CN109680495A - A kind of preparation method and antibacterial fabric of nano particle antibacterial fabric - Google Patents
A kind of preparation method and antibacterial fabric of nano particle antibacterial fabric Download PDFInfo
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- CN109680495A CN109680495A CN201811615478.XA CN201811615478A CN109680495A CN 109680495 A CN109680495 A CN 109680495A CN 201811615478 A CN201811615478 A CN 201811615478A CN 109680495 A CN109680495 A CN 109680495A
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/402—Amides imides, sulfamic acids
- D06M13/432—Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
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- 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
- D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic System; Zincates; Cadmates
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- 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
- D06M14/28—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 by reactions only involving carbon-to-carbon unsaturated bonds
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- 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
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Abstract
The present invention relates to a kind of preparation method of nano particle antibacterial fabric, the step of preparation method is that the organic monomer containing epoxy group and thiocarbamide S1, are grafted to textile substrate surface by graft copolymerization；S2, amino is introduced by carrying out surface chemical modification to nano granular of zinc oxide；S3, the textile substrate surface with epoxy group will be coated in through amido modified nano granular of zinc oxide, epoxy group and amino carry out opening, so that nano granular of zinc oxide is secured firmly to textile substrate surface, nano particle antibacterial fabric is obtained.Overcome adhesive and by adsorbing the shortcomings that fixing nanoparticle, utilize the method for radiation grafting and ring-opening polymerisation, nano particle is fixed on the textile with covalent bond, to maintain the lasting anti-microbial property of textile while improve wash durability, any pre-treatment is not needed, radiation grafting process nanoparticle and organic monomer dosage are few, maintain the original performance of fiber.
Description
Technical field
The present invention relates to the antimicrobial treatment technical fields of textile, more particularly, to a kind of nano particle antibacterial fabric
Preparation method and antibacterial fabric.
Background technique
Textile is one of key components of human lives along with the various fields of human lives, therefore the mankind
All kinds of pathogen and bacterium and microorganism in life all can be by textiles, this direct human contact's body passes
It broadcasts.All kinds of bacteriums and pathogen are done harm to huamn body by textile propagation in order to prevent, and the people of countries in the world take
A series of measure improves the system of public health health and disease prevention.Wherein by preventing bacterium on the textile of source
Propagation be one of crucial effective method.The method that building can prevent bacterium and pathogen from propagating on the textile is mainly wrapped
The modification to textile is included, because original textile does not have the function of preventing bacterium and pathogen from propagating, and pathogenic bacteria
It can grow and breed on textile fiber, to accelerate the diffusion and propagation of disease.
Integration of the building antibacterial system mainly to textile progress antibacterial agent on the textile at present, such as containing anti-
The organic molecule and nano metal particles (nano silver) and metal salt (mantoquita, silver salt etc.) of bacterium functional group are integrated on textile
Antibacterial is carried out, since metallic and salt have the function of excellent destruction cell membrane, so as to cause the dead of bacterium and pathogen
It dies, achievees the purpose that antibacterial.But what traditional combination method mainly utilized is physical absorption and the effect of chemisorption by function
Energy molecule and group are adsorbed on textile, will lead to the durability deterioration of antibacterial fabric in this way, rear antibiotic property is used for multiple times
It can be remarkably decreased, and antibacterial integration needs pre-treatment, for example need specific to the modified raising in fiber textile progress surface
Performance to it is convenient or be conducive to it is subsequent integrate antibacterial agent, pre-treatments many in this way certainly will will affect the performance of fiber itself
Such as mechanical performance and durability.And part antibacterial group selectivity is poor, have certain cytotoxicity, to human body with
The skin of human contact will cause the physiological reactions such as repulsion or even threaten human health.Therefore antibacterial body of the building to human security
It is textile, and realizes that the durable wear-resistant of antibacterial fabric realizes there is the retainable antibacterial weaving of efficient primitiveness simultaneously
Product are vital.
Currently, nanoscale zinc oxide particles are with excellent anti-microbial property by increasingly in nanoparticle antibacterial agent
More concerns.It is strong to pathogenic bacterias such as Escherichia coli, detection of Salmonella to kill and inhibiting effect shows nano-class antibacterial
The superperformance of agent.For example show direct phase interaction between zinc oxide nano-particle and bacterial cell membrane by electrochemical research
It is dead so as to cause Escherichia coli with the rupture that will lead to Bacillus coli cells film.The main quilt of nanoscale zinc particles at present
It is added in the spinning solution of printing and dyeing solution or chemical fibre, textile surface is attached to by physical and chemical adsorption effect, or
Person is fixed using certain adhesive.But these methods can all influence the performance of fiber, and lead to nanoparticle
Anti-microbial property can be remarkably decreased after washing.
Therefore exploitation the superior Nano-class zinc oxide antibacterial fabric of performance, realize high-efficiency antimicrobial selectively, technique mistake
Journey prepares simple and effective, water-fastness nano oxidized property antibiotic fabric to the application study of antibiotic fabric with extremely important
Value and significance.
Summary of the invention
Technical problem to be solved by the invention is to provide the preparation methods and antibacterial of a kind of nano particle antibacterial fabric
Textile overcomes technique and antibiotic fabric wash resistant effect complicated in the preparation method of existing nano oxidized property antibiotic fabric
The disadvantage of difference.
The technical scheme adopted by the invention to solve the technical problem is that: a kind of preparation side of nano particle antibacterial fabric
The step of method, the preparation method is,
S1, the organic monomer containing epoxy group and thiocarbamide are grafted to textile substrate table by graft copolymerization
Face, it is spare；
S2, amino is introduced by carrying out surface chemical modification to nano granular of zinc oxide, it is spare；
S3, it is obtained what step S2 was obtained coated in step S1 with epoxy group through amido modified nano granular of zinc oxide
The textile substrate surface of group, epoxy group and amino carry out opening, so that nano granular of zinc oxide securely fixes
On textile substrate surface, nano particle antibacterial fabric is obtained.
Further specifically, the textile substrate is by natural fiber and synthesizes one of macromolecular fibre or two
Kind mixing is weaved.
Further specifically, the natural fiber includes one of plant cotton fiber, flaxen fiber, wool fibre or a variety of
Mixing；The synthesis macromolecular fibre includes polyether-ketone, polyvinyl chloride, polystyrene, polyethylene, polypropylene, polyvinylidene fluoride
One of alkene, nylon, terylene, polycarbonate, polyester terephthalate, poly terephthalic acid propyl ester, polyamide are a variety of mixed
It closes.
Further specifically, the polymerization methods of the graft polymerization reaction are bulk polymerization, suspend and gather in step sl
One of conjunction, polymerisation in solution and emulsion polymerization.
Further specifically, in step sl the graft polymerization reaction by chemical initiator, ultraviolet light, radiation, etc.
One of gas ions are caused.
Further specifically, the chemical structure of the organic monomer containing epoxy group is monomer point in step sl
Contain epoxy group and carbon-carbon double bond in son simultaneously.
Further specifically, the organic monomer containing epoxy group includes glycidyl in step sl
One of ester (GAA), glycidyl methacrylate (GMA), 4- hydroxyl butyl propyleneglycol acid glycidyl ester (4-HB) are more
Kind mixing.
Further specifically, in step s 2 the surface chemical modification be using the silane coupling agent containing amino and
The hydroxyl of surface of nanometer zinc oxide is reacted, so that amino is introduced into surface of nanometer zinc oxide.
Further specifically, the pH value of the opening is controlled 7~14 in step s3.
Further specifically, in step s3 through amido modified nano granular of zinc oxide in the opening
It controls with the weight ratio of the textile substrate with epoxy group 0.05%~10%.
It is a kind of to use antibacterial fabric made from above-mentioned preparation method.
It is had the advantage that during preparing nano particle antibacterial fabric using the above method
1, other organic chemical reagents during the preparation process, are not needed, and textile does not need any pre-treatment, pole
The earth reduces costs.
2, other complicated consersion units and instrument during the preparation process, are not needed, it is only necessary to the instrument of this field routine
Equipment, and treatment process is simple and easy, simplifies the preparation method and process of traditional antibiotic fabric, needed for significantly reducing
The cost wanted, to realize that industrial applications are provided convenience.
3, the antibacterial fabric of this method preparation has the advantages that wide spectrum inhibits and kills bacterium, and due to nano particle
It is securely fixed on textile fiber by covalent bond, can prevent nano particle from falling in environment, so antibacterial is spun
The wash resistant effect of fabric is very good.
4, during the preparation process, the dosage of required nano particle and organic monomer is considerably less, and utilization efficiency is non-
Chang Gao, for the nano particle and organic monomer of loss less than 5 percent, the advantages of innovation, is nanometer used in the present invention
The partial size of grain has excellent inhibition and killing effect less than 50 nanometers, to salmonella.
5, after introducing thiocarbamide in connecing branch copolyreaction, thiocarbamide meeting and epoxy group occur " to gather in brilliant road in textile surface
Close ", to make epoxy group efficiently, in an orderly manner polymerize in textile surface, and brilliant road polymerization reaction can improve significantly
Steric hindrance when amino is reacted with epoxy group, to obtain the textile of a kind of strong broad-spectrum antiseptic, durable antibiotic endurance.
6, it overcomes current adhesive and by adsorbing the shortcomings that fixing nanoparticle, utilizes radiation grafting and ring-opening polymerisation
Method, nano particle is fixed on the textile with covalent bond, to maintain the lasting anti-microbial property of textile while mention
High wash durability.And operation is simple for method provided by the invention, and fiber does not need any pre-treatment, radiation grafting
Process nanoparticle and monomer dosage are few, this greatly maintains the original performance of fiber.
Specific embodiment
The present invention is further illustrated below, but therefore do not limit the present invention to the explanation and scope of embodiments it
It is interior.
A kind of the step of preparation method of nano particle antibacterial fabric, the preparation method is,
S1, the organic monomer containing epoxy group and thiocarbamide are grafted to textile substrate table by graft copolymerization
Face, it is spare；Textile substrate can be woven cloths either non-woven cloth in this step；Wherein textile substrate can be day
Right fiber either synthesizes macromolecular fibre and weaves, be also possible to natural fiber and synthesis macromolecular fibre mixing weaving and
At；Implement preferably have plant cotton fiber, flaxen fiber and wool fibre in the selection of natural fiber, wherein using a kind of or more
Kind mixing；Implement preferably have polyether-ketone, polyvinyl chloride, polystyrene, poly- second in the selection of synthesis macromolecular fibre
Alkene, polypropylene, Kynoar, nylon, terylene, polycarbonate, polyester terephthalate, poly terephthalic acid propyl ester and polyamides
Amine, wherein using one or more kinds of mixing；And it can be caused using chemical initiator in connecing branch copolyreaction, is ultraviolet
Light-initiated, radiation causes, plasma causes, and polymerization methods are mainly bulk polymerization, suspension polymerisation, polymerisation in solution or lotion
Polymerization；Wherein, the chemical structure characteristic of the organic monomer containing epoxy group be in monomer molecule simultaneously containing epoxy group and
Carbon-carbon double bond, this organic monomer include glycidyl acrylate (GAA), glycidyl methacrylate (GMA), 4- hydroxyl
One of butyl propyleneglycol acid glycidyl ester (4-HB) or a variety of mixing；Thiocarbamide is dissolved in together with organic monomer when in use
In water, the concentration for controlling thiocarbamide is 2g/L；In graft copolymerization, the organic monomer containing epoxy group is on textile substrate
Grafting rate be 0.1~200%, preferably 2~50%.
S2, amino is introduced by carrying out surface chemical modification to nano granular of zinc oxide, it is spare；It is used nano oxidized
The partial size of zinc particle is 1~900 nanometer, wherein optimal partial size is 20~200 nanometers；In this step, using containing amino
Silane coupling agent reacted with the hydroxyl of surface of nanometer zinc oxide, time of reaction controls at 5 minutes~24 hours, most preferably
Reaction time is 0.5~6 hour, so that amino is introduced to surface of nanometer zinc oxide, the silane coupling agent containing amino includes
3- aminopropyl trimethoxysilane (A-1110), gamma-aminopropyl-triethoxy-silane (KH550, WD-50), N- (β-aminoethyl)-
One of gamma-aminopropyl-triethoxy-silane (WD-52), γ-aminopropyltriethoxy diethoxy silane (WD-57) is a variety of mixed
It closes.
S3, it is obtained what step S2 was obtained coated in step S1 with epoxy group through amido modified nano granular of zinc oxide
The textile substrate surface of group, epoxy group and amino carry out opening, so that nano granular of zinc oxide securely fixes
On textile substrate surface, nano particle antibacterial fabric is obtained；The temperature of opening is controlled at 18 DEG C~100 DEG C,
Optimal reaction temperature is 45 DEG C~70 DEG C, and at 1 minute~12 hours, the optimal reaction time was 0.5~6 small for reaction time control
When, 7~14, best pH value is 9~12 for the pH value control of reaction environment；Through amido modified nano oxygen in opening
Change weight ratio control of the zinc particle with the textile substrate with epoxy group 0.05%~10%, optimum weight ratio is
0.1%~3%.
In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions, or says according to commodity
Bright book selection；Raw material used in embodiment, drug are commercially available.
Embodiment 1: scribbled fabric (cotton/wash=99/1) radiates solution graft copolymerization altogether and prepares antibacterial textile
By scribbled fabric (weight average molecular weight 550,000) infiltration into the aqueous solution containing grafting organic monomer and thiocarbamide,
Ultrasound 10 minutes.Wherein organic monomer is glycidyl acrylate, and organic monomer dosage is 10g/L aqueous solution, thiocarbamide dosage
For 2g/L, it is passed through nitrogen in the mixture and is bubbled the 15 minutes oxygen removed in reaction system, cobalt -60 is sent into after sealing and is irradiated
Room irradiates 17 hours, and dosage rate 2kGy/h takes out sample after irradiation, is rinsed 5~10 times with deionized water, and drying is
Obtain the textile substrate with epoxy group；0.5g Zinc oxide nanoparticle is weighed, is dispersed in 100mL acetone, 2mL silicon is added
Alkane coupling agent WD50, centrifugation drying is after being stirred at room temperature 4 hours to get through amido modified nano granular of zinc oxide；Weigh 0.2g
It through amido modified nano granular of zinc oxide, is dispersed in the aqueous solution of 5ml, coated in the textile substrate for having epoxy group
On, after heating 2 hours.
The load capacity of textile substrate nano surface particle is measured with weight method as 13.5%.
Embodiment 2: polyurethane fiber (weight average molecular weight 700,000) plasma causes glycidyl methacrylate and connects
Branch prepares antibacterial textile
It prepares containing organic monomer methacrylic acid ethylene oxidic ester, methanol is grafted, wherein the concentration of organic monomer is
15g/L, thiocarbamide dosage are 2g/L, and the dosage of methanol is 20% (v/v), the air in ultrasonic 15 minutes removal systems, stand to
With.
Polyurethane fiber is subjected to surface activation process with low temperature plasma equipment in air atmosphere, is activated 20
Minute, it then takes out and is put into the above-mentioned solution prepared, be passed through nitrogen 20 minutes, be then sealed processing, and heat
To 50~70 DEG C, initiated polymerization the reaction time 5 hours, is after reaction taken out polyurethane fiber, clear with deionized water
It washes 5-10 times, places into Soxhlet extractor and extracted 24 hours with water, the textile substrate obtained by drying with epoxy group；Claim
0.5g nano granular of zinc oxide is taken, is dispersed in 100mL acetone, 2mL silane coupling agent WD50 is added, after being stirred at room temperature 4 hours
Centrifugation drying is to get through amido modified nano granular of zinc oxide；0.2g is weighed through amido modified nano granular of zinc oxide, is divided
Be dispersed in the aqueous solution of 5ml, coated in epoxy group textile substrate on, heating 2 hours after.
The load capacity of textile substrate nano surface particle is measured with weight method as 18.2%.
Embodiment 3: nylon-6 radiates solution graft copolymerization altogether and prepares antibacterial textile
By nylon-6 (weight average molecular weight 1,000,000) infiltration to the aqueous solution for containing grafting organic monomer, thiocarbamide, ethylenediamine
In.The preparation method is the same as that of Example 1 for the mixture, and by mixture ultrasound 10 minutes, wherein organic monomer was methacrylic acid contracting
Water glyceride, organic monomer dosage are 18g/L aqueous solution, and thiocarbamide dosage is 2g/L, and the concentration of ethylenediamine is 1% (v/v)；Mixed
It closes and is passed through the oxygen that nitrogen is bubbled in 30 minutes removing reaction systems in object, -60 radiation chamber of cobalt is sent into after sealing, irradiation 17 is small
When, dosage rate 1.5kGy/h takes out sample after irradiation, is rinsed 5~10 times, is drying to obtain with epoxy with deionized water
The textile substrate of group；0.5g nano granular of zinc oxide is weighed, is dispersed in 100mL acetone, 2mL silane coupling A-is added
1110, centrifugation drying is after being stirred at room temperature 4 hours to get through amido modified nano granular of zinc oxide；0.1g is weighed to repair through amino
The Zinc oxide nanoparticle of decorations, is dispersed in the aqueous solution of 4ml, coated on the textile substrate with epoxy group, heats 2
After hour.
The load capacity of textile substrate nano surface particle is measured with weight method as 25%.
Embodiment 4: the ultraviolet light-initiated solution graft copolymerization of polyethylene fibre prepares antibacterial textile
The sundries on polyethylene fibre (weight average molecular weight 600,000) surface is cleaned up, by 10% 4- hydroxyl butylacrylic acid
Ethylene oxidic ester and 1% mixed aqueous solution of thiocarbamide apply and are rolled in the surface of polyethylene fibre, and polyethylene fibre is placed in poly- second
Sealing is vacuumized in alkene sack, the initiation grafting polymerization reaction in the case where the ultraviolet lamp of 256nm shines is unlocked sealing sack and stopped after 30 minutes
It only reacts, polyethylene fibre taking-up is cleaned 5-10 times with deionized water, is drying to obtain the textile substrate with epoxy group；
0.5g nano granular of zinc oxide is weighed, is dispersed in 100mL acetone, 2mL silane coupling agent WD52 is added, is stirred at room temperature 4 hours
Centrifugation drying is afterwards to get through amido modified nano granular of zinc oxide；0.1g is weighed through amido modified nano granular of zinc oxide,
Be dispersed in the aqueous solution of 4ml, coated in epoxy group textile substrate on, heating 2 hours after.
The load capacity of textile substrate nano surface particle is measured with weight method as 12%.
Embodiment 5: polyethanol terephthalate (weight average molecular weight 800,000) radiates solution graft copolymerization preparation antibacterial weaving altogether
Object
By polyethanol terephthalate infiltration to containing grafting organic monomer and thiocarbamide, methanol aqueous solution in.This is mixed
Closing object, the preparation method is the same as that of Example 1, and by mixture ultrasound 20 minutes, wherein organic monomer was methyl propenoic acid glycidyl
Ester, organic monomer dosage are 20g/L aqueous solution, and the concentration of methanol is 20% (v/v), are passed through nitrogen in the mixture and are bubbled 30 points
Clock removes the oxygen in reaction system, and -60 radiation chamber of cobalt is sent into after sealing, irradiates 17 hours, dosage rate 2kGy/h, irradiation knot
Sample is taken out after beam, is rinsed 5~10 times with deionized water, is drying to obtain the textile substrate with epoxy group；Weigh 0.5g
Nano granular of zinc oxide is dispersed in 100mL acetone, and 2mL silane coupling agent WD50 is added, and is centrifuged and is dried after being stirred at room temperature 4 hours
It does to get through amido modified nano granular of zinc oxide；0.15g is weighed through amido modified nano granular of zinc oxide, is dispersed in
In the aqueous solution of 4ml, coated in epoxy group textile substrate on, heating 2 hours after.
The load capacity of textile substrate nano surface particle is measured with weight method as 22%.
Embodiment 6: cotton fiber (100% cotton) electron beam irradiation causes solution graft copolymerization and prepares antibacterial textile
By the infiltration of cotton fiber into the aqueous solution containing the organic monomer and thiocarbamide, propyl alcohol that are grafted.The system of the mixture
Preparation Method is with embodiment 1, and by mixture ultrasound 20 minutes, wherein organic monomer was 4- hydroxyl butyl propyleneglycol acid glycidyl ester, is had
Machine monomer dosage is 12g/L aqueous solution, and the concentration of propyl alcohol is 15% (v/v), and the cotton fiber infiltrated is taken out, poly- second is put into
Sealing is vacuumized in alkene sack, is put into radiation-initiated polymerization in electron-beam accelerator and is reacted, irradiates 4 hours, total absorbed dose is
20kGy takes out sample after irradiation, is rinsed 5~10 times with deionized water, is drying to obtain the textile base with epoxy group
Material；0.5g Zinc oxide nanoparticle is weighed, is dispersed in 100mL acetone, 2mL silane coupling agent WD57 is added, it is small to be stirred at room temperature 4
When after centrifugation drying to get through amido modified nano granular of zinc oxide；0.17g is weighed through amido modified nano zine oxide
Grain, be dispersed in the aqueous solution of 4ml, coated in epoxy group textile substrate on, heating 2 hours after.
The load capacity of textile substrate nano surface particle is measured with weight method as 8.8%.
Embodiment 7: natural silk fabrics electron beam irradiation solution graft copolymerization prepares antibacterial textile
By the infiltration of natural silk fabrics into the aqueous solution containing the organic monomer and thiocarbamide, ethylenediamine that are grafted.The mixture
The preparation method is the same as that of Example 1, and by mixture ultrasound 20 minutes, wherein organic monomer was 4- hydroxyl butyl propyleneglycol acid glycidyl
Ester, organic monomer dosage are 18g/L aqueous solution, and the concentration of ethylenediamine is 4% (v/v)；The cotton fiber infiltrated is taken out, is put
Enter and vacuumize sealing in polyethylene bags, is put into radiation-initiated polymerization in electron-beam accelerator and reacts, irradiate 4 hours, it is total to absorb
Dosage is 100kGy, takes out sample after irradiation, is rinsed 5~10 times, is drying to obtain with epoxy group with deionized water
Textile substrate；0.5g nano granular of zinc oxide is weighed, is dispersed in 100mL acetone, 2mL silane coupling agent WD52, room is added
Centrifugation drying is after temperature stirring 4 hours to get through amido modified nano granular of zinc oxide；0.09g is weighed through amido modified oxygen
Change zinc nanoparticles, be dispersed in the aqueous solution of 5ml, coated in epoxy group textile substrate on, heating 2 hours after
?.
The load capacity of textile substrate nano surface particle is measured with weight method as 9.8%.
Embodiment 8: polyethylene polypropylene blend fibre (PE/PP) pre-irradiated solution graft copolymerization prepares antibacterial textile
A certain amount of PE/PP fiber is put into irradiation tube, it is small that -60 radioactive source radiation 24 of cobalt is put under air conditions
When, irradiation dose 45kGy is spare as storing in ice cube after irradiation.
It takes water as a solvent, prepares the mixed solution containing glycidyl acrylate and thiocarbamide, ethyl alcohol, wherein organic monomer is dense
Degree is 15g/L, and thiourea concentration 2g/L, the concentration of ethyl alcohol is 20% (v/v), by mixed solution ultrasound as being uniformly mixed, then
By above-mentioned PE/PP fiber as in mixed solution, being passed through nitrogen 30 minutes, then heated sealed is to about 60 DEG C of initiated polymerizations,
Reaction 5 hours is passed through oxygen and stops reaction, takes out fiber and is rinsed 5~10 times with deionized water, is drying to obtain with epoxy group
Textile substrate；0.5g Zinc oxide nanoparticle is weighed, is dispersed in 100mL acetone, 2mL silane coupling agent WD50 is added,
Centrifugation drying is after being stirred at room temperature 4 hours to get through amido modified nano granular of zinc oxide；0.12g is weighed through amido modified
Nano granular of zinc oxide is dispersed in the aqueous solution of 5ml, coated on the textile substrate with epoxy group, is heated 2 hours
Afterwards.
The load capacity of textile substrate nano surface particle is measured with weight method as 14.8%.
Antibacterial textile is prepared using common mode and the preparation method without thiocarbamide below, is comparative example.
Comparative example 1: polyethylene polypropylene fiber (PE/PP) fabric radiation solution prepares antibacterial textile
Polyethylene polypropylene fiber is immersed in the thiourea solution containing nano granular of zinc oxide and methanol, it is nano oxidized
Zinc granule density is 20g/L, and methanol concentration is 10% (v/v), thiourea concentration 2g/L, is led to nitrogen 15 minutes, cobalt is sent into sealing
Source irradiates 17 hours, and dosage rate 1.5kGy takes out sample after irradiation, is rinsed 5~10 times with deionized water, and drying is
?.
The load capacity of textile substrate nano surface particle is measured with weight method as 15.8%.
Comparative example 2: polyurethane loomage radiation solution graft copolymerization prepares antibacterial textile
Polyurethane loomage is cut into it is appropriately sized, be immersed in containing methanol and grafting organic monomer solution in, methanol
Concentration is (10%), and wherein organic monomer is glycidyl acrylate, and organic monomer dosage is 5g/L aqueous solution, leads to nitrogen 15
Minute, sealing is sent into cobalt source and is irradiated 17 hours, and dosage rate 1.5kGy takes out sample after irradiation, rinses 5 with deionized water
~10 times, the textile substrate that is dried to obtain that treated；0.5g nano granular of zinc oxide is weighed, is dispersed in 100mL acetone, adds
Enter 2mL silane coupling agent WD50, centrifugation drying is after being stirred at room temperature 4 hours to get through amido modified nano granular of zinc oxide；Claim
It takes 0.12g through amido modified nano granular of zinc oxide, is dispersed in the aqueous solution of 5ml, be coated in treated textile base
On material, after heating 2 hours.
The load capacity of textile substrate nano surface particle is measured with weight method as 4.3%.
In order to test the anti-microbial property of antibiotic fabric, GB/T 21510-2008 is to embodiment 1-8 and right according to national standards
Ratio 1-2 tests staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa, candida albicans and salmonella inhibition and killing effect,
As shown in the table.
As seen from the above table, antibacterial textile of the invention is more than after 12% in nano surface particulate load amount, and antibacterial is spun
The anti-microbial property of fabric has obtained significant raising, antibiotic fabric of the load capacity less than 10% of nano particle, anti-microbial property
It is insufficient.In addition, all samples for having loaded nano particle are equal to salmonella in antibacterial textile prepared by the present invention
Show outstanding inhibition and killing effect, though the load capacity of nano particle when less than 10%, still to salmonella
Outstanding inhibition and killing effect are shown, this is because nano granular of zinc oxide partial size used in the embodiment of the present invention
At 30 nanometers hereinafter, being less than the most of nano particle of tradition.In addition, can be seen that from comparative example 2 in no introducing thiocarbamide,
The load capacity of nano particle is remarkably decreased, and reflects that introducing thiocarbamide promotes nano particle in the grafting rate of textile surface,
To enhance the broad-spectrum antimicrobial effect of textile, this illustrates that thiocarbamide polymerize with organic monomer in the brilliant road that textile surface occurs
It plays an important role to the antibacterial effect of textile.
The anti-microbial property after embodiment 1-8 and comparative example 1-2 washing is tested simultaneously, according to ATCC61-2006,
The acceleration wash conditions of 2A, accelerate 30 circulations (primary accelerate wash cycle be equivalent to 5 household washings) of washing, then with above-mentioned
Method tests antibacterial effect, as a result as shown in the table.
The anti-microbial property of antibiotic fabric does not change substantially it can be seen from 2 embodiment 1-8 of table, this is because nanometer
Grain is fixed on fiber surface by the covalent bond that monomer polymerization is formed when ring-opening reaction, so washing by 150 households
Afterwards, fiber still has very strong anti-microbial property, this illustrates the excellent durability of antibiotic fabric prepared by the present invention.Simultaneously from right
Ratio 1 and 2 is passed through as can be seen that when the covalent bond that nano particle does not have coverlet body to be formed is securely fixed in fiber surface
After household washing, anti-microbial property a sharp decline of fiber.
It is emphasized that: the above is only presently preferred embodiments of the present invention, not make in any form to the present invention
Limitation, any simple modification, equivalent change and modification to the above embodiments according to the technical essence of the invention,
All of which are still within the scope of the technical scheme of the invention.
Claims (11)
1. a kind of preparation method of nano particle antibacterial fabric, which is characterized in that the step of preparation method is,
S1, the organic monomer containing epoxy group and thiocarbamide are grafted to textile substrate surface by graft copolymerization, it is standby
With；
S2, amino is introduced by carrying out surface chemical modification to nano granular of zinc oxide, it is spare；
S3, it is obtained what step S2 was obtained coated in step S1 with epoxy group through amido modified nano granular of zinc oxide
Textile substrate surface, epoxy group and amino carry out opening, so that nano granular of zinc oxide is secured firmly to spin
Fabric substrate surface obtains nano particle antibacterial fabric.
2. the preparation method of nano particle antibacterial fabric according to claim 1, which is characterized in that the textile
Substrate by natural fiber with synthesize one of macromolecular fibre or two kinds mix and weave.
3. the preparation method of nano particle antibacterial fabric according to claim 2, which is characterized in that the natural fibre
Dimension includes one of plant cotton fiber, flaxen fiber, wool fibre or a variety of mixing；The synthesis macromolecular fibre includes polyethers
Ketone, polyvinyl chloride, polystyrene, polyethylene, polypropylene, Kynoar, nylon, terylene, polycarbonate, poly terephthalic acid
One of ester, poly terephthalic acid propyl ester, polyamide or a variety of mixing.
4. the preparation method of nano particle antibacterial fabric according to claim 1, which is characterized in that institute in step sl
The polymerization methods for the graft polymerization reaction stated are one of bulk polymerization, suspension polymerisation, polymerisation in solution and emulsion polymerization.
5. the preparation method of nano particle antibacterial fabric according to claim 1, which is characterized in that institute in step sl
The graft polymerization reaction stated is caused by one of chemical initiator, ultraviolet light, radiation, plasma.
6. the preparation method of nano particle antibacterial fabric according to claim 1, which is characterized in that institute in step sl
The chemical structure for the organic monomer containing epoxy group stated is to contain epoxy group and carbon-carbon double bond in monomer molecule simultaneously.
7. the preparation method of nano particle antibacterial fabric according to claim 6, which is characterized in that institute in step sl
The organic monomer containing epoxy group stated includes glycidyl acrylate (GAA), glycidyl methacrylate
(GMA), one of 4- hydroxyl butyl propyleneglycol acid glycidyl ester (4-HB) or a variety of mixing.
8. the preparation method of nano particle antibacterial fabric according to claim 1, which is characterized in that institute in step s 2
The surface chemical modification stated be reacted with the hydroxyl of surface of nanometer zinc oxide using the silane coupling agent containing amino, thus
Amino is introduced into surface of nanometer zinc oxide.
9. the preparation method of nano particle antibacterial fabric according to claim 1, which is characterized in that institute in step s3
The pH value for the opening stated is controlled 7~14.
10. the preparation method of nano particle antibacterial fabric according to claim 1, which is characterized in that in step s3
Weight in the opening through amido modified nano granular of zinc oxide with the textile substrate with epoxy group
Amount is than control 0.05%~10%.
11. a kind of using antibacterial fabric made from preparation method described in any one of claim 1~10.
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