CN111364246A - Preparation method of antibacterial non-woven fabric - Google Patents
Preparation method of antibacterial non-woven fabric Download PDFInfo
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- CN111364246A CN111364246A CN202010210801.6A CN202010210801A CN111364246A CN 111364246 A CN111364246 A CN 111364246A CN 202010210801 A CN202010210801 A CN 202010210801A CN 111364246 A CN111364246 A CN 111364246A
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- 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
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
- D06M15/267—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof of unsaturated carboxylic esters having amino or quaternary ammonium groups
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- 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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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/34—Esters containing nitrogen, e.g. N,N-dimethylaminoethyl (meth)acrylate
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
- D06M14/26—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin
- D06M14/30—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention discloses a preparation method of an antibacterial non-woven fabric, which comprises the following steps: firstly, the following components in parts by weight: preparing 90-100 parts of PET, 8-10 parts of glycidyl methacrylate grafted polyolefin elastomer and 3-4 parts of modified chitosan; secondly, preparing a copolymer from PET and modified chitosan; thirdly, carrying out electrostatic spinning on the copolymer to prepare base cloth; fourthly, modifying the surface of the base cloth; fifthly, preparing the antibacterial base cloth; and sixthly, performing hydrophilic modification on the surface. According to the invention, the modified chitosan is added into the raw materials and is uniformly distributed in the PET matrix, so that the base fabric has good antibacterial performance, and the quaternary ammonium salt antibacterial treatment is carried out on the surface of the base fabric, so that the antibacterial performance is further improved, and the two reinforcing modes have strong water washing resistance, so that the non-woven fabric has lasting antibacterial performance; the anti-pollution capability is improved by improving the hydrophilic performance of the non-woven fabric; the non-woven fabric obtained by the invention has wide application value in the field of sewage treatment.
Description
Technical Field
The invention belongs to the field of non-woven fabrics, and particularly relates to a preparation method of an antibacterial non-woven fabric.
Background
The non-woven fabric is a non-woven fabric which is formed by directly utilizing high polymer slices, short fibers or filaments to form a net through air flow or machinery, then carrying out spunlace, needling or hot rolling reinforcement, and finally carrying out after-treatment. A novel fiber product having a soft, air-permeable and planar structure has the advantages of no generation of lint, toughness, durability, silky softness, and a cotton feel. The terylene (PET) non-woven fabric as a filtering material and a base cloth material has the advantages of high strength, good chemical stability, corrosion resistance, no toxicity, no stimulation and the like, and is widely applied to water pollution treatment. Ordinary (PET) non-woven fabrics in the use, do not have antibacterial property by itself, are in sewage environment for a long time, and the surface gathers a large amount of bacteriums, and then influences the performance of non-woven fabrics as the treatment film.
The Chinese patent with the patent number of CN201611272815.0 discloses an antibacterial non-woven fabric and a preparation method thereof, wherein the non-woven fabric comprises a spun-bonded non-woven fabric layer, a first antibacterial non-woven fabric layer, a second antibacterial non-woven fabric layer and a viscose non-woven fabric layer, the first antibacterial non-woven fabric layer and the second antibacterial non-woven fabric layer are positioned between the anti-sticking non-woven fabric layer and the viscose non-woven fabric layer, the first antibacterial non-woven fabric layer is positioned above the second antibacterial non-woven fabric layer, and a melt-blown non-woven fabric layer is also arranged between the first antibacterial non-woven fabric layer and the second antibacterial non-woven fabric; the first antibacterial non-woven fabric layer comprises the following raw materials in parts by weight: 8-12 parts of silver nitrate solution, 10-15 parts of chitosan, 20-40 parts of polyacrylic acid solution, 3-5 parts of zinc pyrithione and 40-60 parts of absorbent fiber; the second antibacterial non-woven fabric layer comprises the following raw materials in parts by weight: 10-20 parts of silver-carrying antibacterial material, 60-80 parts of polyethylene and polyethylene wax with the molecular weight of 2000-3000. Although silver-based antibacterial bodies are added between the layers of the nonwoven fabric, the nonwoven fabric has a drawback that the antibacterial active ingredient is not firmly bonded to the matrix fiber and is not uniformly dispersed.
Disclosure of Invention
The invention aims to provide a preparation method of an antibacterial non-woven fabric, which comprises the steps of adding modified chitosan into a base fabric raw material, uniformly distributing the chitosan in a PET matrix, stably exerting antibacterial performance, enabling the base fabric to have good antibacterial performance, and grafting an antibacterial agent on the surface of the base fabric through a chemical bonding mode by performing quaternary ammonium salt antibacterial treatment on the surface of the base fabric, so that the antibacterial performance of the non-woven fabric is further improved, and the two modes of reinforcing the PET non-woven fabric have strong water washing resistance, so that the non-woven fabric has lasting antibacterial performance; in addition, the hydrophilic property of the PET non-woven fabric is improved by carrying out hydrophilic modification treatment on the surface of the non-woven fabric, so that the anti-pollution capacity of the non-woven fabric is improved; the non-woven fabric obtained by the invention has lasting antibacterial performance and anti-pollution capacity, has higher filtering efficiency in the sewage treatment process, and has wide application value.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of an antibacterial non-woven fabric comprises the following steps:
firstly, the following components in parts by weight: 90-100 parts of PET, 8-10 parts of glycidyl methacrylate grafted polyolefin elastomer and 3-4 parts of modified chitosan, and weighing the raw materials;
secondly, vacuum drying PET at 120 ℃ until the water content is less than 50ppm, vacuum drying the modified chitosan at 80 ℃ for 12h, and then adding the PET and the modified chitosan into a double-screw extruder for extrusion granulation to obtain a copolymer;
thirdly, dissolving the copolymer in hexafluoroisopropanol to prepare 200g/L spinning solution, and then performing electrostatic spinning to prepare base cloth;
fourthly, putting the base cloth into absolute ethyl alcohol for ultrasonic treatment for 30-40min, then washing the base cloth with ultrapure water, immersing the base cloth into an ethanol solution of 1, 5-pentanediamine, reacting for 18-20h in a water bath kettle at 55 ℃, taking out the base cloth, washing the base cloth with the ultrapure water, immersing the base cloth into the ethanol solution of glutaraldehyde, oscillating the base cloth for reaction for 120-130min at 26-30 ℃, taking out the base cloth, washing the base cloth for 3-4 times with the ultrapure water, and placing the base cloth in a refrigerator at 4-5 ℃ for later use;
fifthly, weighing methacryloyloxyethyl trimethyl ammonium chloride, acrylamide and allyl glycidyl ether, putting the weighed materials into a four-neck flask according to a certain proportion, adding an initiator ammonium persulfate under the conditions of nitrogen atmosphere and constant temperature of 70 ℃, reacting for 4-5h, cooling at room temperature, repeatedly purifying by acetone and ethanol, and drying in vacuum to obtain the antibacterial agent; dissolving an antibacterial agent in absolute ethyl alcohol to obtain an antibacterial liquid with the mass fraction of 7% -8%, immersing the base cloth treated in the fourth step into the antibacterial liquid, carrying out oscillation reaction for 2 hours at the temperature of 30-35 ℃, taking out and repeatedly washing with a large amount of pure water to obtain the antibacterial base cloth;
sixthly, dissolving benzophenone by using isopropanol, then adding a certain amount of hydroxyethyl methacrylate, fully stirring to form a uniform and stable solution, then adding deionized water, and uniformly stirring to prepare a modified solution; soaking the antibacterial base fabric in the modified solution for 12h, introducing nitrogen for 5-8min, irradiating the system under 365nm ultraviolet rays for 50-60min, taking out, soaking in acetone for 12h, washing with clear water for 5-6 times, and drying in an oven at 70 ℃ to obtain the non-woven fabric.
Further, the modified chitosan in the first step is prepared by the following method:
dissolving chitosan in an acetic acid solution to prepare a chitosan-acetic acid solution with the mass concentration of 1%, and standing for defoaming for later use; dropwise adding citral into the chitosan-acetic acid solution according to the volume ratio of 1:40, stirring for 12h, and adjusting the pH value to 4.8-5.0; dropwise adding a 15% sodium borohydride aqueous solution into the reaction system under stirring at 500r/min, adjusting the pH value of the reaction system to 7 after 2h, repeatedly washing with absolute ethyl alcohol, performing suction filtration, and performing vacuum drying and grinding to obtain the modified chitosan.
Further, the concentration of the ethanol solution of 1, 5-pentanediamine in the fourth step was 2mol/L, and the volume fraction of the ethanol solution of glutaraldehyde was 10%.
Further, the mass ratio of the methacryloyloxyethyl trimethyl ammonium chloride to the acrylamide in the fifth step is 2: 1; the addition amounts of the allyl glycidyl ether and the initiator ammonium persulfate are respectively 5 percent and 2 percent of the total mass of the system.
Furthermore, the dosage ratio of the benzophenone, the isopropanol and the hydroxyethyl methacrylate in the sixth step is 0.1:10: 4; the ratio of isopropanol/deionized water was 1: 4.
The invention has the beneficial effects that:
the modified chitosan and the elastomer are added into the raw material of the base fabric, and the base fabric is obtained by melting and blending PET, the modified chitosan and the elastomer; the glycidyl methacrylate grafted polyolefin elastomer is an elastomer, the epoxy group of GMA-g-POE and the terminal carboxyl or terminal hydroxyl of a PET molecular chain are subjected to chemical reaction to generate a copolymer, and the copolymer is used as an interface modifier to improve the compatibility of a matrix and a disperse phase and reduce the interface tension, so that the notch impact strength of the blend can be improved; in addition, when the blending material is subjected to instant impact, the elastomer in the blending system can absorb most impact energy instantly, so that the toughness of the PET is effectively improved; the chitosan surface contains active amino-NH2Functional group, -NH2Under the action of sodium borohydride, the organic silicon-boron-containing organic silicon-boron composite material reacts with aldehyde groups on citrus aldehyde, so that a citrus aldehyde molecular chain is grafted on a chitosan molecule, on one hand, the citrus aldehyde molecule contains a longer alkyl chain and a six-membered ring with larger steric hindrance, the agglomeration phenomenon among the chitosan molecules can be effectively reduced, the longer alkyl chain and the six-membered ring have higher compatibility with a PET matrix, the chitosan is promoted to be uniformly distributed in the PET matrix, and the antibacterial performance is stably exerted; on the other hand, the myrac aldehyde molecules contain unsaturated C ═ C double bonds, and when the prepared non-woven fabric base fabric is subjected to subsequent ultraviolet irradiation grafting, the unsaturated C ═ C double bonds can be subjected to grafting reaction with the C ═ C double bonds on the hydroxyethyl methacrylate, so that the grafting rate of the non-woven fabric to the hydroxyethyl methacrylate is improved, and the hydrophilic performance of the non-woven fabric is further improved;
the invention adopts quaternary ammonium salt to carry out antibacterial modification treatment on base cloth, and the base cloth is coated with methacryloyloxyethyl trimethyl ammonium chlorideThe C ═ C double bond and the C ═ C double bond on acrylamide are subjected to free radical polymerization reaction under the action of an initiator, and the generated polymer is an antibacterial agent because methacryloyloxyethyl trimethyl ammonium chloride is a quaternary ammonium salt (the quaternary ammonium salt antibacterial agent has high antibacterial efficiency and is nontoxic); the antibacterial agent contains-NH on the molecule2The amino group reacts with the aldehyde group exposed on the base fabric, so that the antibacterial agent is grafted on the surface of the non-woven fabric in a chemical bonding mode, and the non-woven fabric is endowed with good antibacterial performance; the antibacterial agent is connected to the non-woven fabric through chemical bonding, and has the advantage of water washing resistance;
according to the invention, hydrophilic modification treatment is carried out on the non-woven fabric, double bonds on the surface of hydroxyethyl methacrylate can react with terminal carboxyl on a PET molecular chain under the irradiation of an ultraviolet lamp and can also react with chitosan grafted double bonds in a matrix, so that the molecular chain of the hydroxyethyl methacrylate is grafted on the surface of the non-woven fabric, and the purpose of introducing hydroxyl-OH is further achieved, OH is a hydrophilic functional group, and the hydrophilicity of the non-woven fabric can be effectively improved; generally, increasing the hydrophilicity of non-woven fabrics is one of the approaches to solving the pollution problem of non-woven fabrics, and generally, the hydrophilicity of the membranes is improved, and the pollution resistance of the membranes is inevitably enhanced; in addition, the hydroxyethyl methacrylate is bonded on the molecular chain of the non-woven fabric through a chemical bond, so that the bonding strength is high, and the washing resistance is good;
according to the invention, the modified chitosan is added into the raw material of the base fabric, and the chitosan is uniformly distributed in the PET matrix, so that the antibacterial performance is stably exerted, the base fabric has good antibacterial performance, and the quaternary ammonium salt antibacterial treatment is carried out on the surface of the base fabric, so that the antibacterial agent is grafted to the surface of the non-woven fabric in a chemical bonding mode, and the antibacterial performance of the non-woven fabric is further improved; in addition, the hydrophilic property of the PET non-woven fabric is improved by carrying out hydrophilic modification treatment on the surface of the non-woven fabric, so that the anti-pollution capacity of the non-woven fabric is improved; the non-woven fabric obtained by the invention has lasting antibacterial performance and anti-pollution capacity, has higher filtering efficiency in the sewage treatment process, and has wide application value.
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.
A preparation method of an antibacterial non-woven fabric comprises the following steps:
firstly, the following components in parts by weight: 90-100 parts of polyester resin (PET), 8-10 parts of glycidyl methacrylate grafted polyolefin elastomer (GMA-g-POE) and 3-4 parts of modified chitosan;
the glycidyl methacrylate grafted polyolefin elastomer is an elastomer, the epoxy group of GMA-g-POE and the terminal carboxyl or terminal hydroxyl of a PET molecular chain are subjected to chemical reaction to generate a copolymer, and the copolymer is used as an interface modifier to improve the compatibility of a matrix and a disperse phase and reduce the interface tension, so that the notch impact strength of the blend can be improved; in addition, when the blending material is subjected to instant impact, the elastomer in the blending system can absorb most impact energy instantly, so that the toughness of the PET is effectively improved;
the modified chitosan is prepared by the following method:
dissolving chitosan in an acetic acid solution to prepare a chitosan-acetic acid solution with the mass concentration of 1%, and standing for defoaming for later use; dropwise adding citral into the chitosan-acetic acid solution according to the volume ratio of 1:40, stirring for 12h, and adjusting the pH value to 4.8-5.0; dropwise adding a 15% sodium borohydride aqueous solution into the reaction system under stirring at 500r/min, adjusting the pH value of the reaction system to 7 after 2 hours, repeatedly washing and filtering with absolute ethyl alcohol, and drying and grinding in vacuum to obtain modified chitosan;
wherein, the adding amount of the sodium borohydride aqueous solution is 8 to 10 percent of the volume of the reaction system;
the chitosan surface contains active amino-NH2Functional group, -NH2In the presence of sodium borohydrideUnder the action, the chitosan reacts with aldehyde groups on the citral to graft a citral molecular chain onto the chitosan molecules, so that on one hand, the citral molecules contain longer alkyl chains and six-membered rings with larger steric hindrance, the agglomeration phenomenon among the chitosan molecules can be effectively reduced, the longer alkyl chains and the six-membered rings have higher compatibility with a PET matrix, the chitosan is promoted to be uniformly distributed in the PET matrix, and the antibacterial performance is stably exerted; on the other hand, the myrac aldehyde molecules contain unsaturated C ═ C double bonds, and when the prepared non-woven fabric base fabric is subjected to subsequent ultraviolet irradiation grafting, the unsaturated C ═ C double bonds can be subjected to grafting reaction with the C ═ C double bonds on the hydroxyethyl methacrylate, so that the grafting rate of the non-woven fabric to the hydroxyethyl methacrylate is improved, and the hydrophilic performance of the non-woven fabric is further improved;
secondly, vacuum drying PET at 120 ℃ until the water content is less than 50ppm, vacuum drying the modified chitosan at 80 ℃ for 12h, and then adding the PET and the modified chitosan into a double-screw extruder for extrusion granulation to obtain a copolymer;
thirdly, dissolving the copolymer in hexafluoroisopropanol to prepare 200g/L spinning solution, and then performing electrostatic spinning to prepare base cloth;
fourthly, putting the base cloth into absolute ethyl alcohol for ultrasonic treatment for 30-40min, then washing the base cloth with ultrapure water, immersing the base cloth into an ethanol solution of 1, 5-pentanediamine (the concentration of the ethanol solution of the 1, 5-pentanediamine is 2mol/L), reacting for 18-20h in a water bath kettle at 55 ℃, taking out the base cloth, washing the base cloth with the ultrapure water, immersing the base cloth into the ethanol solution of glutaraldehyde (the volume fraction of the ethanol solution of the glutaraldehyde is 10%), oscillating and reacting for 120-130min at 26-30 ℃, taking out, washing the base cloth with the ultrapure water for 3-4 times, and placing the base cloth in a refrigerator at 4-5 ℃ for standby application;
1, 5-Pentanediamine is a compound having amino groups at both ends, amino-NH2Can react with hydroxyl-OH or carboxyl-COOH on the molecular chain of PET to graft 1, 5-pentanediamine on the surface of the base cloth, and only one end of the molecular chain of the 1, 5-pentanediamine is-NH because the molecular chain of the 1, 5-pentanediamine is short2Can react with PET molecular chain, and the other end is left with naked-NH2(ii) a Similarly, after glutaraldehyde treatment, the exposed amino group on the glutaraldehyde continues to react with the aldehyde at one end of the glutaraldehyde moleculeThe base reacts, glutaraldehyde molecules are grafted on the other end of the glutaraldehyde, and aldehyde groups on one exposed end of the glutaraldehyde;
fifthly, weighing methacryloyloxyethyl trimethyl ammonium chloride, acrylamide and allyl glycidyl ether, putting the weighed materials into a four-neck flask according to a certain proportion, adding an initiator ammonium persulfate under the conditions of nitrogen atmosphere and constant temperature of 70 ℃, reacting for 4-5h, cooling at room temperature, repeatedly purifying by acetone and ethanol, and drying in vacuum to obtain the antibacterial agent; dissolving an antibacterial agent in absolute ethyl alcohol to obtain an antibacterial liquid with the mass fraction of 7% -8%, immersing the base cloth treated in the fourth step into the antibacterial liquid, carrying out oscillation reaction for 2 hours at the temperature of 30-35 ℃, taking out and repeatedly washing with a large amount of pure water to obtain the antibacterial base cloth;
the mass ratio of the methacryloyloxyethyl trimethyl ammonium chloride to the acrylamide is 2: 1; the addition amounts of the allyl glycidyl ether and the initiator ammonium persulfate are respectively 5 percent and 2 percent of the total mass of the system;
the C ═ C double bond on the methacryloxyethyl trimethyl ammonium chloride and the C ═ C double bond on the acrylamide are subjected to free radical polymerization reaction under the action of an initiator, and the methacryloxyethyl trimethyl ammonium chloride is a quaternary ammonium salt (the quaternary ammonium salt antibacterial agent has high antibacterial efficiency and is non-toxic), so that the generated polymer is an antibacterial agent; the antibacterial agent contains-NH on the molecule2The amino group reacts with the aldehyde group exposed on the base fabric, so that the antibacterial agent is grafted on the surface of the non-woven fabric in a chemical bonding mode, and the non-woven fabric is endowed with good antibacterial performance; the antibacterial agent is connected to the non-woven fabric through chemical bonding, and has the advantage of water washing resistance;
sixthly, dissolving benzophenone by using isopropanol, then adding a certain amount of hydroxyethyl methacrylate, fully stirring to form a uniform and stable solution, then adding deionized water, and uniformly stirring to prepare a modified solution (the ratio of isopropanol to water is 1: 4); soaking the antibacterial base fabric in the modified solution for 12h, introducing nitrogen for 5-8min, irradiating the system under 365nm ultraviolet rays for 50-60min, taking out, soaking with acetone for 12h to remove surface homopolymers and impurities, washing with clear water for 5-6 times, and drying in a 70 ℃ oven to obtain a non-woven fabric;
the dosage ratio of the benzophenone, the isopropanol and the hydroxyethyl methacrylate is 0.1:10: 4;
double bonds on the surface of the hydroxyethyl methacrylate can react with terminal carboxyl on a PET molecular chain under the irradiation of an ultraviolet lamp and can also react with chitosan grafted double bonds in a matrix, so that the molecular chain of the hydroxyethyl methacrylate is grafted on the surface of the non-woven fabric, and the aim of introducing hydroxyl-OH is fulfilled, wherein-OH is a hydrophilic functional group, and the hydrophilicity of the non-woven fabric can be effectively improved; generally, increasing the hydrophilicity of non-woven fabrics is one of the approaches to solving the pollution problem of non-woven fabrics, and generally, the hydrophilicity of the membranes is improved, and the pollution resistance of the membranes is inevitably enhanced; in addition, the hydroxyethyl methacrylate is bonded on the molecular chain of the non-woven fabric through a chemical bond, so that the bonding strength is high, and the washing resistance is good.
Example 1
An antibacterial non-woven fabric is prepared by the following steps:
firstly, the following components in parts by weight: weighing 90 parts of PET, 8 parts of glycidyl methacrylate grafted polyolefin elastomer and 3 parts of modified chitosan;
secondly, vacuum drying PET at 120 ℃ until the water content is less than 50ppm, vacuum drying the modified chitosan at 80 ℃ for 12h, and then adding the PET and the modified chitosan into a double-screw extruder for extrusion granulation to obtain a copolymer;
thirdly, dissolving the copolymer in hexafluoroisopropanol to prepare 200g/L spinning solution, and then performing electrostatic spinning to prepare base cloth;
fourthly, putting the base cloth into absolute ethyl alcohol for ultrasonic treatment for 30min, then washing the base cloth with ultrapure water, immersing the base cloth into an ethanol solution of 1, 5-pentanediamine, reacting for 18h in a water bath kettle at 55 ℃, taking out the base cloth, washing the base cloth with the ultrapure water, immersing the base cloth into the ethanol solution of glutaraldehyde, oscillating and reacting for 120min at 26 ℃, taking out the base cloth, washing the base cloth for 3-4 times with the ultrapure water, and placing the base cloth in a refrigerator at 4 ℃ for later use;
fifthly, weighing methacryloyloxyethyl trimethyl ammonium chloride, acrylamide and allyl glycidyl ether, putting the weighed materials into a four-neck flask according to a certain proportion, adding an initiator ammonium persulfate under the conditions of nitrogen atmosphere and constant temperature of 70 ℃, reacting for 4 hours, cooling at room temperature, repeatedly purifying by acetone and ethanol, and drying in vacuum to obtain the antibacterial agent; dissolving an antibacterial agent in absolute ethyl alcohol to obtain an antibacterial liquid with the mass fraction of 7%, immersing the base cloth treated in the fourth step into the antibacterial liquid, carrying out oscillation reaction for 2 hours at the temperature of 30 ℃, taking out and repeatedly washing the base cloth by using a large amount of pure water to obtain the antibacterial base cloth;
sixthly, dissolving benzophenone by using isopropanol, then adding a certain amount of hydroxyethyl methacrylate, fully stirring to form a uniform and stable solution, then adding deionized water, and uniformly stirring to prepare a modified solution; soaking the antibacterial base fabric in the modified solution for 12h, introducing nitrogen for 6.5min, irradiating the system with 365nm ultraviolet rays for 55min, taking out, soaking in acetone for 12h, washing with clear water for 5 times, and oven drying at 70 deg.C to obtain the non-woven fabric.
Example 2
An antibacterial non-woven fabric is prepared by the following steps:
firstly, the following components in parts by weight: weighing 95 parts of PET, 9 parts of glycidyl methacrylate grafted polyolefin elastomer and 3.5 parts of modified chitosan;
secondly, vacuum drying PET at 120 ℃ until the water content is less than 50ppm, vacuum drying the modified chitosan at 80 ℃ for 12h, and then adding the PET and the modified chitosan into a double-screw extruder for extrusion granulation to obtain a copolymer;
thirdly, dissolving the copolymer in hexafluoroisopropanol to prepare 200g/L spinning solution, and then performing electrostatic spinning to prepare base cloth;
fourthly, putting the base cloth into absolute ethyl alcohol for 35min by ultrasonic treatment, then washing the base cloth by using ultrapure water, immersing the base cloth into an ethanol solution of 1, 5-pentanediamine, reacting for 19h in a water bath kettle at 55 ℃, taking out the base cloth, washing the base cloth by using the ultrapure water, immersing the base cloth into the ethanol solution of glutaraldehyde, oscillating and reacting for 125min at 28 ℃, taking out the base cloth, washing the base cloth for 4 times by using the ultrapure water, and placing the base cloth in a refrigerator at 5 ℃ for later use;
fifthly, weighing methacryloyloxyethyl trimethyl ammonium chloride, acrylamide and allyl glycidyl ether, putting the weighed materials into a four-neck flask according to a certain proportion, adding an initiator ammonium persulfate under the conditions of nitrogen atmosphere and constant temperature of 70 ℃, reacting for 5 hours, cooling at room temperature, repeatedly purifying by acetone and ethanol, and drying in vacuum to obtain the antibacterial agent; dissolving an antibacterial agent in absolute ethyl alcohol to obtain an antibacterial solution with the mass fraction of 8%, immersing the base cloth treated in the fourth step into the antibacterial solution, carrying out oscillation reaction for 2 hours at the temperature of 32 ℃, taking out and repeatedly washing the base cloth by using a large amount of pure water to obtain the antibacterial base cloth;
sixthly, dissolving benzophenone by using isopropanol, then adding a certain amount of hydroxyethyl methacrylate, fully stirring to form a uniform and stable solution, then adding deionized water, and uniformly stirring to prepare a modified solution; soaking the antibacterial base fabric in the modified solution for 12h, introducing nitrogen for 7min, irradiating the system with 365nm ultraviolet rays for 55min, taking out, soaking in acetone for 12h, washing with clear water for 5 times, and oven drying at 70 deg.C to obtain the non-woven fabric.
Example 3
An antibacterial non-woven fabric is prepared by the following steps:
firstly, the following components in parts by weight: weighing 100 parts of PET, 10 parts of glycidyl methacrylate grafted polyolefin elastomer and 4 parts of modified chitosan;
secondly, vacuum drying PET at 120 ℃ until the water content is less than 50ppm, vacuum drying the modified chitosan at 80 ℃ for 12h, and then adding the PET and the modified chitosan into a double-screw extruder for extrusion granulation to obtain a copolymer;
thirdly, dissolving the copolymer in hexafluoroisopropanol to prepare 200g/L spinning solution, and then performing electrostatic spinning to prepare base cloth;
fourthly, putting the base fabric into absolute ethyl alcohol for ultrasonic treatment for 40min, then washing the base fabric with ultrapure water, immersing the base fabric into an ethanol solution of 1, 5-pentanediamine, reacting for 20h in a water bath kettle at 55 ℃, taking out the base fabric, washing the base fabric with the ultrapure water, immersing the base fabric into the ethanol solution of glutaraldehyde, oscillating and reacting for 130min at 30 ℃, taking out the base fabric, washing the base fabric for 3-4 times with the ultrapure water, and placing the base fabric in a refrigerator at 5 ℃ for later use;
fifthly, weighing methacryloyloxyethyl trimethyl ammonium chloride, acrylamide and allyl glycidyl ether, putting the weighed materials into a four-neck flask according to a certain proportion, adding an initiator ammonium persulfate under the conditions of nitrogen atmosphere and constant temperature of 70 ℃, reacting for 5 hours, cooling at room temperature, repeatedly purifying by acetone and ethanol, and drying in vacuum to obtain the antibacterial agent; dissolving an antibacterial agent in absolute ethyl alcohol to obtain an antibacterial solution with the mass fraction of 8%, immersing the base cloth treated in the fourth step into the antibacterial solution, carrying out oscillation reaction for 2 hours at the temperature of 35 ℃, taking out and repeatedly washing the base cloth by using a large amount of pure water to obtain the antibacterial base cloth;
sixthly, dissolving benzophenone by using isopropanol, then adding a certain amount of hydroxyethyl methacrylate, fully stirring to form a uniform and stable solution, then adding deionized water, and uniformly stirring to prepare a modified solution; soaking the antibacterial base fabric in the modified solution for 12h, introducing nitrogen for 8min, irradiating the system with 365nm ultraviolet ray for 60min, taking out, soaking in acetone for 12h, washing with clear water for 6 times, and oven drying at 70 deg.C to obtain the non-woven fabric.
Comparative example 1
The modified chitosan in example 1 was replaced with normal chitosan, and the remaining raw materials and preparation process were unchanged.
Comparative example 2
The fourth and fifth steps of example 1 were eliminated and the remaining raw materials and preparation were unchanged.
Comparative example 3
The sixth step in example 1 was eliminated and the remaining raw materials and preparation were unchanged.
Comparative example 4
PET non-woven fabric.
The nonwoven fabrics obtained in examples 1 to 3 and comparative examples 1 to 3 were subjected to the following performance tests: testing the mechanical property of the non-woven fabric by reference to GB/T3923-2013; testing the bacteriostasis rate of the non-woven fabric to escherichia coli and staphylococcus aureus, and testing the water contact angle; testing the soaping fastness by referring to GB/T3921-; the test results are given in the following table:
as can be seen from the above table, the warp breaking strength of the nonwoven fabrics prepared in examples 1-3 is 1.85-1.91MPa, and the value breaking strength is 1.49-1.56MPa, which indicates that the nonwoven fabrics prepared by the invention have higher mechanical properties through blending of elastomers compared with pure PET nonwoven fabrics; the water contact angle of the non-woven fabrics prepared in the examples 1 to 3 is 57.6 to 57.9 degrees, which shows that the non-woven fabrics of the invention have better hydrophilic performance; the bacteriostasis rate of the non-woven fabrics prepared in the embodiments 1-3 to escherichia coli is 99.6-99.9%, and the bacteriostasis rate to staphylococcus aureus is 98.3-98.6%, which shows that the non-woven fabrics prepared by the invention have higher antibacterial performance; after the water-based antibacterial fabric is waterborne, the reduction degree of the antibacterial rate of the non-woven fabric to escherichia coli and staphylococcus aureus is very small, which shows that the antibacterial performance of the water-based antibacterial fabric has durability and water washing resistance; the comparative example 1 is combined to show that the chitosan can improve the compatibility with a PET matrix after being modified, so as to exert the antibacterial performance, and the chitosan can have a synergistic effect with the subsequent hydrophilic modification after being modified, so as to react with a hydrophilic monomer, so as to improve the hydrophilic modification effect; the antibacterial property of the nonwoven fabric can be further improved by the quaternary ammonium salt antibacterial treatment performed on the surface of the nonwoven fabric, compared with comparative example 2.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (5)
1. The preparation method of the antibacterial non-woven fabric is characterized by comprising the following steps:
firstly, the following components in parts by weight: 90-100 parts of PET, 8-10 parts of glycidyl methacrylate grafted polyolefin elastomer and 3-4 parts of modified chitosan, and weighing the raw materials;
secondly, vacuum drying PET at 120 ℃ until the water content is less than 50ppm, vacuum drying the modified chitosan at 80 ℃ for 12h, and then adding the PET and the modified chitosan into a double-screw extruder for extrusion granulation to obtain a copolymer;
thirdly, dissolving the copolymer in hexafluoroisopropanol to prepare 200g/L spinning solution, and then performing electrostatic spinning to prepare base cloth;
fourthly, putting the base cloth into absolute ethyl alcohol for ultrasonic treatment for 30-40min, then washing the base cloth with ultrapure water, immersing the base cloth into an ethanol solution of 1, 5-pentanediamine, reacting for 18-20h in a water bath kettle at 55 ℃, taking out the base cloth, washing the base cloth with the ultrapure water, immersing the base cloth into the ethanol solution of glutaraldehyde, oscillating the base cloth for reaction for 120-130min at 26-30 ℃, taking out the base cloth, washing the base cloth for 3-4 times with the ultrapure water, and placing the base cloth in a refrigerator at 4-5 ℃ for later use;
fifthly, weighing methacryloyloxyethyl trimethyl ammonium chloride, acrylamide and allyl glycidyl ether, putting the weighed materials into a four-neck flask according to a certain proportion, adding an initiator ammonium persulfate under the conditions of nitrogen atmosphere and constant temperature of 70 ℃, reacting for 4-5h, cooling at room temperature, repeatedly purifying by acetone and ethanol, and drying in vacuum to obtain the antibacterial agent; dissolving an antibacterial agent in absolute ethyl alcohol to obtain an antibacterial liquid with the mass fraction of 7% -8%, immersing the base cloth treated in the fourth step into the antibacterial liquid, carrying out oscillation reaction for 2 hours at the temperature of 30-35 ℃, taking out and repeatedly washing with a large amount of pure water to obtain the antibacterial base cloth;
sixthly, dissolving benzophenone by using isopropanol, then adding a certain amount of hydroxyethyl methacrylate, fully stirring to form a uniform and stable solution, then adding deionized water, and uniformly stirring to prepare a modified solution; soaking the antibacterial base fabric in the modified solution for 12h, introducing nitrogen for 5-8min, irradiating the system under 365nm ultraviolet rays for 50-60min, taking out, soaking in acetone for 12h, washing with clear water for 5-6 times, and drying in an oven at 70 ℃ to obtain the non-woven fabric.
2. The method for preparing an antibacterial non-woven fabric according to claim 1, wherein the modified chitosan in the first step is prepared by the following method:
dissolving chitosan in an acetic acid solution to prepare a chitosan-acetic acid solution with the mass concentration of 1%, and standing for defoaming for later use; dropwise adding citral into the chitosan-acetic acid solution according to the volume ratio of 1:40, stirring for 12h, and adjusting the pH value to 4.8-5.0; dropwise adding a 15% sodium borohydride aqueous solution into the reaction system under stirring at 500r/min, adjusting the pH value of the reaction system to 7 after 2h, repeatedly washing with absolute ethyl alcohol, performing suction filtration, and performing vacuum drying and grinding to obtain the modified chitosan.
3. The method of claim 1, wherein the concentration of the ethanol solution of 1, 5-pentanediamine in the fourth step is 2mol/L, and the volume fraction of the ethanol solution of glutaraldehyde is 10%.
4. The method for preparing the antibacterial non-woven fabric according to claim 1, wherein the mass ratio of the methacryloyloxyethyl trimethyl ammonium chloride to the acrylamide in the fifth step is 2: 1; the addition amounts of the allyl glycidyl ether and the initiator ammonium persulfate are respectively 5 percent and 2 percent of the total mass of the system.
5. The method for preparing the antibacterial non-woven fabric according to claim 1, wherein the dosage ratio of the benzophenone, the isopropanol and the hydroxyethyl methacrylate in the sixth step is 0.1:10: 4; the ratio of isopropanol/deionized water was 1: 4.
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