CN111974088B - Method for manufacturing filter material - Google Patents
Method for manufacturing filter material Download PDFInfo
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- CN111974088B CN111974088B CN202010808815.8A CN202010808815A CN111974088B CN 111974088 B CN111974088 B CN 111974088B CN 202010808815 A CN202010808815 A CN 202010808815A CN 111974088 B CN111974088 B CN 111974088B
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- woven fabric
- fabric layer
- filter material
- chitosan
- ferulic acid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/08—Filter cloth, i.e. woven, knitted or interlaced material
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
- A41D13/05—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches protecting only a particular body part
- A41D13/11—Protective face masks, e.g. for surgical use, or for use in foul atmospheres
- A41D13/1192—Protective face masks, e.g. for surgical use, or for use in foul atmospheres with antimicrobial agent
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/02—Layered materials
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/12—Hygroscopic; Water retaining
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/14—Air permeable, i.e. capable of being penetrated by gases
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/30—Antimicrobial, e.g. antibacterial
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/0001—Making filtering elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/0027—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions
- B01D46/0028—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions provided with antibacterial or antifungal means
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; 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
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
- D06M10/025—Corona discharge or low temperature plasma
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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
- D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
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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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/356—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms
- D06M15/3562—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms containing nitrogen
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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
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D2500/00—Materials for garments
- A41D2500/30—Non-woven
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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
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
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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
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
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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
- D06M2101/32—Polyesters
Abstract
The invention relates to a method for manufacturing a filter material, which comprises the following steps of firstly, mixing ferulic acid-chitosan graft copolymer, polycaprolactone and polypropylene in a mass ratio of 1-5: 1-10: 70-90, performing melt blending, and performing spray melting technology to obtain a non-woven fabric layer; secondly, carrying out surface modification treatment on the obtained non-woven fabric layer by adopting polyvinylpyrrolidone and ammonium persulfate solution, and loading silver-loaded nano titanium dioxide powder on the surface of the non-woven fabric layer; then preparing a polytetrafluoroethylene microporous membrane with the thickness not more than 1mmHot-pressing and compounding the polytetrafluoroethylene microporous membrane and the non-woven fabric layer obtained in the step 2 to obtain a composite filter layer; the obtained composite filter layer was subjected to corona treatment and had a stored charge density of 3X 10‑4～5.7×10‑3C/m2(ii) a And finally, respectively compounding the waterproof non-woven fabric layer and the spunlace non-woven fabric layer on two sides of the obtained composite filter layer. The filter material filter effect of this application is good, and the gas permeability is good and the fibre has fine chemical stability, thermostability, hydrophilicity and bacterinertness.
Description
Technical Field
The invention relates to the field of mask filter materials, in particular to a manufacturing method of a filter material.
Background
The mask is a sanitary article, is generally worn on the mouth and nose for filtering air entering the mouth and nose so as to achieve the effect of blocking harmful gas, smell, spray, virus and other substances, and is made of gauze or paper and the like. The mask has a certain filtering function on air entering the lung, and has a very good protection function when the mask is worn for operation in an environment polluted by dust and the like when respiratory infectious diseases are prevalent. The mask is generally divided into three layers, a water absorption layer, a filter layer and a waterproof layer, and the filter layer plays a main role. At present, the filter layer for the mask is mainly polyethylene melt-blown non-woven fabric or polytetrafluoroethylene microporous membrane, and the polyethylene melt-blown non-woven fabric has good filterability, barrier property, heat preservation and adsorptivity because its fibre piles up and forms netted through structure, and polytetrafluoroethylene microporous membrane has very good filtration efficiency because the reticular structure that its nanofiber crisscross arrangement formed.
In the market, the pores formed by stacking polyethylene melt-blown non-woven fabric fibers are large, fine particles cannot be effectively collected, and the filtering efficiency of particles with the particle size of 0.3 mu m is below 50%; whereas polytetrafluoroethylene microporous membranes rely purely on physical filtration, which means small pores and low gas permeability. Moreover, the antibacterial property of the filter layer is also very important for the mask, and the antibacterial property of the filter layer of the mask in general market is obtained by loading antibacterial metal ions such as silver, copper, tin, zinc, etc. on the surface of the filter layer, and the antibacterial effect obtained in this way is not stable. Therefore, there is a need to develop a filtering material suitable for a mask to solve the above problem.
Disclosure of Invention
In order to solve the problems, the invention provides a method for manufacturing a filter material.
The technical scheme adopted by the invention is that the manufacturing method of the filter material specifically comprises the following steps:
step 1: the ferulic acid-chitosan graft copolymer, polycaprolactone and polypropylene are mixed according to the mass ratio of 1-5: 1-10: 70-90, performing melt blending, and performing spray melting technology to obtain a non-woven fabric layer;
step 2: carrying out surface modification treatment on the non-woven fabric layer obtained in the step (1) by adopting polyvinylpyrrolidone and ammonium persulfate solution, and loading silver-loaded nano titanium dioxide powder on the surface of the non-woven fabric layer;
and step 3: preparing a polytetrafluoroethylene microporous membrane with the thickness not more than 1mm, and performing hot-pressing compounding on the polytetrafluoroethylene microporous membrane and the non-woven fabric layer obtained in the step 2 to obtain a composite filter layer;
and 4, step 4: performing corona treatment on the composite filter layer obtained in the step 3, wherein the storage charge density is 3 multiplied by 10-4~5.7×10-3C/m2；
And 5: and (4) respectively compounding a waterproof non-woven fabric layer and a spunlace non-woven fabric layer on two sides of the composite filter layer obtained in the step (4).
Preferably, in the step 1, the preparation step of the ferulic acid-chitosan graft copolymer comprises:
step A: dissolving chitosan powder in a citric acid-sodium citrate buffer solution with the pH value of 6.0-4.8, adding 60-100 mL of 30% hydrogen peroxide solution, and reacting at 50-70 ℃ for 60-90 min to obtain a chitosan solution with the chitosan concentration of 100 mmol; cooling the chitosan solution to room temperature, sequentially adding the methanol solution dissolved with the ferulic acid and the laccase, and uniformly stirring to obtain a mixed solution;
and B: and introducing oxygen into the mixed solution, wherein the oxygen introduction amount is 30-50L/min, after the mixed solution reacts for 1.5-3 h, dialyzing for 72h by using a dialysis membrane with the molecular weight of 14000, removing unreacted ferulic acid, thoroughly rinsing the product obtained by dialysis by using methanol, ethanol and water, and drying in vacuum to obtain the chitosan-ferulic acid graft copolymer.
Preferably, in the step 1, menthol essential oil is added, and the adding amount of the menthol essential oil is 0.5-2 parts by mass.
Preferably, in the step 2, the silver-loaded nano-dioxideAdding titanium oxide powder into 100-1000 parts by weight of deionized water to prepare silver-loaded nano TiO with the concentration of 0.2-1 mg/mL2And adding 30-80 parts of polyvinylpyrrolidone and 0.05-5 parts of ammonium persulfate into the dispersion liquid, fully mixing by adopting a mechanical stirring or ultrasonic dispersion method, and spraying to the non-woven fabric layer.
Preferably, the fiber diameter of the polytetrafluoroethylene microporous membrane is 60-80 nm, the air permeability is 0.3-0.5 m/s, and the thickness is 0.05-0.3 mm.
Preferably, in the step 4, corona discharge is performed on the surface of the composite filter layer for 1.5-3 s by using high-frequency high voltage for corona treatment, and the voltage of the corona treatment is 11000-13000V/m2The discharge frequency is 15 KHz-25 Kz.
Preferably, in the step 2, the particle size of the silver-loaded nano titanium dioxide powder is 10-15 nm.
Preferably, the concentration of the ferulic acid in the mixed solution prepared in the step A is 5-10 mmol, and the density of the laccase is 2.5-3.0U/mL.
Preferably, in the step 1, the fiber diameter of the non-woven fabric layer is 100 to 200nm, the air permeability is 0.5 to 0.8m/s, and the thickness is 0.5 to 2 mm.
The invention has the beneficial effects that:
1. the filter material contains ferulic acid-chitosan graft copolymer which has stronger antibacterial property and oxidation resistance, when microbes such as bacteria or viruses are attached to the filter material, more effective amino groups with positive charges are in chitosan in the ferulic acid-chitosan graft copolymer, and the chitosan is easy to adsorb electronegative bacteria, so that the microbes are denatured or a layer of polymer film is formed on the surface of cells from the outside, the selective permeability of the cells is changed, and nutrient substances are blocked from entering to cause the death of the bacteria, and the chitosan enters the inside of the bacteria, is combined with components required by the survival of the bacteria to destroy the metabolic balance of the bacteria, thereby inhibiting the growth and the propagation of the microbes, and disturbing the replication and the transcription of DNA in the cells; in addition, the ferulic acid has strong antibacterial activity and antioxidant activity, and can well inhibit the growth and reproduction of pathogenic bacteria such as escherichia coli, pneumonia bacillus, enterobacter and the like; moreover, the ferulic acid-chitosan graft copolymer can enable the filter material to have an antibacterial function and good antibacterial stability;
2. the ferulic acid-chitosan graft copolymer, the polycaprolactone and the polypropylene are melt blended, the polycaprolactone has good biocompatibility, good organic polymer compatibility and good biodegradability, and the polycaprolactone and the polypropylene can be compatible with each other, so that the degradability of the filter material is better and the environment is protected; moreover, the polycaprolactone is used as a supporting material for loading the ferulic acid-chitosan graft copolymer, so that the ferulic acid-chitosan graft copolymer has better compatibility with polypropylene, and the fiber of the non-woven fabric layer has good chemical stability, thermal stability, hydrophilicity, antibacterial property and the like;
3. the surface of the non-woven fabric layer is modified by polyvinylpyrrolidone and ammonium persulfate, the polyvinylpyrrolidone and trace ammonium persulfate can enhance the adhesion of polypropylene, so that the adhesive strength of silver-loaded nano titanium dioxide powder of the non-woven fabric layer on the non-woven fabric layer is obviously improved, and the polyvinylpyrrolidone is physically adsorbed on the surface of the non-woven fabric layer, so that the non-woven fabric layer has good hydrophilicity and is beneficial to absorbing sweat, saliva and the like; in addition, the silver-loaded nano titanium dioxide powder is dispersed around the microporous structure of the non-woven fabric layer in a pure physical mode, so that the hole structure of the non-woven fabric layer is maintained, the air permeability of the non-woven fabric layer is improved, and the silver-loaded nano titanium dioxide powder has strong oxidation and reduction properties, so that microorganisms such as viruses or bacteria loaded on the filter material can be decomposed from the outer membrane until the cells die, and the antibacterial property is improved;
4. according to the composite filter layer, the polytetrafluoroethylene microporous membrane and the non-woven fabric layer are subjected to hot-pressing compounding to obtain the composite filter layer, the fiber diameter and the pore size of the polytetrafluoroethylene microporous membrane are small, so that a gas exchange channel with an outer side gap larger than an inner side gap can be formed in the filter material, and the filter material is favorably ensured to have good air permeability, filterability and barrier property;
5. after the composite filter layer is prepared, the corona treatment, the polytetrafluoroethylene and the carrier are carried outThe silver nano titanium dioxide powder, the polypropylene and the like are electret materials, and the density of stored charges of the composite layer after corona treatment is 3 multiplied by 10-4~5.7×10-3C/m2The composite filtering layer can directly attract charged particles in the air and capture the charged particles by means of electrostatic force or induce neutral particles in the air to generate polarity and capture the neutral particles in the air besides the original mechanical blocking effect, so that submicron particles in the air can be more effectively filtered, and the filtering efficiency is obviously improved under the condition of not increasing air resistance; moreover, the electrostatic field and the micro-current in the composite filter layer can stimulate microorganisms such as bacteria and viruses, so that proteins, nucleic acids and the like of the microorganisms are mutated, cell walls and cell membranes of the microorganisms are damaged, the surface structures of the microorganisms are damaged, the biological balance inside and outside the cell membranes is damaged, and the microorganisms are inhibited or even killed.
6. The filter material of this application has added menthol essential oil, and the menthol essential oil has obvious antibacterial activity to microorganisms such as escherichia coli, staphylococcus aureus, candida albicans, when breathing the respiratory track of acting on the human body, because the stimulation and the effect of menthol composition can reach the effect of relieving a cough and eliminating phlegm, alleviating nasal obstruction, cool and refreshing.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The starting materials employed in the examples of the present invention are those conventionally commercially available in the art, and the equipment used is equipment conventional in the art, unless otherwise specified.
The preparation method of the ferulic acid-chitosan graft copolymer comprises the following steps:
step A: dissolving chitosan powder in citric acid-sodium citrate buffer solution with pH value of 5.5, adding 80mL of 30% hydrogen peroxide solution, and reacting at 65 ℃ for 90min to obtain chitosan solution with chitosan concentration of 100 mmol; cooling the chitosan solution to room temperature, sequentially adding 10mL of methanol solution dissolved with ferulic acid and laccase, and uniformly stirring to obtain a mixed solution, wherein the concentration of the ferulic acid in the mixed solution is 10mmol, and the density of the laccase is 3.0U/mL;
and B: introducing oxygen into the mixed solution, introducing oxygen at 35L/min, reacting the mixed solution for 2.5h, dialyzing with a dialysis membrane with molecular weight of 14000 for 72h, removing unreacted ferulic acid, thoroughly rinsing the product obtained by dialysis with methanol, ethanol and water, and vacuum drying to obtain the chitosan-ferulic acid graft copolymer.
Through the steps, the ferulic acid-chitosan graft copolymer has high preparation efficiency and high generation rate, and the prepared ferulic acid-chitosan graft copolymer contains chitosan-g-cinnamic acid with the grafting rate of about 20%, chitosan-g-caffeic acid with the grafting rate of 18% and chitosan-g-ferulic acid with the grafting rate of 20%.
The tetrafluoroethylene microporous membrane is prepared by a biaxial tension technology, and the specific steps are as follows:
1) uniformly mixing the auxiliary agent oil, the surfactant and polytetrafluoroethylene, placing the mixture in a constant-temperature oven for curing for 48 hours, and prepressing the mixture into a columnar material blank; wherein, the auxiliary oil can be gasoline or aviation kerosene, and the surfactant can be fluorine-containing acrylic resin or modified nano organic silicon;
2) putting the columnar material blank into an extruder, and preparing a base band through the processes of extrusion, rolling, additive removal and drying;
3) longitudinal stretching and transverse stretching, namely firstly carrying out gradient temperature rise on the base band to gradually longitudinally stretch, and then carrying out gradient temperature rise on the longitudinally stretched base band to gradually transversely stretch;
4) sintering and shaping to obtain the polytetrafluoroethylene microporous membrane.
Although the above description exemplifies only one specific implementation production method of the ferulic acid-chitosan graft copolymer and the tetrafluoroethylene microporous membrane, it will be understood by those skilled in the art that the production method not limited to a specific manner (particularly, the method within the scope defined by the present invention) can also achieve substantially the same production of the ferulic acid-chitosan graft copolymer, and is not particularly limited thereto.
Example 1
A manufacturing method of a filter material specifically comprises the following steps:
step 1: ferulic acid-chitosan graft copolymer, polycaprolactone and polypropylene are mixed according to the mass ratio of 5: 10: 85, melting and blending, and adopting a spray melting technology to obtain a non-woven fabric layer, wherein the fiber diameter of the non-woven fabric layer is 135-142 nm, the air permeability is 0.6m/s, and the thickness is 1 mm;
step 2: adding silver-loaded nano titanium dioxide powder with the particle size of 10-15 nm into 500 parts by weight of deionized water to prepare silver-loaded nano TiO with the concentration of 0.5mg/mL2Adding 50 parts of polyvinylpyrrolidone and 1 part of ammonium persulfate into the dispersion, fully mixing by an ultrasonic dispersion method, and uniformly spraying the dispersion on two sides of the surface of the non-woven fabric layer by an XKD-AS600 spraying machine at the spraying pressure of 0.05Mpa and the spraying amount of 0.05ml/cm 2;
and step 3: preparing a polytetrafluoroethylene microporous membrane by utilizing a biaxial stretching technology, and carrying out hot-pressing compounding on the polytetrafluoroethylene microporous membrane and the non-woven fabric layer obtained in the step (2) to obtain a composite filter layer; wherein the fiber diameter of the polytetrafluoroethylene microporous membrane is 60-80 nm, the air permeability is 0.35m/s, and the thickness is 0.2 mm;
and 4, step 4: performing corona treatment on the composite filter layer obtained in the step 3, wherein the density of stored charges of the composite filter layer is 3 multiplied by 10-3C/m2The corona treatment utilizes high-frequency high voltage to perform corona discharge on the surface of the composite filter layer for 2s, and the voltage of the corona treatment is 12000V/m2The discharge frequency is 20 Kz;
and 5: and (4) respectively compounding a waterproof non-woven fabric layer and a spunlace non-woven fabric layer on two sides of the composite filter layer obtained in the step (4).
Example 2
A manufacturing method of a filter material specifically comprises the following steps:
step 1: ferulic acid-chitosan graft copolymer, menthol essential oil, polycaprolactone and polypropylene are mixed according to the mass ratio of 5: 1: 9: 85, melting and blending, and adopting a spray melting technology to obtain a non-woven fabric layer, wherein the fiber diameter of the non-woven fabric layer is 137-151 nm, the air permeability is 0.6m/s, and the thickness is 1 mm;
step 2: the particle diameter is 1Adding 0-15 nm silver-loaded nano titanium dioxide powder into 500 parts by weight of deionized water to prepare silver-loaded nano TiO with the concentration of 0.5mg/mL2Adding 50 parts of polyvinylpyrrolidone and 1 part of ammonium persulfate into the dispersion, fully mixing by an ultrasonic dispersion method, and uniformly spraying the dispersion on two sides of the surface of the non-woven fabric layer by an XKD-AS600 spraying machine at the spraying pressure of 0.05Mpa and the spraying amount of 0.05ml/cm 2;
and step 3: preparing a polytetrafluoroethylene microporous membrane by utilizing a biaxial stretching technology, and carrying out hot-pressing compounding on the polytetrafluoroethylene microporous membrane and the non-woven fabric layer obtained in the step (2) to obtain a composite filter layer; wherein the fiber diameter of the polytetrafluoroethylene microporous membrane is 60-80 nm, the air permeability is 0.35m/s, and the thickness is 0.2 mm;
and 4, step 4: performing corona treatment on the composite filter layer obtained in the step 3, wherein the density of stored charges of the composite filter layer is 3 multiplied by 10-3C/m2The corona treatment utilizes high-frequency high voltage to perform corona discharge on the surface of the composite filter layer for 2s, and the voltage of the corona treatment is 12000V/m2The discharge frequency is 20 Kz;
and 5: and (4) respectively compounding a waterproof non-woven fabric layer and a spunlace non-woven fabric layer on two sides of the composite filter layer obtained in the step (4).
Example 3
A manufacturing method of a filter material specifically comprises the following steps:
step 1: ferulic acid-chitosan graft copolymer, menthol essential oil, polycaprolactone and polypropylene are mixed according to the mass ratio of 3: 1: 6: 90, melting and blending, and adopting a spray melting technology to obtain a non-woven fabric layer, wherein the fiber diameter of the non-woven fabric layer is 145-160 nm, the air permeability is 0.8m/s, and the thickness is 1 mm;
step 2: adding silver-loaded nano titanium dioxide powder with the particle size of 10-15 nm into 500 parts by weight of deionized water to prepare silver-loaded nano TiO with the concentration of 0.5mg/mL2Adding 50 parts of polyvinylpyrrolidone and 1 part of ammonium persulfate into the dispersion, fully mixing by an ultrasonic dispersion method, and uniformly spraying the dispersion on two sides of the surface of the non-woven fabric layer by an XKD-AS600 spraying machine at the spraying pressure of 0.05Mpa and the spraying amount of 0.05ml/cm 2;
and step 3: preparing a polytetrafluoroethylene microporous membrane by utilizing a biaxial stretching technology, and carrying out hot-pressing compounding on the polytetrafluoroethylene microporous membrane and the non-woven fabric layer obtained in the step (2) to obtain a composite filter layer; wherein the fiber diameter of the polytetrafluoroethylene microporous membrane is 60-80 nm, the air permeability is 0.35m/s, and the thickness is 0.2 mm;
and 4, step 4: performing corona treatment on the composite filter layer obtained in the step 3, wherein the density of stored charges of the composite filter layer is 3.2 multiplied by 10-3C/m2The corona treatment utilizes high-frequency high voltage to perform corona discharge on the surface of the composite filter layer for 2s, and the voltage of the corona treatment is 12000V/m2The discharge frequency is 20 Kz;
and 5: and (4) respectively compounding a waterproof non-woven fabric layer and a spunlace non-woven fabric layer on two sides of the composite filter layer obtained in the step (4).
Example 4
A manufacturing method of a filter material specifically comprises the following steps:
step 1: ferulic acid-chitosan graft copolymer, menthol essential oil, polycaprolactone and polypropylene are mixed according to the mass ratio of 5: 1: 9: 85, melting and blending, and adopting a spray melting technology to obtain a non-woven fabric layer, wherein the fiber diameter of the non-woven fabric layer is 137-151 nm, the air permeability is 0.6m/s, and the thickness is 1 mm;
step 2: adding silver-loaded nano titanium dioxide powder with the particle size of 10-15 nm into 500 parts by weight of deionized water to prepare silver-loaded nano TiO with the concentration of 0.2mg/mL2Adding 30 parts of polyvinylpyrrolidone and 0.5 part of ammonium persulfate into the dispersion, fully mixing by adopting an ultrasonic dispersion method, and uniformly spraying the dispersion on two sides of the surface of the non-woven fabric layer by an XKD-AS600 spraying machine in an atomized manner, wherein the spraying pressure is 0.05Mpa, and the spraying amount is 0.05ml/cm 2;
and step 3: preparing a polytetrafluoroethylene microporous membrane by utilizing a biaxial stretching technology, and carrying out hot-pressing compounding on the polytetrafluoroethylene microporous membrane and the non-woven fabric layer obtained in the step (2) to obtain a composite filter layer; wherein the fiber diameter of the polytetrafluoroethylene microporous membrane is 60-80 nm, the air permeability is 0.35m/s, and the thickness is 0.2 mm;
and 4, step 4: performing corona treatment on the composite filter layer obtained in the step 3, wherein the density of stored charges of the composite filter layer is 1 multiplied by 10-4C/m2Corona treatment using high frequencyThe high voltage is corona discharge on the surface of the composite filter layer for 2s, and the voltage of corona treatment is 12000V/m2The discharge frequency is 20 Kz;
and 5: and (4) respectively compounding a waterproof non-woven fabric layer and a spunlace non-woven fabric layer on two sides of the composite filter layer obtained in the step (4).
Comparative example 1
A manufacturing method of a mask filter material comprises the following steps:
step 1: polycaprolactone, menthol essential oil and polypropylene are mixed according to a mass ratio of 9: 1: 90, melting and blending, and adopting a spray melting technology to obtain a non-woven fabric layer; the rest steps are the same as the above example 2, the preparation conditions and the environment are the same as the above example 2, the fiber diameter of the prepared non-woven fabric layer is 135-142 nm, the air permeability is 0.8m/s, and the thickness is 1 mm.
Comparative example 2
A manufacturing method of a mask filter material comprises the following steps:
step 1: mixing ferulic acid-chitosan graft copolymer, menthol essential oil and polypropylene in a mass ratio of 5: 1: 94 melting and blending, adopting spray melting technology to obtain a non-woven fabric layer; the other steps were the same as in example 2, the preparation conditions and environment were the same as in example 2, and the nonwoven fabric layer obtained had a fiber diameter of 2 μm, an air permeability of 1.0m/s and a thickness of 1 mm.
Comparative example 3
KN95 filter material for protective mask manufactured by Kangfu medical science and technology Limited.
Comparative example 4
KN90 filter material for protective mask manufactured by Kangfu medical science and technology Limited.
Performance testing
The following performance tests were performed using the filter media of comparative examples 1 to 4 as a control group and the filter media prepared in the above examples 1 to 4 as a test group:
firstly, testing the filtration efficiency according to YY 0469-2011;
performing inspiration resistance test and expiration resistance test according to GB/T2626 and 2019;
carrying out biodegradability test according to GB/T19275 standard.
Test results
The results of the filter efficiency tests of the filter materials of comparative examples 1 to 4 and examples 1 to 4 are shown in the following table 1:
TABLE 1 Filter media filtration efficiency test results
| Group of | Efficiency of particle filtration | Bacterial filtration efficiency |
| Example 1 | 99.9% | 99.1% |
| Example 2 | 99.9% | 99.8% |
| Example 3 | 98.1% | 97.1% |
| Example 4 | 96.5% | 96.2% |
| Comparative example 1 | 96.3% | 96.0% |
| Comparative example 2 | 95.6% | 95.5% |
| Comparative example 3 | 95.2% | 95.0% |
| Comparative example 4 | 92.4% | 90.2% |
According to the data in table 1, it can be analyzed that the particle filtration efficiency and the bacteria filtration efficiency of the comparative example 2 are significantly reduced compared with those of the comparative example 2 in the comparative example 1, because the basic component in the filter material prepared in the comparative example 2 lacks polycaprolactone, the associativity of the ferulic acid-chitosan graft copolymer and the polypropylene is reduced, and the overall structure stability of the filter material is affected; in comparative example 1, the basic components of examples 2 to 4 contained the ferulic acid-chitosan graft copolymer, compared to examples 2 to 4, and thus the added amount of the ferulic acid-chitosan graft copolymer directly affected the bacterial filtration efficiency of the filter material; in addition, the essential oil of menthol obtained in example 1 has a certain antibacterial property.
The results of the test of the inhalation resistance and exhalation resistance of the filter materials of comparative examples 1 to 4 and examples 1 to 4 are shown in the following table 2:
TABLE 2 test results of inhalation resistance and exhalation resistance of filter media
| Group of | Resistance to air suction | Resistance to exhalation |
| Example 1 | 135Pa | 130Pa |
| Example 2 | 128Pa | 122Pa |
| Example 3 | 122Pa | 118Pa |
| Example 4 | 127Pa | 121Pa |
| Comparative example 1 | 116Pa | 110Pa |
| Comparative example 2 | 107Pa | 102Pa |
| Comparative example 3 | 202Pa | 200Pa |
| Comparative example 4 | 160Pa | 157Pa |
According to the data in table 2, it can be analyzed that the difference between the inhalation resistance and the exhalation resistance is large in the embodiments 1 to 4 and the comparative examples 1 to 2, and the pressure value of the inhalation resistance is larger than that of the exhalation resistance, which is beneficial to filtering; in addition, the inhalation resistance and exhalation resistance of examples 1 to 4 were significantly lower than those of comparative examples 3 and 4, and the air permeability of examples 1 to 4 was better.
The results of the biodegradability tests of the filters of comparative examples 1 to 4 and examples 1 to 4 are shown in Table 3 below:
TABLE 3 biodegradability test results of the filters
As can be analyzed from the results of the biodegradability test of the filter material in Table 3, examples 1 to 4 and comparative examples 1 to 2 are significantly superior to comparative examples 3 and 4, and therefore, the biodegradability of the filter material can be improved by adding ferulic acid-chitosan graft copolymer and polycaprolactone to the base component of the filter material, and the environment friendliness is improved.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (8)
1. A method for manufacturing a filter material is characterized in that: the method specifically comprises the following steps:
step 1: the ferulic acid-chitosan graft copolymer, polycaprolactone and polypropylene are mixed according to the mass ratio of 1-5: 1-10: 70-90, performing melt blending, and performing spray melting technology to obtain a non-woven fabric layer;
step 2: carrying out surface modification treatment on the non-woven fabric layer obtained in the step (1) by adopting polyvinylpyrrolidone and ammonium persulfate solution, and loading silver-loaded nano titanium dioxide powder on the surface of the non-woven fabric layer;
and step 3: preparing a polytetrafluoroethylene microporous membrane with the thickness not more than 1mm, and performing hot-pressing compounding on the polytetrafluoroethylene microporous membrane and the non-woven fabric layer obtained in the step 2 to obtain a composite filter layer;
and 4, step 4: performing corona treatment on the composite filter layer obtained in the step 3, wherein the storage charge density is 3 multiplied by 10-4～5.7×10-3C/m2(ii) a Corona treatment is carried out for 1.5-3 s by utilizing high-frequency high voltage to carry out corona discharge on the surface of the composite filter layer, and the voltage of the corona treatment is 11000-13000V/m2The discharge frequency is 15 KHz-25 Kz;
and 5: and (4) respectively compounding a waterproof non-woven fabric layer and a spunlace non-woven fabric layer on two sides of the composite filter layer obtained in the step (4).
2. The method for manufacturing a filter material according to claim 1, wherein: in the step 1, the preparation of the ferulic acid-chitosan graft copolymer comprises the steps of:
step A: dissolving chitosan powder in a citric acid-sodium citrate buffer solution with the pH value of 6.0-4.8, adding 60-100 mL of 30% hydrogen peroxide solution, and reacting at 50-70 ℃ for 60-90 min to obtain a chitosan solution with the chitosan concentration of 100 mmol; cooling the chitosan solution to room temperature, sequentially adding the methanol solution dissolved with the ferulic acid and the laccase, and uniformly stirring to obtain a mixed solution;
and B: and introducing oxygen into the mixed solution, wherein the oxygen introduction amount is 30-50L/min, after the mixed solution reacts for 1.5-3 h, dialyzing for 72h by using a dialysis membrane with the molecular weight of 14000, removing unreacted ferulic acid, thoroughly rinsing the product obtained by dialysis by using methanol, ethanol and water, and drying in vacuum to obtain the chitosan-ferulic acid graft copolymer.
3. The method for manufacturing a filter material according to claim 1, wherein: in the step 1, 0.5-2 parts by mass of menthol essential oil is added.
4. The method for manufacturing a filter material according to claim 1, wherein: in the step 2, the silver-loaded nano titanium dioxide powder is added into 100 to 1000 parts by weight of deionized water to prepare silver-loaded nano TiO with the concentration of 0.2mg/mL to 1mg/mL2And adding 30-80 parts of polyvinylpyrrolidone and 0.05-5 parts of ammonium persulfate into the dispersion liquid, fully mixing by adopting a mechanical stirring or ultrasonic dispersion method, and spraying to the non-woven fabric layer.
5. The method for manufacturing a filter material according to claim 1, wherein: in the step 3, the fiber diameter of the polytetrafluoroethylene microporous membrane is 60-80 nm, the air permeability is 0.3-0.5 m/s, and the thickness is 0.05-0.3 mm.
6. The method for manufacturing a filter material according to claim 1 or 4, wherein: in the step 2, the particle size of the silver-loaded nano titanium dioxide powder is 10-15 nm.
7. The method for manufacturing a filter material according to claim 2, wherein: and D, the concentration of the ferulic acid in the mixed solution prepared in the step A is 5-10 mmol, and the density of the laccase is 2.5-3.0U/mL.
8. The method for manufacturing a filter material according to claim 1, wherein: in the step 1, the fiber diameter of the non-woven fabric layer is 100-200 nm, the air permeability is 0.5-0.8 m/s, and the thickness is 0.5-2 mm.
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| CN105771421A (en) * | 2016-03-09 | 2016-07-20 | 仙桃永利医疗用品有限公司 | Non-woven composite material for filter respirator |
| CN111364246A (en) * | 2020-03-24 | 2020-07-03 | 新昌县高纤纺织有限公司 | Preparation method of antibacterial non-woven fabric |
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| KR20010095335A (en) * | 2000-04-27 | 2001-11-07 | 김기진 | Filter cartridge using chitosan as binder and its production method |
| CN105771421A (en) * | 2016-03-09 | 2016-07-20 | 仙桃永利医疗用品有限公司 | Non-woven composite material for filter respirator |
| CN111364246A (en) * | 2020-03-24 | 2020-07-03 | 新昌县高纤纺织有限公司 | Preparation method of antibacterial non-woven fabric |
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