CN1467314A - Antibacterial nanofiber material and preparation method thereof - Google Patents
Antibacterial nanofiber material and preparation method thereof Download PDFInfo
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Abstract
本发明的抗菌纳米纤维材料包括高分子超细纤维、抗菌剂超细粒子，其中按重量百分比计算，高分子超细纤维占材料总重量的60％～98％，抗菌剂占材料总重量的2％～40％。抗菌纳米纤维材料由高分子与抗菌剂超细粒子混合物电纺制备。抗菌纳米纤维材料可以用于防护材料、杀菌过滤材料、组织修复、促进愈合的组织覆盖材料。制备方法为：将一种或多种高分子材料分散或溶于溶剂中成为透明溶液或混合物，粒度小于20微米的抗菌剂超细粒子分散在上述溶液中，得到电纺混合物，或者将一种或多种高分子与抗菌剂超细粒子熔融混合，得到电纺混合物；然后加入储罐中，通过注射泵和导管连接到一个或多个喷射头，得到含抗菌剂超细粒子的抗菌纳米纤维材料。The antibacterial nanofiber material of the present invention comprises macromolecular ultrafine fibers and antibacterial agent ultrafine particles, wherein calculated by weight percentage, macromolecular ultrafine fibers account for 60% to 98% of the total weight of the material, and the antibacterial agent accounts for 2% of the total weight of the material. %~40%. The antibacterial nanofiber material is prepared by electrospinning the mixture of macromolecule and antibacterial agent ultrafine particles. Antibacterial nanofiber materials can be used for protective materials, bactericidal filter materials, tissue repair, and tissue covering materials that promote healing. The preparation method is as follows: disperse or dissolve one or more polymer materials in a solvent to form a transparent solution or mixture, and disperse ultrafine particles of antibacterial agents with a particle size of less than 20 microns in the above solution to obtain an electrospinning mixture, or a or a variety of polymers and antibacterial ultrafine particles are melt-mixed to obtain an electrospun mixture; then added to a storage tank, connected to one or more injection heads through a syringe pump and a catheter, and antibacterial nanofibers containing antibacterial ultrafine particles are obtained Material.
Description
One, technical field:
The present invention is antibacterial nano fiber material and preparation method thereof, belongs to the technical field of antibiotic superfine fibre material preparation.
Two, background technology:
Protection, filtering material can adopt natural fabric or synthetic textiles, can also adopt nonwoven fabric, the cotton yarn mouth mask is the material that modal protection particle etc. enters respiratory tract, medical mask nonwoven fabric commonly used is made, the diameter of fiber is about 20 microns, aperture between the fiber is bigger, and is not so good to fine grain filter effect.
Vest is often made by nonwoven fabric, and the aperture between the same fiber is bigger.A kind of protective materials is to sandwich plastic film material etc. in the fabric, gives heat-preserving function.The vest dress of being made by the gas-impermeable plastics thin-film material makes people's discomfort.
In mouth mask, add the active carbon interlayer and can improve the short grained effect of obstruct, but relatively poor to intercepting aerocolloidal effect.
Another kind of protective materials is to add bactericidal additive etc. in the fabric, gives functions such as protective materials sterilization.
Another protective materials is to add counter infrared ray radiation agent and anti-ultraviolet radiation agent etc. in the fabric, gives the protective materials specific function.
Above-mentioned protective materials or employing general fibre material, fibre diameter is thicker.To intercepting superfine particle or aerocolloidal effect is relatively poor.
Also have and a kind ofly be used for protection sterilization that skin surface covers, promote that the material of healing is the thicker non-woven fabric compounded material of fibre diameter.
In the prior art, molten spin or anti-bacterial fibre diameter that the melt-spun method obtains thicker, usually more than 3 microns.Limited fibrous material filtering ultrafine particle and containing the fines of virus and the application aspect the aerosol, also limited this fibrous material at commodity such as clothes, and the application aspect medical science.
So, it is little to be necessary to develop a fiber material diameter, can effectively intercept superfine particle or aerocolloidal protection, filtering material, it is little to be necessary to develop a fiber material diameter, can the superfine particle of obstruct effectively antibacterial or sterilization or aerocolloidal protection, filtration, antibacterial, sterilization material.
Three, summary of the invention:
(1) goal of the invention
The purpose of this invention is to provide a kind of good permeability, good anti-bacterial effect, filter efficiency height, simple antibacterial nano fiber material of processing technology and preparation method thereof.
(2) technical scheme
Antibacterial nano fiber material of the present invention and preparation method thereof.This material comprises high molecular superfine fiber, antiseptic ultrafine particle, wherein counts by weight percentage, and high molecular superfine fiber accounts for 60%～98% of material gross weight, and antiseptic accounts for 2%～40% of material gross weight.Antiseptic is the inorganic ultrafine particle of argentiferous or zinc or copper ion, or the inorganic zeolite ultrafine particle of argentiferous or zinc or copper ion, or one or more the mixture in the zinc oxide, zinc sulfate, titanium dioxide, or chitin, shitosan ultrafine particle, its granularity is less than 20 microns.Antibacterial nano fiber material is by macromolecule and the preparation of antiseptic ultrafine particle mixture electrospinning.Because fiber is piled up regularly, the loose structure of formation rule, hole dimension is several microns.
High molecular superfine fiber is polyolefin, polyalkenyl halides, polysiloxanes, polyethers, polyamide, polyester, Merlon, polyurethane, epoxy resin, polyacrylonitrile, polyacrylic acid family macromolecule, polyphenylene oxide, poly-acid anhydrides, poly--a-amino acid, polyphenylene sulfide, or two or more blend wherein.Or a kind of or their derivative in the chitin, shitosan, hyaluronic acid, chondroitin sulfate, collagen, carrageenan, mosanom, calcium alginate, gelatin, agar, glucan, fibrin, silk-fibroin or two or more blend wherein.Fibre diameter is between 20 nanometers-3 micron.
Can also contain trace mineral supplement in the antibacterial nano fiber material and be in antistatic additive, organic bactericide, medicine, enzyme, polypeptide or protein, essence, the Chinese medicine extract one or more, wherein count by weight percentage, high molecular superfine fiber accounts for 60%～96% of material gross weight, antiseptic accounts for 2%～38% of material gross weight, and trace mineral supplement accounts for below 2% of material gross weight.
A kind of preparation method of antibacterial nano fiber material is: one or more macromolecules are disperseed or be dissolved in and become clear solution or mixture in the solvent, granularity is dispersed in the above-mentioned solution less than 20 microns antiseptic ultrafine particle, obtain the electrospinning mixture, perhaps with one or more macromolecules and antiseptic ultrafine particle melting mixing, obtain the electrospinning mixture, add in the storage tank then, be connected to one or more injector heads by syringe pump and conduit, injector head connects high voltage electric field, and voltage is 3 kilovolts-120 kilovolts.Accept partial earthing, carry out electrostatic spinning or EFI then, obtain containing the high molecular superfine fiber material of antiseptic ultrafine particle.What be connected with one or more injector heads can be single electrospinning mixture or multiple electrospinning mixture.The electric field that injector head connects is high pressure positive electric field or high pressure negative electric field or high-voltage alternating electric field.
(3) technique effect
(1) the present invention compared with prior art has following advantage:
(2) antibacterial nano fiber material provided by the invention is the composite of membranaceous or other shape that contains the high molecular superfine fiber of ultrafine particle, and fibre diameter is 20 nanometers-3000 nanometers.
(3) antibacterial nano fiber material provided by the invention has the simple feature of processing technology.Adopt macromolecule to mix electrospinning technology and obtain the superfine fibre composite with the antiseptic ultrafine particle, through after process, obtain various filtration, protection, antibacterial, sterilization, the promotion organization healing materials of being used for, can obtain good effect.
(4) antibacterial nano fiber protection filtering material provided by the invention superfine particle or aerosol are had efficient barrier property characteristics, and permeability is good.The nanofiber protective materials intercepts 0.3 micron aerocolloidal efficient and reaches more than 96%.
(5) antibacterial nano fiber material provided by the invention has good bactericidal action to bacteriums such as staphylococcus, Escherichia coli.
Four, the specific embodiment
Antibacterial nano fiber material of the present invention, this material comprise high molecular superfine fiber, antiseptic ultrafine particle, wherein count by weight percentage, and high molecular superfine fiber accounts for 60%～98% of material gross weight, and antiseptic accounts for 2%～40% of material gross weight.Antiseptic is the inorganic ultrafine particle of argentiferous or zinc or copper ion, or the inorganic zeolite ultrafine particle of argentiferous or zinc or copper ion, or chitin, shitosan ultrafine particle, or one or more the mixture in the zinc oxide, zinc sulfate, titanium dioxide, its granularity is less than 20 microns.Antibacterial nano fiber material is by macromolecule and the preparation of antiseptic ultrafine particle mixture electrospinning.Because fiber is piled up regularly, the loose structure of formation rule, hole dimension is several microns.
High molecular superfine fiber is polyolefin, polyalkenyl halides, polysiloxanes, polyethers, polyamide, polyester, Merlon, polyurethane, epoxy resin, polyacrylonitrile, polyacrylic acid family macromolecule, polyphenylene oxide, poly-acid anhydrides, poly--a-amino acid, polyphenylene sulfide, or two or more blend wherein.Or a kind of or their derivative in the chitin, shitosan, hyaluronic acid, chondroitin sulfate, collagen, carrageenan, mosanom, calcium alginate, gelatin, agar, glucan, fibrin, silk-fibroin or two or more blend wherein.Fibre diameter is between 20 nanometers-3 micron.
Can also contain trace mineral supplement in the antibacterial nano fiber material and be in antistatic additive, organic bactericide, medicine, enzyme, polypeptide or protein, essence, the Chinese medicine extract one or more, wherein count by weight percentage, high molecular superfine fiber accounts for 60%～96% of material gross weight, antiseptic accounts for 2%～38% of material gross weight, and trace mineral supplement accounts for below 2% of material gross weight.
The preparation method of antibacterial nano fiber material of the present invention is: one or more macromolecules are disperseed or be dissolved in and become clear solution or mixture in the solvent, granularity is dispersed in the above-mentioned solution less than 20 microns antiseptic ultrafine particle, obtain the electrospinning mixture, perhaps with one or more macromolecules and antiseptic ultrafine particle melting mixing, obtain the electrospinning mixture, add in the storage tank then, be connected to one or more injector heads by syringe pump and conduit, injector head connects high voltage electric field, and voltage is 3 kilovolts-120 kilovolts.Accept partial earthing, carry out electrostatic spinning or EFI then, obtain containing the high molecular superfine fiber material of antiseptic ultrafine particle.What be connected with one or more injector heads can be single electrospinning mixture or multiple electrospinning mixture.The electric field that injector head connects is high pressure positive electric field or high pressure negative electric field or high-voltage alternating electric field.
Antibacterial nano fiber material proposed by the invention can be used for the cladding material of protective materials, disinfection filtering material, tissue repair, promotion healing.Nanofiber protective materials proposed by the invention can be used for protective mask, vest, and the protection tent can also be used for filtering material such as air conditioner filter etc.
Embodiment 1
The preparation of antibacterial nano fiber material: macromolecule can be a polyolefin, polyethylene, polypropylene, polybutadiene, polyisoprene, polyester, polyethylene terephthalate, poly-to the dibenzoic acid butanediol ester, polybutylene terephthalate (PBT), Merlon, polyamide, nylon 6, nylon 66, nylon 1010, NYLON610, polyethers, polyoxyethylene, polyoxypropylene, poly-halogenated hydrocarbons, polystyrene, polymethylstyrene, polyacrylonitrile, polyvinyl acetate, polyvinyl alcohol, polyacrylic acid, polyacrylate, polymethylacrylic acid, polymethacrylates, polyimides, polyphenylene oxide, poly terephthalic acid p-phenylenediamine (PPD), poly-M-phthalic acid m-phenylene diamine (MPD).
For example, 2 gram nylon 6 are dissolved in the 20ml formic acid, be made into the Polymer Solution of 10% (mass fraction), the zeolite ultrafine particle that adds 0.4 gram argentiferous, particle size is about 100 nanometers, be uniformly dispersed, be connected to injector head by syringe pump and conduit, injector head connects the high pressure positive electric field, copper mesh ground connection, distance is controlled at about 6cm between injector head and copper mesh, solution flow rate 3ml/h, voltage are about 10kv, carry out electrospinning, obtain the nylon 6/nanometer tunica fibrosa that one deck contains the antiseptic ultrafine particle, obtain antibacterial nano fiber material.This material is 99% to the barriering efficiency of 300 nano particles.
Embodiment 2
The preparation of antibacterial nano fiber material: 5 gram polystyrene are dissolved in 50 milliliters of carrene, the zeolite ultrafine particle that adds 0.2 gram argentiferous, particle size is about 100 nanometers, is uniformly dispersed, and is connected to 6 injector heads by syringe pump and conduit, injector head connects high voltage electric field, distance is controlled at about 6cm between injector head and copper mesh reception thing, copper mesh ground connection, and voltage is about 10kv, carry out electrospinning, obtain the pipe/polyhenylethylene nano fibrous material.
Embodiment 3
The preparation of antibacterial nano fiber material: 5 gram polystyrene are dissolved in 50 milliliters of oxolanes, the zeolite ultrafine particle that adds 1 gram argentiferous, particle size is about 100 nanometers, is uniformly dispersed, and is connected to 6 injector heads by syringe pump and conduit, injector head connects high voltage electric field, distance is controlled at about 6cm between injector head and copper mesh reception thing, copper mesh ground connection, and voltage is about 10kv, carry out electrospinning, obtain the pipe/polyhenylethylene nano tunica fibrosa.5 gram nylon 6 are dissolved in the 50ml formic acid, be made into the Polymer Solution of 10% (mass fraction), be connected to 6 injector heads by syringe pump and conduit, injector head connects high voltage electric field, receiving thing is above-mentioned pipe/polyhenylethylene nano fiber, and solution flow rate 3ml/h, voltage are about 10kv, carry out electrospinning, obtain double-deck antibacterial nano fiber film.
Embodiment 4
The preparation of antibacterial nano fiber material: with 0.5 grammes per square metre average molecular weight is that the polyoxyethylene of 130,000 poly (l-lactic acid)s and 0.5 gram-molecular weight 100,000 is dissolved in the 10ml dimethyl formamide, be made into the Polymer Solution of 10% (mass fraction), add 0.04 gram zinc oxide ultra-fine particle, particle size is about 100 nanometers, be uniformly dispersed, mixture joins in the storage tank, and be connected to injector head with conduit, injector head connects high voltage electric field, injector head and copper mesh receive between thing apart from being controlled at about 5cm copper mesh ground connection, solution flow rate 6ml/h, voltage is about 10kv, carries out electrospinning.Obtain poly (l-lactic acid) and polyoxyethylene blend antibacterial nano fiber material.
Embodiment 5
The preparation of antibacterial nano fiber material: 100 gram polyoxyethylene heating and meltings become melt, add 5 gram zinc oxide ultra-fine particles, particle size is about 100 nanometers, is uniformly dispersed, be connected to injector head by syringe pump and conduit, injector head connects high voltage electric field, and receiving thing is the polyester fiber net, and fibroreticulate below is a copper mesh, copper mesh ground connection, distance is controlled at about 10cm between injector head and reception thing, and voltage is about 15kv, carries out electrospinning.Obtain the polyoxyethylene antibacterial nano fiber material.
Embodiment 6
The preparation of antibacterial nano fiber material: 100 gram polyoxyethylene heating and meltings become melt, add 10 gram titanium dioxide ultrafine particles, particle size is about 100 nanometers, is uniformly dispersed, be connected to injector head by syringe pump and conduit, injector head connects high voltage electric field, and receiving thing is the polyester fiber net, and fibroreticulate below is a copper mesh, copper mesh ground connection, distance is controlled at about 10cm between injector head and reception thing, and voltage is about 15kv, carries out electrospinning.Obtain the polyoxyethylene antibacterial nano fiber material.
Embodiment 7
The preparation of antibacterial nano fiber material: with 0.5 grammes per square metre average molecular weight is that the polyoxyethylene of 130,000 poly (l-lactic acid)s and 0.5 gram-molecular weight 100,000 is dissolved in the 10ml dimethyl formamide, be made into the Polymer Solution of 10% (mass fraction), add 0.3 gram chitin ultrafine particle, particle size is about 5 microns, be uniformly dispersed, mixture joins in the storage tank, and being connected to injector head with conduit, injector head connects high voltage electric field, injector head and receive that distance is controlled at about 5cm between thing, receiving thing is the nylon fiber net, fibroreticulate below is a copper mesh, copper mesh ground connection, solution flow rate 6ml/h, voltage is about 10kv, carries out electrospinning.Obtain poly (l-lactic acid) and polyoxyethylene blend antibacterial nano fiber material.
Embodiment 8
The preparation of antibacterial nano fiber material: 2 gram nylon 6 are dissolved in the mixed solvent, be made into the Polymer Solution of 10% (mass fraction), the zeolite ultrafine particle and the 0.1 gram zinc sulfate ultrafine particle that add 0.3 gram argentiferous, particle size is about 100 nanometers, be uniformly dispersed, be connected to injector head by syringe pump and conduit, injector head connects the high pressure positive electric field, and receiving thing is the polyester fiber net, and fibroreticulate below is a copper mesh, copper mesh ground connection, distance is controlled at about 8cm between injector head and reception thing, and solution flow rate 3ml/h, voltage are about 10kv, carry out electrospinning, obtain containing nylon 6 antibacterial nano fiber materials of antiseptic ultrafine particle.
Embodiment 9
The preparation of antibacterial nano fiber material: 2 gram nylon 6 are dissolved in the 20ml formic acid, be made into the Polymer Solution of 10% (mass fraction), the zeolite ultrafine particle that adds 0.4 gram cupric, particle size is about 100 nanometers, be uniformly dispersed, be connected to injector head by syringe pump and conduit, injector head connects the high pressure positive electric field, and receiving thing is the polyester fiber net, and fibroreticulate below is a copper mesh, copper mesh ground connection, distance is controlled at about 6cm between injector head and reception thing, and solution flow rate 3ml/h, voltage are about 10kv, carry out electrospinning, obtain containing nylon 6 antibacterial nano fiber materials of antiseptic ultrafine particle.
Embodiment 10
The preparation of antibacterial nano fiber material: 2 grammes per square metre average molecular weights are about 130,000 poly (l-lactic acid) and are dissolved in the 10ml acetone, be made into the Polymer Solution of 20% (mass fraction), the zeolite ultrafine particle that adds 0.7 gram argentiferous, particle size is about 100 nanometers, be uniformly dispersed, stirred 24 hours, and added then in the storage tank 1.Again 1.5 grammes per square metre average molecular weights are about 130,000 poly (l-lactic acid) and are dissolved in the 10ml dimethyl formamide, be made into the Polymer Solution of 15% (mass fraction), stirred 24 hours, add then in the storage tank 2.Storage tank 1 is connected to injector head by syringe pump and conduit, injector head connects high voltage electric field, receiving thing is nylon cloth, the nylon cloth below is a copper mesh, copper mesh ground connection, and distance is controlled at about 5cm between injector head and reception thing, solution flow rate 6ml/h, voltage is 10 kilovolts, carries out electrospinning, obtains micro/nano fibrous membrane material.Storage tank 2 is connected to another injector head by syringe pump and conduit, injector head connects high voltage electric field, receiving thing is top micro/nano fibrous membrane material, distance is controlled at about 5cm between injector head and reception thing, solution flow rate 1ml/h, voltage is 10 kilovolts, carries out electrospinning, obtains the double-layer nanometer fiber film material.
Embodiment 11
The preparation of antibacterial nano fiber material: 1 grammes per square metre average molecular weight is about 130,000 poly (l-lactic acid) and is dissolved in the 10ml acetone, be made into the Polymer Solution of 20% (mass fraction), add 0.2 and restrain the zeolite ultrafine particle that contains silver ion, particle size is about 100 nanometers, be uniformly dispersed, add the lysozyme aqueous solution that contains 0.02 gram, stirred 24 hours, add in the storage tank then.Storage tank is connected to injector head by syringe pump and conduit, injector head connects high voltage electric field, receiving thing is nylon cloth, the nylon cloth below is a copper mesh, copper mesh ground connection, and distance is controlled at about 5cm between injector head and reception thing, solution flow rate 6ml/h, voltage is 10 kilovolts, carries out electrospinning, obtains the antibacterial nano fiber membrane material.
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2003
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