a nano-silver dispersion liquid to obtain a mask fabric with an active center, spraying a reducing sugar solution on the mask fabric, and dipping the mask fabric in a silver-ammonia aqueous solution; (5) post-treatment process of silver-plated chinlon/spandex face mask cloth. The silver mask cloth can be repeatedly used for many times, can be used every day, and has strong electron conduction effect and good deep moisturizing effect.
Description
Technical Field
The invention relates to the technical field of cosmetics, in particular to silver mask cloth and a preparation method thereof.
Background
The facial mask is a category of skin care products and is a carrier of the skin care products. The facial mask is covered on the face, and water and other active ingredients of small molecules in the facial mask permeate into the horny layer of the epidermis, so that the effects of moisturizing, whitening, resisting aging, balancing grease and the like are realized. The facial mask mainly has four types, namely a paste type, a tearing type, a jelly type and a wet tissue type. Wherein the paste contains more kaolin, and has higher content of antiseptic and mineral; the main components of the tearing type facial mask are macromolecular glue, water and alcohol, the facial mask is fully contacted and adhered with the skin, blackheads, aged cutin and the like on the skin are peeled off by tearing, and the problems of skin looseness, large pores and the like are easily caused; the jelly type facial mask is mainly prepared from high molecular gelatin, polyalcohol, and some alkaline agent and surfactant, and can damage natural barrier of skin; the wet tissue type facial mask mainly comprises silk, all cotton, terylene, blended yarns, tencel, biological fibers and the like, and some materials are added with bleaching agents and other components in the processing process, so that the long-term use of the wet tissue type facial mask can threaten the health.
However, it is well known that the optimal frequency of use of the mask is two to three times a week. Because the skin care mode of the traditional mask is that the face is directly contacted with the moisture through the essence in the mask cloth, the skin is moisturized and nourished from the surface layer in the environment isolated from the air. However, the skin of the face has a skin barrier system, and the skin can be excessively softened by using the facial mask frequently, so that the skin is damaged; meanwhile, the skin of the face is likely to be sucked back, so that the skin is drier and more skin problems are caused. Therefore, the current facial masks are not suitable for use at high frequency for a long time.
The silver ion has the bactericidal effect, can effectively improve the moistening and permeating effects of skin care products, is beneficial to the absorption of skin to nutrient substances, and Chinese patent (application number CN206548844U) discloses a silver fiber superconducting mask.
Disclosure of Invention
The invention aims to provide silver mask cloth and a preparation method thereof, and aims to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a preparation method of silver mask cloth, which comprises the following steps:
(1) pretreating the blended fabric: treating the blended fabric nylon/spandex mask fabric with a lipase solution;
(2) pretreating chitosan: modifying chitosan with glacial acetic acid;
(3) preparing a nano silver dispersion liquid: mixing AgNO3Dispersing the solution in the modified chitosan solution to obtain nano-silver dispersion liquid;
(4) preparing silver-plated chinlon/spandex face mask cloth: dipping the pretreated blended fabric obtained in the step (1) in a nano-silver dispersion liquid to obtain a mask fabric with an active center, spraying a reducing sugar solution on the mask fabric, and dipping the mask fabric in a silver-ammonia aqueous solution;
(5) post-treatment of silver-plated nylon/spandex face film cloth: and mixing fatty acid, ethanol and water to obtain a mixed solution, spraying the mixed solution on the surface of the prepared silver-plated nylon/spandex facial mask cloth, and drying.
Further, the steps specifically include:
(1) pretreating the blended fabric: preparing a lipase solution, putting the blended fabric chinlon/spandex facial mask cloth into the prepared lipase solution, reacting for 10-20 min at 30-50 ℃, heating to 80 ℃ after the reaction is finished, taking out the chinlon/spandex facial mask cloth, and cleaning to obtain the pretreated chinlon/spandex facial mask cloth; in the pretreatment process of the blended fabric, the amide group is changed, the final size is obtained and the size stability is ensured due to the shrinkage of the chinlon and the elastic fiber in the subsequent treatment process;
(2) pretreating chitosan: dissolving chitosan in a buffer solution with the pH value of 4, adding glacial acetic acid to avoid the precipitation of reducing sugar in the chitosan when the pH value is higher than 6, preparing a 0.5-1.0 wt% chitosan solution, adding the buffer solution into the 0.5-1.0 wt% chitosan solution, stirring for 15min, and filtering by using a crucible type filter with the pore diameter of 40-100 mu m to obtain a chitosan solution for later use;
(3) preparing a nano silver dispersion liquid: adding 10-30 mmol/L AgNO3Mixing the solution with the chitosan solution obtained in the step (2) to obtain a mixed solution, stirring the mixed solution for 10-15 min at 20-30 ℃ under a closed condition to form an active precursor species, and then reacting at 70-90 ℃ for 10-15 h to obtain a nano-silver dispersion liquid, wherein the nano-silver dispersion liquid is still stable at the rotating speed of 1500rpm, and the nano-silver dispersion liquid is proved to have good stability, and in the process, hydroxyl, amino and Ag of CS (chitosan) are mixed with the Ag+Coordination bonding occurs, and then at high temperature, Ag+Converting into Ag active center to form stable nanometer silver dispersion liquid;
(4) preparing silver-plated chinlon/spandex face mask cloth: soaking the pretreated chinlon/spandex mask cloth obtained in the step (1) in the nano-silver dispersion liquid obtained in the step (3) at the temperature of 60-80 ℃ for 10-15 min, taking out, and cleaning with distilled water to obtain the mask cloth with an active center, wherein in the process, amino on the surface of the mask cloth can react with nano-Ag in the nano-silver dispersion liquid and can react with unreacted Ag+Coordinate bonding, and chitosan is also bonded with-NH in the blended fabric2The active groups act, which is a key factor for improving the active center of the silver and enhancing the firm combination of the active center and the blended fabric, and a reducing sugar solution with the concentration of 1.0-2.0 g/L is sprayed by a spraying methodThe method comprises the following steps of (1) immersing a mask cloth with an active center in a 60-80 mmol/L silver ammonia water solution, and reacting for 20-30 min at the temperature of 25-35 ℃ to obtain silver-plated chinlon/spandex mask cloth;
(5) post-treatment of silver-plated nylon/spandex face film cloth: mixing fatty acid, ethanol and water to obtain a mixed solution, wherein the mixed solution comprises 3-5 wt% of fatty acid, 80-85% of ethanol and 10-17% of water, and spraying the mixed solution on the surface of the prepared silver-plated nylon/spandex facial mask cloth and drying.
Further, in the step (1), the mass ratio of the chinlon to the spandex in the chinlon/spandex mask cloth (80-90%) is (10-20%).
Further, the mass percentage of the lipase in the lipase solution in the step (1) is 0.1-0.2%.
Further, the bath ratio of the mask cloth to the lipase solution in the step (1) is 1: 10-1: 20(kg cloth: L liquid volume).
Further, the chitosan is 70-85% of chitosan with a medium deacetylation degree.
Further, the buffer solution in the step (2) is 0.1M acetic acid-sodium acetate buffer solution.
Further, the feed-liquid ratio of the chitosan to the buffer solution in the step (2) is 1g to 90 mL.
Further, the mass ratio of the amount of the glacial acetic acid added in the step (2) to the chitosan is 0.30-0.34: 1.
Further, AgNO in step (3)3The volume ratio of the solution to the chitosan solution is 0.3-0.5.
Further, in the step (4), the reducing sugar solution is a glucose solution or a sucrose solution, and 2-4 ml of the reducing sugar solution is sprayed on each piece of the facial mask cloth.
The invention also provides the silver mask cloth prepared by the preparation method.
According to the invention, the base cloth is treated by the lipase solution to remove oil stains on the surface of the base cloth, so that the normal proceeding of the subsequent reaction is ensured, and then the amide group is changed by heat treatment, so that the shrinkage of chinlon and elastic fiber in the subsequent treatment process is avoided, the size suitable for preparing the mask is obtained, and the stability of the size is ensured. Meanwhile, the reaction conditions are mild, and the amide group changes, so that certain acting force exists among the subsequent silver particles, chitosan and the amide group, and the binding fastness is improved.
The invention takes the chinlon/spandex facial mask cloth as the base cloth of the facial mask cloth, compared with other types of base cloth, the resistance to alkaline solution is poorer, therefore, the chinlon/spandex facial mask cloth is processed by nano-silver dispersion liquid, active centers are formed on the surface of the chinlon/spandex facial mask cloth, then reducing sugar solution such as glucose or cane sugar is absorbed on the surface of the chinlon/spandex facial mask cloth, and a silver layer is rapidly deposited in alkaline silver plating solution, thereby avoiding the damage of alkaline liquid to the base cloth and ensuring the strength and toughness of the base cloth.
According to the invention, a thin film of a catalytic activity center formed by a biopolymer and nano silver is firstly formed on the surface of the base cloth by using the silver nano dispersion liquid, so that the continuous formation of a subsequent silver layer is ensured, the bonding fastness of the silver layer and the mask base cloth is ensured, the performance of higher washing fastness is achieved, and the repeated utilization for many times is ensured.
The silver fiber mask cloth adopted by the invention is safe and safe according to Rohs (export Europe and America).
The silver mask prepared by the silver mask cloth provided by the invention is light, thin and conformable, is beneficial to the absorption of nutrient substances and moisture, can accelerate facial microcirculation, promotes cell metabolism and helps to absorb moisture to reach the bottom of muscles by utilizing the physical conductivity of the silver mask cloth, and the silver mask cloth is taken down after the silver mask surface is dried slightly after 15-20 minutes. The coating gel layer contains moisturizing factors and nutrients (cosmetic agents), and different nutrients can be added according to different customer requirements.
When the silver mask prepared by the silver mask cloth provided by the invention is contacted with facial skin, a bioelectricity field is generated, facial microcirculation is accelerated, hair follicle sebaceous gland ducts are dredged, moisture is dredged to reach the bottom of the skin, absorption of nutrient components can be promoted, the absorption rate of the nutrient components can be improved, the absorption rate of common mask paper is about 30%, the absorption rate of the nutrient components of the silver mask provided by the invention is up to 90%, and the silver mask cloth can assist skin care products in guiding moisture and nutrition deeply into the skin.
Because the skin care mode of the traditional mask is that the face is directly contacted with the moisture through the essence in the mask cloth, the skin is moisturized and nourished from the surface layer in the environment isolated from the air. However, the skin of the face has a skin barrier system, and the skin can be excessively softened by using the facial mask frequently, so that the skin is damaged; meanwhile, the skin of the face is likely to be sucked back, so that the skin is drier and more skin problems are caused. The injection type nutrition and moisture supplying mode of the silver mask can be deeply introduced and absorbed by the skin, so that the situation of back suction of nutrition and moisture does not exist, and the silver mask can be used every day.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a diagram of a silver mask cloth according to the present invention;
fig. 2 is a diagram of a real object of a mask prepared by using the silver mask cloth of the present invention.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but rather as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The lipase of the invention was purchased from SigmaAldrich.
Example 1
(1) Pretreating the blended fabric: preparing a lipase solution with the mass fraction of lipase in the lipase solution being 0.1% from 80% to 20% of the mass ratio of polyamide to spandex in the blended fabric polyamide/spandex facial mask cloth, putting the blended fabric polyamide/spandex facial mask cloth into the prepared lipase solution, and carrying out bath ratio: reacting at the temperature of 30 ℃ for 10min for 1kg:10L, heating to 80 ℃ after the reaction is finished, taking out the nylon/spandex facial mask cloth, and cleaning to obtain pretreated nylon/spandex facial mask cloth;
(2) pretreating chitosan: dissolving 1.00g of chitosan in 90ml of acetic acid-sodium acetate buffer solution with the pH value of 4, adding 0.32g of glacial acetic acid to avoid the precipitation of reducing sugar in the chitosan when the pH value is higher than 6 to prepare 1.0wt% of chitosan solution, adding the buffer solution into the 1.0wt% of chitosan solution, stirring for 15min, and filtering by using a crucible type filter with the pore diameter of 40 mu m to obtain chitosan solution for later use;
(3) preparing a nano silver dispersion liquid: adding 10mmol/L AgNO3Mixing the solution with the chitosan solution obtained in the step (2) to obtain a mixed solution, wherein the volume ratio of the solution to the chitosan solution is 0.3: 1, stirring the mixed solution for 10min at 20 ℃ under a closed condition to form an active precursor species, and reacting for 10h at 70 ℃ to obtain a nano-silver dispersion solution, wherein the nano-silver dispersion solution is still stable at the rotating speed of 1500 rpm;
(4) preparing silver-plated chinlon/spandex face mask cloth: soaking the pretreated chinlon/spandex facial mask cloth obtained in the step (1) in the nano-silver dispersion liquid obtained in the step (3) at the temperature of 60 ℃ for 10min, taking out, and cleaning with distilled water to obtain the facial mask cloth with an active center, wherein in the process, amino on the surface of the facial mask cloth can react with nano-Ag in the nano-silver dispersion liquid and can react with unreacted Ag+Coordinate bonding, and chitosan is also bonded with-NH in the blended fabric2The active groups act, which is a key factor for improving the active center of silver and enhancing the firm combination of the active center and the blended fabric, 2mL of glucose solution with the concentration of 1.0/L is sprayed on the mask fabric with the active center by using a spraying method, and then the mask fabric is immersed in 15mL of 60mmol/L silver-ammonia aqueous solution and reacts for 20min at the temperature of 25 ℃ to obtain silver-plated nylon/spandex mask fabric;
(5) post-treatment of silver-plated nylon/spandex face film cloth: mixing fatty acid, ethanol and water to obtain a mixed solution, wherein the mixed solution comprises 3 wt% of fatty acid, 80 wt% of ethanol and 17 wt% of water by mass, and spraying the mixed solution on the surface of the prepared silver-plated nylon/spandex facial mask cloth and drying the surface of the prepared silver-plated nylon/spandex facial mask cloth.
Example 2
(1) Pretreating the blended fabric: preparing a lipase solution with the mass fraction of lipase in the lipase solution being 0.1% from 90% to 10% of the mass ratio of polyamide to spandex in the blended fabric polyamide/spandex facial mask cloth, putting the blended fabric polyamide/spandex facial mask cloth into the prepared lipase solution, and carrying out bath ratio: reacting at the temperature of 40 ℃ for 10min for 1kg and 20L, heating to 80 ℃ after the reaction is finished, taking out the nylon/spandex facial mask cloth, and cleaning to obtain pretreated nylon/spandex facial mask cloth;
(2) pretreating chitosan: dissolving 1.00g of chitosan in 90ml of acetic acid-sodium acetate buffer solution with the pH value of 4, adding 0.32g of glacial acetic acid to avoid the precipitation of reducing sugar in the chitosan when the pH value is higher than 6 to prepare 1.0wt% of chitosan solution, adding the buffer solution into the 1.0wt% of chitosan solution, stirring for 15min, and filtering by using a crucible type filter with the pore diameter of 50 mu m to obtain chitosan solution for later use;
(3) preparing a nano silver dispersion liquid: 20mmol/L of AgNO3Mixing the solution with the chitosan solution obtained in the step (2) to obtain a mixed solution, wherein the volume ratio of the solution to the chitosan solution is 0.4: 1, stirring the mixed solution for 10min at 25 ℃ under a closed condition to form an active precursor species, and reacting for 10h at 80 ℃ to obtain a nano-silver dispersion solution, wherein the nano-silver dispersion solution is still stable at the rotating speed of 1500 rpm;
(4) preparing silver-plated chinlon/spandex mask cloth: soaking the pretreated chinlon/spandex facial mask cloth obtained in the step (1) in the nano-silver dispersion liquid obtained in the step (3) at the temperature of 70 ℃ for 10min, taking out, and cleaning with distilled water to obtain the facial mask cloth with an active center, wherein in the process, amino on the surface of the facial mask cloth can react with nano-Ag in the nano-silver dispersion liquid and can react with unreacted Ag+Coordinate bonding, and chitosan is also bonded with-NH in the blended fabric2The active groups act, which is a key factor for improving the active center of silver and enhancing the firm combination of the active center and the blended fabric, 3mL of glucose solution with the concentration of 2.0/L is sprayed on the mask fabric with the active center by using a spraying method, and then the mask fabric is immersed in 20mL of 70mmol/L silver-ammonia aqueous solution and reacts for 20min at the temperature of 30 ℃ to obtain silver-plated nylon/spandex mask fabric;
(5) post-treatment of silver-plated nylon/spandex face film cloth: mixing fatty acid, ethanol and water to obtain a mixed solution, wherein the mixed solution comprises 4 wt% of fatty acid, 82 wt% of ethanol and 14 wt% of water by mass, and spraying the mixed solution on the surface of the prepared silver-plated nylon/spandex facial mask cloth and drying the surface of the prepared silver-plated nylon/spandex facial mask cloth.
Example 3
(1) Pre-treating blended cloth: preparing a lipase solution with the mass fraction of lipase in the lipase solution being 0.2% from 90% to 10% of the mass ratio of polyamide to spandex in the blended fabric polyamide/spandex facial mask cloth, putting the blended fabric polyamide/spandex facial mask cloth into the prepared lipase solution, and carrying out bath ratio: reacting at 50 ℃ for 20min for 1kg:15L, heating to 80 ℃ after the reaction is finished, taking out the nylon/spandex facial mask cloth, and cleaning to obtain pretreated nylon/spandex facial mask cloth;
(2) pretreating chitosan: dissolving 1.00g of chitosan in 90ml of acetic acid-sodium acetate buffer solution with the pH value of 4, adding 0.32g of glacial acetic acid to avoid the precipitation of reducing sugar in the chitosan when the pH value is higher than 6 to prepare 1.0wt% of chitosan solution, adding the buffer solution into the 1.0wt% of chitosan solution, stirring for 15min, and filtering by using a crucible type filter with the pore diameter of 80 mu m to obtain chitosan solution for later use;
(3) preparing a nano silver dispersion liquid: mixing 30mmol/L AgNO3Mixing the solution with the chitosan solution obtained in the step (2) to obtain a mixed solution, wherein the volume ratio of the solution to the chitosan solution is 0.5: 1, stirring the mixed solution for 15min at 30 ℃ under a closed condition to form an active precursor species, and reacting for 15h at 80 ℃ to obtain a nano-silver dispersion solution, wherein the nano-silver dispersion solution is still stable at the rotating speed of 1500 rpm;
(4) preparing silver-plated chinlon/spandex mask cloth: soaking the pretreated chinlon/spandex mask cloth obtained in the step (1) in the nano-silver dispersion liquid obtained in the step (3), taking out after soaking for 10min at the temperature of 80 ℃, and cleaning with distilled water to obtain the mask cloth with an active center, wherein in the process, amino on the surface of the mask cloth can react with nano-Ag in the nano-silver dispersion liquid and react with unreacted Ag+Coordinate bonding, and chitosan is also bonded with-NH in the blended fabric2The method comprises the following steps of (1) waiting for the action of active groups, which is a key factor for improving the firm combination of a silver active center and blended cloth, spraying 4mL of sucrose solution with the concentration of 2.0/L onto the mask cloth with the active center by using a spraying method, then immersing the mask cloth into 20mL of 80mmol/L silver-ammonia aqueous solution, and reacting for 30min at the temperature of 35 ℃ to obtain silver-plated nylon/spandex mask cloth;
(5) post-treatment of silver-plated nylon/spandex face film cloth: mixing fatty acid, ethanol and water to obtain a mixed solution, wherein the fatty acid accounts for 5wt%, the ethanol accounts for 85 wt% and the water accounts for 10 wt% of the mixed solution, and spraying the mixed solution on the surface of the prepared silver-plated nylon/spandex facial mask cloth and drying the silver-plated nylon/spandex facial mask cloth.
Example 4
(1) Pretreating the blended fabric: preparing a lipase solution with the mass fraction of lipase in the lipase solution being 0.2% from 85% to 15% of the mass ratio of polyamide to spandex in the blended fabric polyamide/spandex facial mask cloth, putting the blended fabric polyamide/spandex facial mask cloth into the prepared lipase solution, and carrying out bath ratio: reacting at the temperature of 50 ℃ for 15min for 1 kg/20L, heating to 80 ℃ after the reaction is finished, taking out the nylon/spandex facial mask cloth, and cleaning to obtain pretreated nylon/spandex facial mask cloth;
(2) pretreating chitosan: dissolving 1.00g of chitosan in 90ml of acetic acid-sodium acetate buffer solution with the pH value of 4, adding 0.32g of glacial acetic acid to avoid the precipitation of reducing sugar in the chitosan when the pH value is higher than 6, preparing 1.0wt% of chitosan solution, adding the buffer solution into the 1.0wt% of chitosan solution, stirring for 15min, and filtering by using a crucible type filter with the pore diameter of 100 mu m to obtain the chitosan solution for later use;
(3) preparing a nano silver dispersion liquid: adding 25mmol/L AgNO3Mixing the solution with the chitosan solution obtained in the step (2) to obtain a mixed solution, wherein the volume ratio of the solution to the chitosan solution is 0.3: 1, stirring the mixed solution for 15min at 30 ℃ under a closed condition to form an active precursor species, and reacting for 15h at 75 ℃ to obtain a nano-silver dispersion solution, wherein the nano-silver dispersion solution is still stable at the rotating speed of 1500 rpm;
(4) preparing silver-plated chinlon/spandex mask cloth: soaking the pretreated chinlon/spandex facial mask cloth obtained in the step (1) in the nano-silver dispersion liquid obtained in the step (3) at the temperature of 70 ℃ for 15min, taking out, and cleaning with distilled water to obtain the facial mask cloth with an active center, wherein in the process, amino on the surface of the facial mask cloth can react with nano-Ag in the nano-silver dispersion liquid and can react with unreacted Ag+Coordinate bonding, and chitosan is also bonded with-NH in the blended fabric2The active groups act to promote the active center of silver and strengthen the silver and blended fabricThe key factor of firm combination is that 3mL of sucrose solution with the concentration of 1.0/L is sprayed on the mask cloth with the active center by a spraying method, and then the mask cloth is immersed in 20mL of 60mmol/L silver ammonia water solution and reacts for 25min at the temperature of 35 ℃ to obtain silver-plated nylon/spandex mask cloth;
(5) post-treatment of silver-plated nylon/spandex face film cloth: mixing fatty acid, ethanol and water to obtain a mixed solution, wherein the mixed solution comprises 5wt% of fatty acid, 80 wt% of ethanol and 15 wt% of water by mass, spraying the mixed solution on the surface of the prepared silver-plated nylon/spandex facial mask cloth, and drying.
Example 5
(1) Pretreating the blended fabric: preparing a lipase solution with the mass fraction of lipase in the lipase solution being 0.2% from 80% to 20% of the mass ratio of polyamide to spandex in the blended fabric polyamide/spandex facial mask cloth, putting the blended fabric polyamide/spandex facial mask cloth into the prepared lipase solution, and carrying out bath ratio: reacting at 45 ℃ for 15min for 1 kg/20L, heating to 80 ℃ after the reaction is finished, taking out the nylon/spandex facial mask cloth, and cleaning to obtain pretreated nylon/spandex facial mask cloth;
(2) pretreating chitosan: dissolving 1.00g of chitosan in 90ml of acetic acid-sodium acetate buffer solution with the pH value of 4, adding 0.32g of glacial acetic acid to avoid the precipitation of reducing sugar in the chitosan when the pH value is higher than 6 to prepare 1.0wt% of chitosan solution, adding the buffer solution into the 1.0wt% of chitosan solution, stirring for 15min, and filtering by using a crucible type filter with the pore diameter of 90 mu m to obtain chitosan solution for later use;
(3) preparing a nano silver dispersion liquid: adding 25mmol/L AgNO3Mixing the solution with the chitosan solution obtained in the step (2) to obtain a mixed solution, wherein the volume ratio of the solution to the chitosan solution is 0.5: 1, stirring the mixed solution for 15min at 25 ℃ under a closed condition to form an active precursor species, and reacting for 15h at 70 ℃ to obtain a nano-silver dispersion solution, wherein the nano-silver dispersion solution is still stable at the rotating speed of 1500 rpm;
(4) preparing silver-plated chinlon/spandex mask cloth: soaking the pretreated chinlon/spandex mask cloth obtained in the step (1) in the nano-silver dispersion liquid obtained in the step (3) at the temperature of 70 ℃ for 10min, and taking outWashing with distilled water to obtain mask cloth with active center, wherein the amino group on the surface of the mask cloth can react with the nano Ag in the nano silver dispersion liquid and unreacted Ag+Coordinate bonding, and chitosan is also bonded with-NH in the blended fabric2The method comprises the following steps of (1) spraying 2mL of sucrose solution with the concentration of 1.0/L onto the mask cloth with the active center by using a spraying method, then soaking the mask cloth into 15mL of 60mmol/L silver-ammonia aqueous solution, and reacting for 20min at the temperature of 30 ℃ to obtain silver-plated nylon/spandex mask cloth;
(5) post-treatment of silver-plated nylon/spandex face film cloth: mixing fatty acid, ethanol and water to obtain a mixed solution, wherein the mixed solution comprises 5wt% of fatty acid, 85 wt% of ethanol and 10 wt% of water by mass, spraying the mixed solution on the surface of the prepared silver-plated nylon/spandex facial mask cloth, and drying.
Comparative example 1
The preparation method is the same as that of example 1, except that the blended fabric is not pretreated and is subjected to conventional treatment.
Comparative example 2
The preparation method is the same as that of example 1, except that the chitosan pretreatment process is not performed, and the nano silver dispersion liquid is a conventional nano silver dispersion liquid.
Comparative example 3
The difference is that the nylon/spandex facial mask cloth which is not pretreated is activated by the nano silver dispersion liquid and is directly plated with silver as in the example 1.
The silver facial mask cloth of the examples 1-5 and the comparative examples 1-3 is detected according to IEC 62321-4: 2013; IEC 62321-5: 2013; IEC 62321-6: 2015; IEC 62321-7: 2017; IEC 62321-8:2017, environment was detected according to European Union RoHS directive 2011/65/EU (RoHS 2.0) and its revision directive (EU) 2015/863: temperature (22-28) DEG C; humidity (45-75)% RH, and detection results are shown in Table 1.
TABLE 1
Note: 1)1 mg/kg-1 ppm-0.0001%;
2) MDL ═ lower limit of detection;
3) ND ═ undetected (< MDL).
As is clear from the results in table 1, the silver mask cloth of the present invention can be used with confidence by RoHS (export europe and america) test.
The antibacterial performance of the silver mask cloth of the examples 1-5 and the comparative examples 1-3 is detected according to GB/T21510-: colony number of 0h blank control sample of Candida albicans is 4.50 multiplied by 104cfu/mL, 24h blank control colony count 4.40X 104cfu/mL; trichophyton mentagrophytes 0h blank control colony number 3.60 × 104cfu/mL, 24h blank control colony count 3.50X 104cfu/mL; staphylococcus aureus 0h blank control colony count 4.30X 104cfu/mL, 24h blank control colony count 4.20X 104cfu/mL; coli 0h blank 4.60X 10 colony count4cfu/mL, 24h blank control colony count 4.40X 104cfu/mL; average number of recovered colonies of Candida albicans 0h control sample is 1.78 multiplied by 104cfu/mL, average number of colonies recovered from post-operative control sample 4.60X 105cfu/mL, the results are shown in Table 2.
TABLE 2
The mask cloths of examples 1 to 5 and comparative examples 1 to 3 were washed with water 200 times, and it was found that the mask cloths of examples 1 to 5 had an antibacterial rate of > 99.9% even after washing with water 200 times, the mask cloth of comparative example 1 had an antibacterial rate of > 89% after washing with water 200 times, the mask cloth of comparative example 2 had an antibacterial rate of > 45% after washing with water 200 times, and the mask cloth of comparative example 3 had an antibacterial rate of > 25% after washing with water 200 times.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (8)
1. The preparation method of the silver mask cloth is characterized by comprising the following steps:
(1) pretreating the blended fabric: preparing a lipase solution, putting the blended fabric chinlon/spandex facial mask cloth into the prepared lipase solution, reacting for 10-20 min at 30-50 ℃, heating to 80 ℃ after the reaction is finished, taking out the chinlon/spandex facial mask cloth, and cleaning to obtain the pretreated chinlon/spandex facial mask cloth;
(2) pretreating chitosan: dissolving chitosan in a buffer solution, adding glacial acetic acid to prepare a 0.5-1.0 wt% chitosan solution, adding the buffer solution into the 0.5-1.0 wt% chitosan solution, stirring for 15min, and filtering to obtain a chitosan solution for later use;
(3) preparing a nano silver dispersion liquid: adding 10-30 mmol/L AgNO3Mixing the solution with the chitosan solution obtained in the step (2) to obtain a mixed solution, firstly stirring the mixed solution for 10-15 min at 20-30 ℃ under a closed condition to form an active precursor species, and then reacting at 70-90 ℃ for 10-15 h to obtain a nano-silver dispersion liquid;
(4) preparing silver-plated chinlon/spandex mask cloth: dipping the pretreated nylon/spandex facial mask cloth obtained in the step (1) in the nano-silver dispersion liquid obtained in the step (3), taking out after dipping for 10-15 min at the temperature of 60-80 ℃, washing with distilled water to obtain facial mask cloth with an active center, spraying a reducing sugar solution with the concentration of 1.0-2.0 g/L on the facial mask cloth with the active center, then dipping the facial mask cloth into a silver ammonia solution with the concentration of 60-80 mmol/L, and reacting for 20-30 min at the temperature of 25-35 ℃ to obtain silver-plated nylon/spandex facial mask cloth;
(5) post-treatment of silver-plated nylon/spandex face film cloth: mixing fatty acid, ethanol and water to obtain a mixed solution, wherein the mixed solution comprises 3-5 wt% of fatty acid, 80-85% of ethanol and 10-17% of water, and spraying the mixed solution on the surface of the prepared silver-plated nylon/spandex facial mask cloth and drying;
the ratio of the chinlon to the spandex in the blended fabric chinlon/spandex mask cloth in the step (1) (80-90%) is (10-20%).
2. The preparation method of the silver mask cloth according to claim 1, wherein the mass percentage of the lipase in the lipase solution in the step (1) is 0.1-0.2%.
3. The preparation method of the silver facial mask cloth according to claim 1, wherein the bath ratio of the facial mask cloth to the lipase solution in the step (1) is 1: 10-1: 20.
4. The method for preparing the silver mask cloth according to claim 1, wherein the chitosan is 70-85% of chitosan with a medium deacetylation degree.
5. The method for preparing silver facial mask cloth according to claim 1, wherein the buffer solution in the step (2) is 0.1M acetic acid-sodium acetate buffer solution.
6. The method for preparing silver facial mask cloth according to claim 1, wherein AgNO in the step (3)3The volume ratio of the solution to the chitosan solution is 0.3-0.5.
7. The preparation method of the silver facial mask cloth according to claim 1, wherein the reducing sugar solution in the step (4) is a glucose solution, and 2-4 ml of the reducing sugar solution is sprayed on each piece of facial mask cloth.
8. A silver mask cloth prepared by the preparation method of any one of claims 1 to 7.
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