CN107044053A - A kind of antibacterial fabric and preparation method thereof - Google Patents
A kind of antibacterial fabric and preparation method thereof Download PDFInfo
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- CN107044053A CN107044053A CN201610082582.1A CN201610082582A CN107044053A CN 107044053 A CN107044053 A CN 107044053A CN 201610082582 A CN201610082582 A CN 201610082582A CN 107044053 A CN107044053 A CN 107044053A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M14/32—Polyesters
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M14/02—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin
- D06M14/04—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin of vegetal origin, e.g. cellulose or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M14/02—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin
- D06M14/06—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin of animal origin, e.g. wool or silk
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M14/08—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of synthetic origin
- D06M14/12—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials 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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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M14/20—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 natural origin
- D06M14/22—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 natural origin of vegetal origin, e.g. cellulose or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M14/28—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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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M14/34—Polyamides
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a kind of antibacterial fabric and preparation method thereof.The preparation method of the present invention, which is included on textile substrate to trigger, produces living radical, then carries out polymerisation with the organic monomer of the structure containing ionic liquid, you can.There are durable broad spectrum antibacterial functions by antibacterial fabric made from the preparation method of the present invention, applicable textile substrate scope is wide.The method of the present invention is simple and easy to apply, and cost is relatively low, is adapted to batch production, it is easy to promote.
Description
Technical field
The present invention relates to a kind of antibacterial fabric and preparation method thereof.
Background technology
Since own human history, the infectious disease caused by pathogenic microorganism is always the main of human health
Threaten.With the improvement of living standards with the progress of traffic technique, the scope of activities of the mankind is bigger, contact
Frequently, the propagation and outburst of serious infectious diseases happen occasionally, and personal hygiene health and public health are increasingly
It is valued by people.
It is to prevent infectious disease from occurring and popular important measures to prevent infringement of the pathogenic bacteria to human body, and is avoided
Or it is to reduce the effective means that human body is encroached on to reduce contact of the pathogenic bacteria with human body.
Flat textile product does not have inhibitory action to microorganisms such as bacterium and fungies, and pathogenic bacteria are easily in common textile
Growth and breeding on product, and contact and infringement human body.Antibacterial fabric can block the approach of transmission germ,
The breeding of germ on the textile is prevented, so as to be effectively isolated contact of the pathogenic bacteria with human body, human body is reduced
The risk encroached on by pathogenic bacteria, reduces the cross-infection rate of PE.In addition, antibacterial fabric may be used also
To avoid textile from being damaged because of the erosion of microorganism, suppress the pollution of bacterium decomposition on fabric and produce
Peculiar smell, it is ensured that the health of human body with it is comfortable.
At present, antiseptic is mainly attached on textile by the production of antibacterial fabric.Antiseptic includes
Nano metal particles (such as Nano Silver), metal salt (copper system, salt such as copper sulphate etc. of silver system) and
Some have antibacterial functions natural polymer such as chitosan etc..However, current conventional production method is scarce
Point is that antimicrobial component is mainly combined with textile by physical absorption etc., and its adhesion is weaker, makes
It can be lost in quickly with antimicrobial component after washing, the antibacterial effect of textile is not lasting.And utilize chemistry side
Method processing so that with covalent bond strong bonded between antiseptic and textile, is expected to obtain durable antibiotic spinning
Fabric, wherein, improve material anti-microbial property part research report in material surface grafting.For example,
Liu Qing et al. (《The preparation of the insoluble high-molecular anti-bacteria material of graft type water and antibacterial characteristics》, process engineering
Report, 2010,10：613-618.) the first grafted polystyrene on silica gel, then make polystyrene and three second
Amine, tri-n-butylamine, triphenylphosphine reaction make silica gel table so as to introduce quaternary ammonium and season phosphine groups in Silica Surface
Antibiotic property in face of Escherichia coli has been improved；But the second step reaction of this method will use chloroform etc. to have
Malicious solvent, is unsuitable for the large-scale application in industrial textile, and chloroform equal solvent can make partial weave
Product base material dissolves, restricted application.Zhang Qian et al. (《Hydroxypropyl cellulose graft modification antibacterial research》,
Colloid and polymer, 2010,28：171-180) it is prepared for a kind of alkoxy of one end with reactivity
Organosilicon antibacterial agent, make the hydroxyl reaction on alkoxy and hydroxypropyl cellulose, by organosilicon antibacterial agent
" grafting " on hydroxypropyl cellulose so that hydroxypropyl cellulose possesses antibacterial functions.It is this " to connect
Branch " is although method can be such that antiseptic is firmly bonded to covalent bond on base material, this " grafting " side
Method owned by France in " graft-to ", it requires all to have on base material and grafted chain molecule and can reacted to each other
Group, this make it that the textile substrate being applicable in this way is limited, and in the selection model of antiseptic
Place and be also extremely limited.
It is corresponding with " graft-to " method in high polymer material graft modification field, there is one kind
The grafting method of " graft-from ".First trigger i.e. in common substrate and produce living radical, recycle
Small molecule monomer polymerize as grafted chain by graft polymerization reaction on base material, and this can will contain special groups
Small molecule monomer be firmly bonded to covalent bond on base material.The grafting method of this " graft-from " by
In not needing there is special reaction group on base material, therefore, be applicable, preparing for all textiles
There are great potentiality on antibacterial fabric.However, this method at present antibacterial fabric preparation should
It is rarely reported with aspect.
Further, since the reason such as abuse of antibiotics, the drug-fast bacteria that resistance is have to antibiosis is threatened the mankind
Increasing, the mankind research and develop a kind of antibiotic and wanted for 10 years, and the disease of this antibiotic of resistance occur
Bacterium only needs 2 years, the available desperate situation of facing mankind antibiotic-free.According to BBC, current full generation
Boundary has 70,000 people to die from drug-fast bacteria infection every year, it is contemplated that to the year two thousand fifty, and dying from that the number of drug-fast bacteria has can
1,000,000 can be risen to.(disease prevention and control center) to have issued the U.S. resistance to for U.S. CDC in 2013
Medicine bacterium survey report, the U.S. has people more than 10,000 to die from drug-fast bacteria every year, more than the number for dying from AIDS.
Wherein, hospital cross-infection be drug-fast bacteria propagate main approach.In view of the threat day of drug-fast bacteria
Beneficial serious, in March, 2015, U.S. government starts " antimicrobial agent plan ", and overriding resistance is significantly increased
The financial allocation of bacterium (appropriation of antimicrobial agent is 1,200,000,000 dollars in U.S.'s financial budget in 2016).And
China, not only nosocomialtion can propagate drug-fast bacteria, and drug-fast bacteria has invaded life area and food
Thing chain.For example in the water source in 2014 Beijing, 6 parks find drug-fast bacteria；In Guangzhou Undergrounds in 2015
It was found that drug-fast bacteria.Find drug-fast bacteria in Chinese plant domesticated animal body and propagate to give people also to have been reported that.
The targeted bacterium of current antibacterial fabric main still Escherichia coli, staphylococcus aureus etc. are often
See bacterium, and the textile for having better effects for fungi and drug-fast bacteria seldom has been reported that, leisure opinion application.
Therefore, the research and development and preparation of the textile of antimicrobial agent, propagation and cross-infection for preventing drug-fast bacteria
It is significant.
The content of the invention
The technical problems to be solved by the invention are to overcome antibacterial functions in existing antibacterial fabric
Lasting, narrow antibacterial range, antibacterial functions group/particle and textile binding strength be not weak, general chemistry
The applicable textile substrate of method is limited in scope and the antibacterial category of conventional antimicrobial agent is limited, resists resistance to
The problems such as medicine bacterium seldom has been reported that, thus combined ionic liquid structure by graft copolymerization there is provided one kind
Method on to textile, the antibacterial fabric with ionic liquid antiseptic that the present invention is prepared resists
Persistently, its applicable textile substrate scope is wide for bacterium function, has the ionic liquid group of antibacterial functions with spinning
Fabric is with covalent bond strong bonded, and the textile prepared has durable broad spectrum antibacterial functions (including anti-
Drug-fast bacteria).
The present invention solves above-mentioned technical problem by following technical proposals：
The invention provides in a kind of organic monomer graft copolymerization by the structure containing ionic liquid to textile
Preparation method, the preparation method, which is included in trigger on described textile substrate, produces living radical,
The organic monomer of the structure containing ionic liquid is triggered to carry out being graft-polymerized instead on textile substrate again
Should, you can.
Wherein, the organic monomer of the structure containing ionic liquid is preferably with formula [A-B]+[C]-Represent,
Described A is the organic structure ele containing carbon-carbon double bond；Described B is described ionic liquid
Cation group；Described C is the anionic group of described ionic liquid；Blank character "-" is represented
Connected between construction unit A and B by covalent bond, but be not limited to carbon-carbon single bond；[A-B]+Represent [A-B]
For the cation of one positive charge of band, [C]-Represent the anion that [C] is one negative electrical charge of band.
It is preferred that described A includes but is not limited to vinyl and its derivative, pi-allyl and its derivative
Thing, acrylate and its derivative, methacrylate and its derivative and Styrene and its derivatives；
More preferably, described A is acrylate group, methacrylic acid ester group or styryl；Most preferably
For acrylate group or methacrylic acid ester group.
It is preferred that described B include but is not limited to imidazole radicals, pyridine radicals, pyrrole radicals, quaternary ammonium group,
Quaternary phosphine base, sulfonate radical；More preferably, described B be sulfonate radical, imidazole radicals or quaternary ammonium group, more preferably for
Imidazole radicals.
It is preferred that described C include but is not limited to halide ion, other inorganic ions or it is organic it is cloudy from
Son etc.；Wherein, described inorganic ions includes OH-、NO3 -、HSO4 -、BF4 -、PF6 -、SbF6 -、
AsF6 -Deng；Described organic anion includes CF3SO3 -、(CF3SO2)2N-、C3F7COO-、C4F9SO3 -、
CF3COO-、(CF3SO2)3C-、(C2F5SO2)3C-、(C2F5SO2)2N-Deng；More preferably, described C
For halide ion, BF4 -Or PF6 -。
Wherein, the described textile substrate scope of application is very wide, including natural polymer base material, artificial conjunction
Into polymer base material either both mixing；Described type of textiles is that this area is conventional described, such as
Fabric, non-woven cloth, yarn or fiber.Wherein, described natural polymer is cotton, hair, silk and fiber crops
In one or more；Described synthesis macromolecule is nylon, terylene, polypropylene fibre, acrylic fibers, polyvinyl, ammonia
Synthetic fibre, polyethylene, polyvinyl chloride, aromatic polyamide, aromatic polyester, polysulfones, polyether sulfone, polyethers
One or more in ketone, polyether-ether-ketone, Kynoar, polystyrene, makrolon and cellulose.
In the present invention, the concrete mode of described graft copolymerization is conventional described for this area, can be according to this hair
The performance requirement of bright obtained antibacterial fabric and selected.Described mode includes：Single kind
The structure containing ionic liquid monomer graft copolymerization on the textile；Two kinds and the above contain ionic liquid
The cograft of the monomer of structure on the textile；The monomer of the structure containing ionic liquid exists with other organic monomers
Cograft on textile.
In the present invention, the mode that described initiation produces living radical can be conventional described for this area, can
Selected according to the property of described base material and monomer, including chemical initiator triggers, ionising radiation is drawn
Hair, ultraviolet light-initiated, plasma trigger or ozone processing triggers etc..
In the present invention, described polymerisation is preferably carried out in closed system, described polymerisation
Reaction temperature and the reaction time can be selected according to the reactivity of described polymerisation；It is preferred that
Described reaction temperature is 10~160 DEG C；The described reaction time is 30min~48h.
In the present invention, the reaction system of described polymerisation is conventional described for this area, can be according to described
The property of monomer selected, be included in the body of monomer, the solution of monomer, the suspension of monomer or
Carried out in the emulsion of monomer.
The present invention still further provides to be grafted by the above-mentioned organic monomer by the structure containing ionic liquid
It is copolymerized to antibacterial fabric made from the preparation method on textile.
In antibacterial fabric produced by the present invention, the organic monomer of the structure containing ionic liquid is on the textile
Grafting rate (DG) is between 0.1% to 200%, and the calculation formula of described grafting rate (DG) is：
DG=(Wg-W0)/W0* 100%；Wherein, WgFor example weight after grafting, W0For sample before grafting
Weight；The measuring method of described grafting rate (DG) is that this area is conventional described, including weight method,
Combination of constituent content method of testing, infrared quantitative method of testing and the above method etc..
Without prejudice to the field on the basis of common sense, above-mentioned each optimum condition, can be combined, and produce this
Invent each preferred embodiments.
Agents useful for same and raw material of the present invention are commercially available.
The positive effect of the present invention is：
1st, the present invention is that the functional group with antibacterial effect is attached into textile in the way of covalent bond
On, binding strength is strong, and with excellent wash resistant, scratch-resistant performance, function is lasting；
2nd, antibacterial fabric prepared by the present invention has broad-spectrum antimicrobial effect, to various bacteria, fungi (bag
Include multiple drug-resistant bacteria) all there is extraordinary antibacterial effect；
3rd, preparation method of the invention need not add adhesive, resin or crosslinking agent, at utmost keep
The performances such as feel, the air-moisture-permeable of former textile, are suitable in terms of clothes, family expenses and industry
Using；
4th, the processing method of relatively current conventional anti-bacterial fibre, method of the invention is simple and easy to apply, into
This is relatively low, is adapted to batch production, it is easy to promote.
Embodiment
The present invention is further illustrated below by the mode of embodiment, but is not therefore limited the present invention to
Among described scope of embodiments.The experimental method of unreceipted actual conditions in the following example, according to normal
Rule method and condition, or selected according to catalogue.
In following embodiments, the grafting rate (DG) of described monomer on fabric is according to macromolecular grafted
General definition is studied, calculation formula is：DG=(Wg-W0)/W0* 100%；Wherein, WgTo connect
Example weight, W after branch0For example weight before grafting.
Raw material, medicine used in embodiment is commercially available.
Embodiment 1：Ultraviolet light-initiated solution graft copolymerization [acrylic acid ethyl trimethylamine] tetrafluoro boric acid of dacron
Preparation
Dacron is cut into appropriately sized, immersion 20 minutes in the acetone soln of benzophenone,
Dacron is then taken out, acetone is vapored away in ventilation so that benzophenone is dispersed in terylene and knitted
Thing surface.The aqueous solution of 10% [acrylic acid ethyl trimethylamine] tetrafluoro boric acid then is sprayed at into terylene to knit
Thing surface.The dacron is transferred in the quartz container that can be sealed, leads to nitrogen deoxygenation 20 minutes,
Sealing, irradiates initiation grafting polymerisation under wavelength 256nm uviol lamp, oxygen is led to after 30 minutes whole
Only react.
Using weight method measure grafting rate of [acrylic acid ethyl trimethylamine] tetrafluoro boric acid on dacron as
6.9%.
Embodiment 2：Silk fabrics chemistry initiation emulsion graft polymerization [1- ethyls -3,3 '-bis- (1- vinyl imidazoles)]
The preparation of two disulfates
Using toluene as dispersed phase, using anhydrous sorbitol hard fatty acid ester as emulsifying agent, under high shear stirring
It is configured to [1- ethyls -3,3 '-bis- (1- the vinyl imidazoles)] water-in-oil emulsion of two disulfates in toluene.
The leaching of 5 × 5cm silks silk is regard as initiator, letting nitrogen in and deoxidizing 20 with emulsion, adding potassium peroxydisulfate
Minute, by container closure, 60 DEG C of initiation grafting polymerisations are heated to, after reacting 5 hours, lead to oxygen
Terminating reaction.
[1- ethyls -3,3 '-bis- (1- vinyl imidazoles)] two disulfates are measured in silk fabrics with weight method
On grafting rate be 105.7%.
Embodiment 3：Cotton radiates the preparation of bulk graft 1- butyl -3- vinyl imidazole villaumites altogether
Pure cotton cloth is cut into suitable size, by 1- butyl -3- vinyl imidazole villaumites in the way of padding
Cotton surface is evenly coated in, cotton is placed as in irradiation tube, leads to nitrogen deoxygenation 20 minutes, is sealed,
Cobalt 60 source radiated by gamma-ray 50kGy is used at room temperature.Cotton after irradiation is using water as solvent, in rope
Extracted 48 hours in family name's extractor, remove unreacted monomer and homopolymer, drying is weighed.
Grafting rate of the 1- butyl -3- vinyl imidazole villaumites on pure cotton cloth is measured as 36.4% using weight method.
Embodiment 4：Polyethylene (PE) non-woven fabric radiation solution graft copolymerization [1- vinyl -3- butyl imidazoles]
The preparation of two (trifluoromethyl) acid amides
[1- vinyl -3- butyl imidazoles] two (trifluoromethyl) acid amides are soluble in water, be made into 10% it is water-soluble
Liquid.10g PE non-woven fabrics is weighed, is put into irradiation tube, is penetrated in air atmosphere with the gamma of cobalt 60 source
Line irradiates 30kGy.By the aqueous solution of foregoing [1- vinyl -3- butyl imidazoles] two (trifluoromethyl) acid amides
100mL is put into conical flask, by irradiated PE non-woven fabrics submergence in the solution, leads to nitrogen deoxygenation
20 minutes, sealing, with heating water bath to 70 DEG C, initiation grafting polymerisation cools after 6 hours and leads to oxygen
Terminating reaction.
[1- vinyl -3- butyl imidazoles] two (trifluoromethyl) acid amides are measured on PE non-woven fabrics with weight method
Grafting rate be 155.2%.
Embodiment 5：Spandex yarn ozone triggers suspension grafting 2- methyl -2- acrylimide propane sulfonic acid salt
Preparation
2- methyl -2- acrylimide propane sulfonic acid salt is poured into DMF, cut by height
Machine high-speed stirred is cut, 10% suspension is configured to.Spandex yarn is coiled on roller, sent out with ozone
Life produces ozone and spandex yarn is surface-treated.2- methyl -2- acrylimide propane sulfonic acid salt is existed
Suspension in DMF is put into conical flask, and the spandex yarn that ozone is treated is soaked
Not in suspension, lead to nitrogen deoxygenation 20 minutes, conical flask sealed, is subsequently heated to 70 DEG C,
Initiation grafting polymerisation, cool logical oxygen terminating reaction after 3 hours.
Grafting rate of the 2- methyl -2- acrylimide propane sulfonic acid salt in spandex yarn is measured by weight method
For 0.9%.
Embodiment 6：Nylon fiber plasma triggers methacrylic acid -2- ethyl season phosphine ester nitric acid and [1-
Ethyl -3,3 '-bis- (1- vinyl imidazoles)] trifluoromethyl sulfonic acid solution cograft
Using water as solvent, configuration methacrylic acid -2- ethyl season phosphine ester nitric acid and [1- ethyl -3,3 '-bis- (1-
Vinyl imidazole)] mixed solution of trifluoromethyl sulfonic acid, wherein, the mol ratio of two kinds of monomers is 1:1,
Total monomer is 20%.
A certain amount of nylon fiber is surface-treated in air atmosphere with low temperature plasma equipment
10 minutes, then treated nylon fiber is put into conical flask, adds the good mixing of above-mentioned configuration
Monomer solution, leads to nitrogen deoxygenation 20 minutes, sealing.It is heated to 50~70 DEG C, initiation grafting polymerisation,
Reaction time is 4 hours.
After reaction terminates, by sample in apparatus,Soxhlet's using water for solvent extraction 72 hours, removal is residual
Monomer and homopolymer are stayed, is dried, elementary analysis, test nitrogen and phosphorus element content is carried out, calculates two
Plant the respective grafting rate of monomer.
The sample prepared with above-mentioned condition, the grafting rate of methacrylic acid -2- ethyl season phosphine ester nitric acid exists
27.9%, the grafting rate of [1- ethyl -3,3 '-bis- (1- vinyl imidazoles)] trifluoromethyl sulfonic acid is 18.4%.
Embodiment 7：Cotton/polyamide fibre blend fabric radiation binary cograft hydroxy-ethyl acrylate and methacrylic acid
The preparation of -2- ethyl season phosphine ester nitric acid
Cotton/polyamide fibre blend fabric (cotton/polyamide fibre content ratio is 60/40) is cut into suitable size.Configuration
The mixed aqueous solution of hydroxy-ethyl acrylate and methacrylic acid -2- ethyl season phosphine ester nitric acid, wherein acrylic acid hydroxyl
The volume ratio of ethyl ester/methacrylic acid -2- ethyl season phosphine ester nitric acid/waters is 10/15/75.By this mixed solution
100mL is placed in irradiation tube, and the cotton cut out/polyamide fibre blend fabric is immersed in solution, leads to nitrogen
Deoxygenation 20 minutes, sealing, at room temperature with Co 60 radiated by gamma-ray 20kGy.Products therefrom is with water
For solvent, extracting 48 hours in apparatus,Soxhlet's, to remove unreacted monomer and homopolymer, then
Modified fabric drying is weighed.
Total grafting rate that two kinds of monomers are measured using weight method is obtained as 52.2% with phosphorus element content measuring and calculation
The grafting rate for going out methacrylic acid -2- ethyl season phosphine ester nitric acid is 36.1%, the grafting rate of hydroxy-ethyl acrylate
For (52.2-36.1) %=16.1%.
Embodiment 8：Cotton radiates the preparation of bulk graft 1- butyl -3- vinylpyridine villaumites altogether
1- butyl -3- vinylpyridine villaumites are evenly coated in cotton surface, exposure dose is 100kGy,
Other conditions such as embodiment 3.1- butyl -3- vinylpyridine villaumites connecing on cotton is measured with weight method
Branch rate such as table 1.
Embodiment 9：The system of cotton pre-irradiated solution graft copolymerization [methacrylic acid ethyl trimethylamine] tetrafluoro boric acid
It is standby
[methacrylic acid ethyl trimethylamine] tetrafluoro boric acid is soluble in water, be made into 10% the aqueous solution.Claim
10g cottons are taken, are put into irradiation tube.Other conditions such as embodiment 4.[methyl-prop is measured with weight method
Olefin(e) acid ethyl trimethylamine] grafting rate of the tetrafluoro boric acid on cotton such as table 1.
Embodiment 10：Cotton yarn ozone triggers the preparation of suspension grafting Methacrylamide quaternary ammonium salt
Methacrylamide quaternary ammonium salt is poured into DMF, by high shear machine at a high speed
Stir, be configured to 10% suspension.Cotton yarn is coiled on roller, produced with ozone generator
Ozone is surface-treated to cotton yarn.Other conditions such as embodiment 4.Methyl-prop is measured with weight method
Grafting rate of the acrylamide quaternary ammonium salt on cotton yarn such as table 1.
Embodiment 11：Silk fabrics chemistry initiation emulsion graft polymerization [1- ethyls -3,3 '-bis- (1- vinylpyridines
Cough up)] preparation of trifluoromethyl sulfonic acid
Using toluene as dispersed phase, using anhydrous sorbitol hard fatty acid ester as emulsifying agent, under high shear stirring
It is configured to [1- ethyls -3,3 '-bis- (1- the vinyl pyrroles)] Water-In-Oil of trifluoromethyl sulfonic acid in toluene
Type emulsion.Other conditions such as embodiment 1.Measured [1- ethyls -3,3 '-bis- (1- vinyl pyrroles)] with weight method
Grafting rate of the trifluoromethyl sulfonic acid on silk fabrics such as table 1.
Embodiment 12：Cotton mutual radiation bulk graft [acrylic acid ethyl trimethylamine] trifluoromethyl sulfonic acid
Prepare
[acrylic acid ethyl trimethylamine] trifluoromethyl sulfonic acid is evenly coated in cotton surface, exposure dose is
100kGy, other conditions such as embodiment 3.[acrylic acid ethyl trimethylamine] trifluoromethyl is measured with weight method
Grafting rate of the sulfonate on cotton such as table 1.
Embodiment 13：The preparation of cotton mutual radiation bulk graft [styryl pyrroles] trifluoromethyl carboxylate
[styryl pyrroles] trifluoromethyl carboxylate is evenly coated in cotton surface, exposure dose is 100
KGy, other conditions such as embodiment 3.[styryl pyrroles] trifluoromethyl carboxylate is measured with weight method to exist
Grafting rate such as table 1 on cotton.
Comparative example 1：Dacron sprays [acrylic acid ethyl trimethylamine] tetrafluoro boric acid
Dacron is cut into appropriately sized, immersion 20 minutes in the acetone soln of benzophenone,
Dacron is then taken out, acetone is vapored away in ventilation so that benzophenone is dispersed in terylene and knitted
Thing surface.The aqueous solution of 10% [acrylic acid ethyl trimethylamine] tetrafluoro boric acid then is sprayed at into terylene to knit
Thing surface.
Comparative example 2：Cotton pads 1- butyl -3- vinyl imidazole villaumites
Pure cotton cloth is cut into suitable size, by 1- butyl -3- vinyl imidazole villaumites in the way of padding
It is evenly coated in cotton surface.
Comparative example 3：Cotton pads levamisole hydrochloride
Pure cotton cloth is cut into suitable size, levamisole hydrochloride is evenly coated in cotton in the way of padding
Surface.
Comparative example 4：Cotton grafting vinyl imidazoles
Pure cotton cloth is cut into suitable size, vinyl imidazole is evenly coated in cotton table in the way of padding
Face, cotton is placed as in irradiation tube, led to nitrogen deoxygenation 20 minutes, Co 60 is used in sealing at room temperature
Source radiated by gamma-ray 50kGy.Cotton after irradiation extracts 48 using water as solvent in apparatus,Soxhlet's
Hour, unreacted monomer and homopolymer are removed, drying is weighed.
Comparative example 5：Polyethylene (PE) non-woven fabric radiates solution graft copolymerization vinyl imidazole
Vinyl imidazole is soluble in water, be made into 10% the aqueous solution.10g PE non-woven fabrics is weighed, is put
Enter in irradiation tube, in air atmosphere with the radiated by gamma-ray 30kGy of cobalt 60 source.By foregoing ethene
The aqueous solution 100mL of base imidazoles is put into conical flask, and irradiated PE non-woven fabrics is immersed in into solution
In, lead to nitrogen deoxygenation 20 minutes, sealing is whole to the logical oxygen of cooling after 70 DEG C, 6 hours with heating water bath
Only react.
With reference to national standard《The evaluation part 2 of GB/T 20944.2-2007 antibacterial textile performances：
Absorption process》, test its anti-Escherichia coli, staphylococcus aureus, Candida albicans, methicillin-resistant
The effect of the antibacterial effect of staphylococcus, vancomycin resistance a coccus.
Test process is, as control sample, to match somebody with somebody corresponding bacterium by national standard with unmodified respective fabric
Determine normal concentration, be added dropwise respectively on modified and unmodified fabric, cultivate corresponding under 37 degrees Celsius
Time., will be thin on sample using the sample for cultivating 24 hours and the sample for cultivating 0 hour as control
Antibiotic rate, its result such as table 1 are tested with the method for plate culture count after bacterium elution.
In order to investigate the durability of fabric and the persistence of antibacterial effect after graft modification, according to ATCC
61-2006,2A standard accelerate 30 circulations of washing, and (equivalent to the 150 times daily washings of family expenses are approached
The overall service life of textile) after, test antibacterial effect as stated above again, its result such as table 2.
Table 1
Table 2
According to standard GB/T/T 12704《Textile fabric penetrability method of testing》, test
State the penetrability of the fabric in embodiment before and after graft modification.As a result find, compared with unmodified fabric,
The water vapour permeability of the textile of the structurally-modified grafting of ionic liquid made from embodiment 1~13 is not deteriorated,
Substantially feel, the breathable moisture permeability of former yarn fabric are maintained.
Claims (10)
1. a kind of organic monomer graft copolymerization by the structure containing ionic liquid is to the preparation method on textile,
Characterized in that, the preparation method, which is included in trigger on textile substrate, produces living radical, then trigger
The organic monomer of the described structure containing ionic liquid carries out graft polymerization reaction on textile substrate, you can.
2. preparation method as claimed in claim 1, it is characterised in that described knot containing ionic liquid
The organic monomer of structure is with formula [A-B]+[C]-Represent；Described A is the organic structure containing carbon-carbon double bond
Unit；Described B is the cation group of described ionic liquid；Described C is described ion
The anionic group of liquid；Blank character "-" represents to connect by covalent bond between construction unit A and B,
But it is not limited to carbon-carbon single bond；[A-B]+Represent the cation that [A-B] is one positive charge of band, [C]-Represent
[C] is the anion of one negative electrical charge of band.
3. preparation method as claimed in claim 2, it is characterised in that described A be vinyl and
Its derivative, pi-allyl and its derivative, acrylate and its derivative, methacrylate and its spread out
One or more in biological and Styrene and its derivatives；Described A be preferably acrylate group,
Methacrylic acid ester group or styryl, are more preferably acrylate group or methacrylic acid ester group.
4. preparation method as claimed in claim 2, it is characterised in that described B be imidazole radicals,
One kind in pyridine radicals, pyrrole radicals, quaternary ammonium group, quaternary phosphines base and sulfonate radical.
5. preparation method as claimed in claim 2, it is characterised in that described C be halide ion,
OH-、NO3 -、HSO4 -、BF4 -、PF6 -、SbF6 -、AsF6 -、CF3SO3 -、(CF3SO2)2N-、C3F7COO-、
C4F9SO3 -、CF3COO-、(CF3SO2)3C-、(C2F5SO2)3C-(C2F5SO2)2N-In one kind.
6. preparation method as claimed in claim 1, it is characterised in that described textile substrate model
Enclose including either both mixing of natural polymer base material, artificial synthesized polymer base material；
It is preferred that described type of textiles is one kind in fabric, non-woven cloth, yarn and fiber；
It is preferred that described natural polymer base material is the one or more in cotton, hair, silk and fiber crops；
It is preferred that described artificial synthesized polymer base material be nylon, terylene, polypropylene fibre, acrylic fibers, polyvinyl,
It is spandex, polyethylene, polyvinyl chloride, aromatic polyamide, aromatic polyester, polysulfones, polyether sulfone, poly-
One kind or many in ether ketone, polyether-ether-ketone, Kynoar, polystyrene, makrolon and cellulose
Kind.
7. preparation method as claimed in claim 1, it is characterised in that the side of described graft copolymerization
Formula includes：The graft copolymerization on the textile of the monomer of the structure containing ionic liquid of single kind, two kinds and
More than the monomer cograft on the textile of the structure containing ionic liquid or the list of the structure containing ionic liquid
Three kinds of body and the cograft of other organic monomers on the textile.
8. preparation method as claimed in claim 1, it is characterised in that described initiation produces activity
The mode of free radical includes chemical initiator initiation, ionising radiation initiation, ultraviolet light-initiated, plasma
Trigger the one kind handled with ozone in triggering；
And/or, described polymerisation is carried out in closed system, and described polymeric reaction temperature is
10~160 DEG C；Described polymerization reaction time is 30min~48h；
And/or, the reaction system of described polymerisation is the body, the solution of monomer, monomer of monomer
One kind in the emulsion of suspension and monomer.
9. a kind of antibacterial fabric as made from preparation method according to any one of claims 1 to 8.
10. antibacterial fabric as claimed in claim 9, it is characterised in that described antibacterial fabric
In, the grafting rate of the organic monomer of the structure containing ionic liquid on the textile is between 0.1% to 200%.
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