CN107287899B - The antibiotic finishing method of cotton fabric - Google Patents

The antibiotic finishing method of cotton fabric Download PDF

Info

Publication number
CN107287899B
CN107287899B CN201710597050.6A CN201710597050A CN107287899B CN 107287899 B CN107287899 B CN 107287899B CN 201710597050 A CN201710597050 A CN 201710597050A CN 107287899 B CN107287899 B CN 107287899B
Authority
CN
China
Prior art keywords
solution
initiator
cotton fabric
nano
water
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201710597050.6A
Other languages
Chinese (zh)
Other versions
CN107287899A (en
Inventor
任一波
俞成丙
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Pulcra Specialty Chemicals Shanghai Co Ltd
Original Assignee
Pulcra Specialty Chemicals Shanghai Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Pulcra Specialty Chemicals Shanghai Co Ltd filed Critical Pulcra Specialty Chemicals Shanghai Co Ltd
Priority to CN201710597050.6A priority Critical patent/CN107287899B/en
Publication of CN107287899A publication Critical patent/CN107287899A/en
Application granted granted Critical
Publication of CN107287899B publication Critical patent/CN107287899B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/356Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms
    • D06M15/3562Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F226/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
    • C08F226/02Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a single or double bond to nitrogen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F292/00Macromolecular compounds obtained by polymerising monomers on to inorganic materials
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/347Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated ethers, acetals, hemiacetals, ketones or aldehydes
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2400/00Specific information on the treatment or the process itself not provided in D06M23/00-D06M23/18
    • D06M2400/01Creating covalent bondings between the treating agent and the fibre

Abstract

The present invention relates to a kind of antibiotic finishing methods of cotton fabric.A kind of antibiotic finishing method of cotton fabric, comprising the following steps: preparation nano-zinc oxide compound solution;Prepare QAS polymer solution;Nano-zinc oxide compound solution and QAS polymer solution are mixed to get zinc oxide-QAS polymer complex antimicrobials;Zinc oxide-QAS polymer complex antimicrobials and water are mixed to get the antibiotic finishing solution that concentration is 50g/L~500g/L;Cotton fabric is carried out using antibiotic finishing solution to pad processing;And cotton fabric is dried to padding that treated.The cotton fabric of the antibiotic finishing method processing of above-mentioned cotton fabric, the antibacterial finishing agent used is the compound of quaternized copolymer and nano zine oxide, fabric has good anti-microbial property, and can according to actual requirement can flexible modulation two types antibacterial agent dosage, strengthen local antibacterial effect, antibacterial finishing agent and cotton fabric binding strength are good simultaneously, wash resistant, durable antibacterial effect.

Description

The antibiotic finishing method of cotton fabric
Technical field
The present invention relates to a kind of antibiotic finishing methods of cotton fabric.
Background technique
Cotton fabric is the most common textile fabric in our daily lifes, but cotton fabric is easy to absorb human sweat glands and sebum The sweat and metabolism product of glandular secretion easily lead to the growth and breeding of microorganism to form the nutrient source of microorganism, Cause the shirt of color-woven fabric to generate bacterial plaque, so that textile is generated mildew, influence human health, thus needs to carry out cotton fabric Antibiotic finish, thus people research and develop always the weaving antibacterial agent of function admirable.
In general, weaving antibacterial agent is divided into inorganic antiseptic, organic antibacterial agent and natural antibacterial agent according to material source, Wherein quaternary polymer antibacterial agent and nano zine oxide are the common antibacterial agents of two classes, and quaternary polymer antibacterial agent is deposited Not washable, easy elution, antibacterial cannot the disadvantage toxic to human body after long-acting, elution;And nano zine oxide has nontoxic, ratio The excellent properties such as surface area is big, anti-ultraviolet radiation and antibacterial, thus attempted to the two is compound, it is total to prepare quaternary ammonium salt The complex antimicrobials of polymers and nano zine oxide, are applied in textile finishing.But existing quaternary high-molecular anti-bacteria Agent and nanometer zinc oxide composite antibiosis agent, there is some intrinsic deficiencies, for example, since nano zine oxide and quaternary ammonium salt are total Binding force between polymers is not strong, leads to the rapidly losing of finishing textiles nano zine oxide in use, can not be long-acting Play the antibacterial effect of nano zine oxide;For another example, nano zine oxide is easily reunited, without preferably solving the reunion of nano material Problem thus greatly reduces the antibacterial effect of nano zine oxide;For another example, nano zine oxide and quaternized copolymer composite antibacterial Agent easily falls off from textile fabric, especially after multiple washing, to lose original anti-microbial property etc..
Summary of the invention
Based on this, it is necessary to provide a kind of antibiotic finish side that can improve antibiotic property and the wash fast cotton fabric of cotton fabric Method.
A kind of antibiotic finishing method of cotton fabric, comprising the following steps:
It prepares nano-zinc oxide compound solution: providing the first reaction raw materials, first reaction raw materials are according to quality hundred Dividing content meter includes: 1%~5% active nano-ZnO, 20%~30% carboxy acrylic class monomer, 5%~10% Allyl glycidyl ether, 3%~6% the first initiator and water, the active nano-ZnO be silicon containing double bonds The coupling agent modified nano zine oxide of alkane, using the water as solvent, the active nano-ZnO, the carboxy acrylic class list Polymerization reaction occurs under the initiation of first initiator for body and the allyl glycidyl ether, and to obtain nano zine oxide multiple Polymer solution;
It prepares QAS polymer solution: the second reaction raw materials is provided, second reaction raw materials contain according to quality percentage Meter include: 25%~35% dimethyl diallyl ammonium chloride, 1%~3% carboxy acrylic class monomer, 0.5%~ 1% allyl glycidyl ether, 3%~6% the second initiator and water, using the water as solvent, the dimethyl diene Propyl ammonium chloride, the carboxy acrylic class monomer and the allyl glycidyl ether are under the initiation of second initiator Polymerization reaction occurs and obtains QAS polymer solution;
The nano-zinc oxide compound solution and the QAS polymer solution are mixed to get zinc oxide-quaternary ammonium salt Polymer complex antimicrobials;
It is 50g/L~500g/L's that the zinc oxide-QAS polymer complex antimicrobials and water, which are mixed to get concentration, Antibiotic finishing solution;
Cotton fabric is carried out using the antibiotic finishing solution to pad processing;And
To padding that treated, the cotton fabric is dried.
The preparation method of the antibiotic finishing method of above-mentioned cotton fabric, has the advantage that
(1) antibiotic finishing method of above-mentioned cotton fabric is more able to satisfy actual needs, and different types of antibacterial agent is to same Kind pathogen has different Antibacterial mechanism and validity, and same antibacterial agent also has different resist for different pathogens Bacterium mechanism of action and inhibition range, can suitably increase nano-zinc oxide compound solution usage on the cotton fabric for having light to irradiate, The dosage of energy flexible modulation nano-zinc oxide compound solution and QAS polymer solution, local strengthening required for reaching Antibacterial effect, such antibiotic finish effect is more able to satisfy final use and actual needs, to more preferably meet the needs of client;
(2) above-mentioned zinc oxide-QAS polymer complex antimicrobials contain a large amount of carboxyl and epoxy group in molecular structure Group can have an effect when being applied to the final finishing of cotton fabric with the hydroxyl on cotton fiber, be formed compared with strong covalent bond, will be compound Antibacterial finishing agent is grafted on cotton fiber, to guarantee to obtain between finishing agent and fiber, binding strength is good, and wash resistant reaches lasting Antibiotic finish effect;
(3) in zinc oxide-QAS polymer complex antimicrobials, nano zine oxide dispersion is extremely uniform, and nanometer is not present The phenomenon that particle aggregation, can effectively play the antibacterial effect of nano zine oxide, the complex antimicrobials by quaternary ammonium salt cationic and The synergistic effect of nano zine oxide can give full play to the antibacterial effect of organic and inorganic materials, the good antibacterial of providing cotton fabric Performance.
In one of the embodiments, by the nano-zinc oxide compound solution and the QAS polymer solution Mass ratio is that 1:1~1:10 is mixed to get the zinc oxide-QAS polymer complex antimicrobials.
It is described in one of the embodiments, using the antibiotic finishing solution to be carried out to cotton fabric the step of padding processing In, it is carried out by the way of second dipping and rolling, the pressure for padding processing is 2kg/cm2~4kg/cm2, described to pad processing Pick-up is 50%~90%.
In one of the embodiments, in the described pair of withering step of cotton fabric of padding that treated, The cotton fabric that will pad that treated bakes 2min in 80 DEG C~100 DEG C preliminary drying 5min~20min, then at 120 DEG C~140 DEG C ~20min.
The silane coupling agent containing double bonds is γ-methacryloxypropyl three in one of the embodiments, Methoxy silane.
The active nano-ZnO is prepared by following steps in one of the embodiments:
After nano zine oxide, γ-methacryloxypropyl trimethoxy silane and solvent are mixed, ultrasonic disperse is obtained To dispersion liquid;And
Active nano-ZnO was obtained by the dispersion liquid back flow reaction 10 hours~20 hours.
The solvent includes ethyl alcohol and water in one of the embodiments, the nano zine oxide, the ethyl alcohol, described Water and the mass ratio of the γ-methacryloxypropyl trimethoxy silane are 1:30~60:10~20:1~5.
First initiator is in sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate in one of the embodiments, At least one, or, first initiator includes at least one of sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate and sulfurous acid Hydrogen sodium;Second initiator is selected from least one of sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate, or, described second draws Sending out agent includes at least one of sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate and sodium hydrogensulfite.
It is described using the water as solvent in one of the embodiments, the active nano-ZnO, the carboxyl propylene Polymerization reaction occurs under the initiation of first initiator and obtains nano oxygen for acrylic monomer and the allyl glycidyl ether The step of changing zinc complexes solution specifically:
By the active nano-ZnO, the water, the half of the carboxy acrylic class monomer, the allyl The half of glycidol ether and the first initiator solution mixing containing the half in first initiator are equal It is even, 70 DEG C~85 DEG C are heated to, is stirred to react 15 minutes~20 minutes and obtains mixed liquor;
By the half of the carboxy acrylic class monomer, the half of the allyl glycidyl ether and contain First initiator solution of the half in first initiator is added dropwise in the mixed liquor, is stirred at 70 DEG C~85 DEG C It mixes reaction and obtains nano-zinc oxide compound solution in 3 hours~4.5 hours.
In one of the embodiments, using the water as solvent, the dimethyl diallyl ammonium chloride, the carboxyl third Polymerization reaction occurs under the initiation of second initiator and obtains quaternary ammonium for alkene acrylic monomer and the allyl glycidyl ether The step of salt polymer solution specifically:
By the dimethyl diallyl ammonium chloride, the water, containing the one third in second initiator Three points in two initiator solutions, the one third in the allyl glycidyl ether and the carboxy acrylic class monomer One of mixing after be heated to 70 DEG C~85 DEG C, be stirred to react 8 minutes~15 minutes and obtain the first reaction solution;
By the second initiator solution, the allyl glycidol containing the one third in second initiator The one third in one third and the carboxy acrylic class monomer in ether is added dropwise in first reaction solution, 70 DEG C~ It is stirred to react at 85 DEG C 10 minutes~20 minutes and obtains the second reaction solution;And
By the second initiator solution, the allyl glycidol containing the one third in second initiator The one third in one third and the carboxy acrylic class monomer in ether is added dropwise in second reaction solution, 70 DEG C~ It is stirred to react at 85 DEG C 3 hours~5 hours and obtains the QAS polymer solution.
Specific embodiment
It is further described in detail below in conjunction with antibiotic finishing method of the specific embodiment to cotton fabric.
The antibiotic finishing method of the cotton fabric of one embodiment, comprising the following steps:
Step S110, it is modified to obtain active nano oxidation using Nano-zinc Oxide by Silane Coupling Agents containing double bonds Zinc.
Silane coupling agent containing double bonds is γ-methacryloxypropyl trimethoxy in one of the embodiments, Base silane.
It is modified and is lived using Nano-zinc Oxide by Silane Coupling Agents containing double bonds in one of the embodiments, The step of property nano zine oxide specifically:
Step S111, after nano zine oxide, γ-methacryloxypropyl trimethoxy silane and solvent being mixed, Ultrasonic disperse obtains dispersion liquid.
Preferably, dispersion liquid is obtained within ultrasonic disperse 1 hour.
Preferably, nano zine oxide and γ-methacryloxypropyl trimethoxy silane mass ratio are 1:1~1: 5。
Preferably, solvent is second alcohol and water, nano zine oxide, ethyl alcohol, water and γ-methacryloxypropyl trimethoxy The mass ratio of base silane is 1:30~60:10~20:1~5.
Step S112, active nano-ZnO was obtained by dispersion liquid back flow reaction 10 hours~20 hours.
Preferably, the back flow reaction at 60 DEG C.
Preferably, the heating water bath back flow reaction by dispersion liquid at 60 DEG C.
Preferably, by dispersion liquid back flow reaction 10 hours~20 hours, it is cooled to room temperature separation of solid and liquid, after solid is washed Obtain active nano-ZnO.It is further preferred that be separated by solid-liquid separation using centrifugation, make solid is washed with deionized and obtain Active nano-ZnO.
Step S120, nano-zinc oxide compound solution is prepared.
Prepare nano-zinc oxide compound solution specifically includes the following steps:
Step S121, the first reaction raw materials are provided.
First reaction raw materials according to the active nano-ZnO that mass percentage meter includes: 1%~5%, 20%~ 30% carboxy acrylic class monomer, 5%~10% allyl glycidyl ether, 3%~6% the first initiator and water.
In one of the embodiments, carboxy acrylic class monomer in acrylic acid and methacrylic acid at least one Kind.
In one of the embodiments, the first initiator in sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate at least It is a kind of.
In one of the embodiments, the first initiator include in sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate at least A kind of and sodium hydrogensulfite.Preferably, the matter of at least one of sodium sulphate, potassium peroxydisulfate and ammonium persulfate and sodium hydrogensulfite Amount is than being 2~4.5:1~1.5.
Water is deionized water in one of the embodiments,.
Step S122, it takes water as a solvent, active nano-ZnO, carboxy acrylic class monomer and allyl glycidyl ether Polymerization reaction occurs under the initiation of the first initiator and obtains nano-zinc oxide compound solution.
In one of the embodiments, step S122 the following steps are included:
Step S1221, active nano-ZnO, water, the half of carboxy acrylic class monomer, allyl glycidyl is sweet The half of oily ether and the first initiator solution containing the half in the first initiator are uniformly mixed, and are heated to 70 DEG C~85 DEG C, it is stirred to react 15 minutes~20 minutes and obtains mixed liquor.
In one of the embodiments, the first initiator in sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate at least One kind, the mass ratio of initiator and water is 3:10~6:10 in the first initiator solution.
In one of the embodiments, the first initiator include in sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate at least A kind of and sodium hydrogensulfite, in the first initiator solution at least one of sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate with The mass ratio of water is 3:20~6:20, and the mass ratio of sodium hydrogensulfite and water is 1:20~1.5:20.
In one of the embodiments, using heating water bath to 70 DEG C~85 DEG C.
Step S1222, by the half of carboxy acrylic class monomer, the half of allyl glycidyl ether and contain There is the first initiator solution of the half in the first initiator to be added dropwise in the mixed liquor, is stirred at 70 DEG C~85 DEG C Reaction obtains nano-zinc oxide compound solution in 3 hours~4.5 hours.
The first initiator is selected from sodium peroxydisulfate, potassium peroxydisulfate in one of the embodiments, And at least one of ammonium persulfate, the mass ratio of the first initiator and water is 3:10~6:10 in the first initiator solution.
In one of the embodiments, the first initiator include in sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate at least A kind of and sodium hydrogensulfite, in the first initiator solution at least one of sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate with The mass ratio of water is 3:20~6:20, and the mass ratio of sodium hydrogensulfite and water is 1:20~1.5:20.
In one of the embodiments, by the initiator solution containing the half in initiator, allyl glycidyl The half in half and carboxy acrylic class monomer in glycerin ether is added dropwise in mixed liquor after mixing.
Obtained nano-zinc oxide compound solution can be used directly, filtered and washed after can also being cooled to room temperature To nano-zinc oxide compound.The structural formula of obtained nano-zinc oxide compound is as follows:
Wherein,For nano zine oxide, R is H or methyl, n1、n2、n3It is integer.
Step S130, QAS polymer solution is prepared.
Prepare QAS polymer solution specifically includes the following steps:
Step S131, the second reaction raw materials are provided.
Propose the dimethyl diallyl chlorination that the second reaction raw materials include: 25%~35% according to mass percentage meter Ammonium, 1%~3% carboxy acrylic class monomer, 0.5%~1% allyl glycidyl ether, 3%~6% second cause Agent and water.
In one of the embodiments, carboxy acrylic class monomer in acrylic acid and methacrylic acid at least one Kind.
In one of the embodiments, the second initiator in sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate at least It is a kind of.
In one of the embodiments, the second initiator include in sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate at least A kind of and sodium hydrogensulfite.Preferably, the matter of at least one of sodium sulphate, potassium peroxydisulfate and ammonium persulfate and sodium hydrogensulfite Amount is than being 2~4.5:1~1.5.
Water is deionized water in one of the embodiments,.
Step S132, it takes water as a solvent, dimethyl diallyl ammonium chloride, carboxy acrylic class monomer and allyl glycidyl Polymerization reaction occurs under the initiation of the second initiator and obtains QAS polymer solution for glycerin ether.
In one of the embodiments, step S132 the following steps are included:
Step S1321, by dimethyl diallyl ammonium chloride, water, second containing the one third in the second initiator After one third mixing in one third and carboxy acrylic class monomer in initiator solution, allyl glycidyl ether 70 DEG C~85 DEG C are heated to, is stirred to react 8 minutes~15 minutes and obtains the first reaction solution.
In one of the embodiments, the second initiator in sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate at least One kind, the mass ratio of the second initiator and water is 3:10~6:10 in the second initiator solution.
In one of the embodiments, the second initiator include in sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate at least A kind of and sodium hydrogensulfite, in the second initiator solution at least one of sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate with The mass ratio of water is 3:20~6:20, and the mass ratio of sodium hydrogensulfite and water is 1:20~1.5:20.
In one of the embodiments, using heating water bath to 70 DEG C~85 DEG C.
Step S1322, the second initiator solution, allyl glycidyl containing the one third in the second initiator is sweet The one third in one third and carboxy acrylic class monomer in oily ether is added dropwise in the first reaction solution, at 70 DEG C~85 DEG C It is stirred to react 10 minutes~20 minutes and obtains the second reaction solution.
In one of the embodiments, the second initiator in sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate at least One kind, the mass ratio of the second initiator and water is 3:10~6:10 in the first initiator solution.
In one of the embodiments, the second initiator include in sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate at least A kind of and sodium hydrogensulfite, in the second initiator solution at least one of sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate with The mass ratio of water is 3:20~6:20, and the mass ratio of sodium hydrogensulfite and water is 1:20~1.5:20.
In one of the embodiments, by the second initiator solution, alkene containing the one third in the second initiator The one third in one third and carboxy acrylic class monomer in propyl glycidyl ether is added dropwise to first after mixing Reaction solution.
Step S1323, the second initiator solution, allyl glycidyl containing the one third in the second initiator is sweet The one third in one third and carboxy acrylic class monomer in oily ether is added dropwise in the second reaction solution, at 70 DEG C~85 DEG C It is stirred to react 3 hours~5 hours and obtains QAS polymer solution.
In one of the embodiments, the second initiator in sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate at least One kind, the mass ratio of the second initiator and water is 3:10~6:10 in the second initiator solution.
In one of the embodiments, the second initiator include in sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate at least A kind of and sodium hydrogensulfite, in the second initiator solution at least one of sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate with The mass ratio of water is 3:20~6:20, and the mass ratio of sodium hydrogensulfite and water is 1:20~1.5:20.
In one of the embodiments, by the second initiator solution, alkene containing the one third in the second initiator The one third in one third and carboxy acrylic class monomer in propyl glycidyl ether is added dropwise to second after mixing Reaction solution.
QAS polymer solution can be used directly.Contain QAS polymer, quaternary ammonium in QAS polymer solution The structural formula of salt polymer is as follows:
Wherein, R is H or methyl, n4、n5、n6It is integer.
Step S140, nano-zinc oxide compound solution and QAS polymer solution are mixed to get zinc oxide-quaternary ammonium Salt polymer complex antimicrobials.
The mass ratio of nano-zinc oxide compound solution and QAS polymer solution is 1 in one of the embodiments: 1~1:10.
Step S150, by zinc oxide-QAS polymer complex antimicrobials and water be mixed to get concentration be 50g/L~ The antibiotic finishing solution of 500g/L.
In the step, concentration is that the antibiotic finishing solution of 50g/L~500g/L refers to zinc oxide-season of step S140 preparation Concentration of the ammonium salt polymer complex antimicrobials in antibiotic finishing solution.
Step S160, cotton fabric is carried out using antibiotic finishing solution padding processing.
It is carried out by the way of second dipping and rolling in one of the embodiments, the pressure for padding processing is 2kg/cm2 ~4kg/cm2, the pick-up for padding processing is 50%~90%.Second dipping and rolling refers to rolling after cotton fabric impregnates through roll It crosses, was rolled after impregnating again later through roll.
Step S170, to padding that treated, cotton fabric is dried.
The cotton fabric that will pad that treated in one of the embodiments, in 80 DEG C~100 DEG C preliminary drying 5min~20min, 2min~20min is baked at 120 DEG C~140 DEG C again.
The antibiotic finishing method of above-mentioned cotton fabric, has the advantage that
(1) antibiotic finishing method of above-mentioned cotton fabric is more able to satisfy actual needs, and different types of antibacterial agent is to same Kind pathogen has different Antibacterial mechanism and validity, and same antibacterial agent also has different resist for different pathogens Bacterium mechanism of action and inhibition range, can suitably increase nano-zinc oxide compound solution usage on the cotton fabric for having light to irradiate, The dosage of energy flexible modulation nano-zinc oxide compound solution and QAS polymer solution, local strengthening required for reaching Antibacterial effect, such antibiotic finish effect is more able to satisfy final use and actual needs, to more preferably meet the needs of client;
(2) above-mentioned zinc oxide-QAS polymer complex antimicrobials contain a large amount of carboxyl and epoxy group in molecular structure Group can have an effect when being applied to the final finishing of cotton fabric with the hydroxyl on cotton fiber, be formed compared with strong covalent bond, will be compound Antibacterial finishing agent is grafted on cotton fiber, to guarantee to obtain between finishing agent and fiber, binding strength is good, and wash resistant reaches lasting Antibiotic finish effect;
(3) in zinc oxide-QAS polymer complex antimicrobials, nano zine oxide dispersion is extremely uniform, and nanometer is not present The phenomenon that particle aggregation, can effectively play the antibacterial effect of nano zine oxide, the complex antimicrobials by quaternary ammonium salt cationic and The synergistic effect of nano zine oxide can give full play to the antibacterial effect of organic and inorganic materials, the good antibacterial of providing cotton fabric Performance.
It is illustrated below in conjunction with specific embodiment.
Following embodiment, such as non-specified otherwise, then do not include the unmentioned other components in addition to inevitable impurity.
Cotton fabric used in the following embodiment is 105g/m2Pure cotton knitting cloth (every piece weight 100g).
Embodiment 1
(1) preparation of nano-zinc oxide compound solution: by 1.0g nano zine oxide, 40g ethyl alcohol, 18g water and 4g γ-first Base acryloyloxypropyltrimethoxysilane is uniformly mixed, after ultrasonic disperse 1h, in 60 DEG C of water-bath back flow reaction 12h, then It is down to room temperature, product obtains active nano-ZnO by centrifuge separation and washing.4g ammonium persulfate is dissolved in 10g deionization In water, two parts are divided into, later by 4.0g active nano-ZnO, 50g deionized water, 12g acrylic acid, 4.0g allyl glycidyl Glycerin ether and 7g potassium persulfate solution are added in three-necked flask, are stirred evenly, and then heating water bath reacts 20min to 80 DEG C; 12g acrylic acid, 4.0g allyl glycidyl ether and 7g potassium persulfate solution are added dropwise again to be down to after insulated and stirred reacts 4.0h Room temperature is to get nano-zinc oxide compound solution.
(2) synthesis of QAS polymer solution: 3.5g ammonium persulfate is dissolved in 10g deionized water first, is divided into Three parts.Then by 30g dimethyl diallyl ammonium chloride, 53.2g deionized water, 0.9g acrylic acid, 0.2g allyl glycidyl are sweet Oily ether and 4.5g ammonium persulfate aqueous solution are added in three-necked flask, are stirred evenly, and then heating water bath is to 80 DEG C, reaction 15min;0.9g acrylic acid, 0.2g allyl glycidyl ether and 4.5g ammonium persulfate aqueous solution are added dropwise again, reacts 15min;Again Secondary dropwise addition 0.9g acrylic acid, 0.2g allyl glycidyl ether, 4.5g ammonium persulfate aqueous solution, after insulated and stirred reacts 4.0h, Room temperature is down to get QAS polymer solution.
Embodiment 2
(1) preparation of nano-zinc oxide compound solution: by 1.0g nano zine oxide, 40g ethyl alcohol, 18g water and 4g γ-first Base acryloyloxypropyltrimethoxysilane is uniformly mixed, after ultrasonic disperse 1h, in 60 DEG C of water-bath back flow reaction 12h, then It is down to room temperature, product obtains active nano-ZnO by centrifuge separation and washing.4g ammonium persulfate is dissolved in 10g deionization In water, two parts are divided into, later by 4.0g active nano-ZnO, 50g deionized water, 12g acrylic acid, 4.0g allyl glycidyl Glycerin ether and 7g potassium persulfate solution are added in three-necked flask, are stirred evenly, and then heating water bath reacts 20min to 80 DEG C; 12g acrylic acid, 4.0g allyl glycidyl ether and 7g potassium persulfate solution are added dropwise again to be down to after insulated and stirred reacts 4.0h Room temperature is to get nano-zinc oxide compound solution.
(2) synthesis of QAS polymer solution: 3.5g ammonium persulfate is dissolved in 10g deionized water first, is divided into Three parts.Then by 30g dimethyl diallyl ammonium chloride, 53.2g deionized water, 0.9g acrylic acid, 0.2g allyl glycidyl are sweet Oily ether and 4.5g ammonium persulfate aqueous solution are added in three-necked flask, are stirred evenly, and then heating water bath is to 80 DEG C, reaction 15min;0.9g acrylic acid, 0.2g allyl glycidyl ether and 4.5g ammonium persulfate aqueous solution are added dropwise again, reacts 15min;Again Secondary dropwise addition 0.9g acrylic acid, 0.2g allyl glycidyl ether, 4.5g ammonium persulfate aqueous solution, after insulated and stirred reacts 4.0h, Room temperature is down to get QAS polymer solution.
Embodiment 3
(1) preparation of nano-zinc oxide compound solution: by 1.0g nano zine oxide, 40g ethyl alcohol, 18g water and 4g γ-first Base acryloyloxypropyltrimethoxysilane is uniformly mixed, after ultrasonic disperse 1h, in 60 DEG C of water-bath back flow reaction 12h, then It is down to room temperature, product obtains active nano-ZnO by centrifuge separation and washing.4g ammonium persulfate is dissolved in 10g deionization In water, two parts are divided into, later by 4.0g active nano-ZnO, 50g deionized water, 12g acrylic acid, 4.0g allyl glycidyl Glycerin ether and 7g potassium persulfate solution are added in three-necked flask, are stirred evenly, and then heating water bath reacts 20min to 80 DEG C; 12g acrylic acid, 4.0g allyl glycidyl ether and 7g potassium persulfate solution are added dropwise again to be down to after insulated and stirred reacts 4.0h Room temperature is to get nano-zinc oxide compound solution.
(2) synthesis of QAS polymer solution: 3.5g ammonium persulfate is dissolved in 10g deionized water first, is divided into Three parts.Then by 30g dimethyl diallyl ammonium chloride, 53.2g deionized water, 0.9g acrylic acid, 0.2g allyl glycidyl are sweet Oily ether and 4.5g ammonium persulfate aqueous solution are added in three-necked flask, are stirred evenly, and then heating water bath is to 80 DEG C, reaction 15min;0.9g acrylic acid, 0.2g allyl glycidyl ether and 4.5g ammonium persulfate aqueous solution are added dropwise again, reacts 15min;Again Secondary dropwise addition 0.9g acrylic acid, 0.2g allyl glycidyl ether, 4.5g ammonium persulfate aqueous solution, after insulated and stirred reacts 4.0h, Room temperature is down to get QAS polymer solution.
Embodiment 4
(1) preparation of nano-zinc oxide compound solution: by 1.0g nano zine oxide, 40g ethyl alcohol, 18g water and 4g γ-first Base acryloyloxypropyltrimethoxysilane is uniformly mixed, after ultrasonic disperse 1h, in 60 DEG C of water-bath back flow reaction 12h, then It is down to room temperature, product obtains active nano-ZnO by centrifuge separation and washing.By 3.8g ammonium persulfate be dissolved in 10g go from Ammonium persulfate aqueous solution is obtained in sub- water, 1.2g sodium hydrogensulfite is dissolved in 10g deionized water to obtain sodium hydrogensulfite water-soluble Liquid, ammonium persulfate aqueous solution and aqueous solution of sodium bisulfite are respectively divided into two parts, later by 4.0g active nano-ZnO, 39g Deionized water, 12g acrylic acid, 4.0g allyl glycidyl ether, 6.9g ammonium persulfate are water-soluble and 5.6g sodium hydrogensulfite is water-soluble Liquid is added in three-necked flask, is stirred evenly, and then heating water bath reacts 20min to 80 DEG C;12g acrylic acid, 4.0g are added dropwise again Allyl glycidyl ether, 6.9g ammonium persulfate be water-soluble and 5.6g aqueous solution of sodium bisulfite, after insulated and stirred reacts 4.0h, drop To room temperature to get nano-zinc oxide compound solution.
(2) synthesis of QAS polymer solution: 3.5g ammonium persulfate is dissolved in 10g deionized water first, is divided into Three parts.Then by 30g dimethyl diallyl ammonium chloride, 53.2g deionized water, 0.9g acrylic acid, 0.2g allyl glycidyl are sweet Oily ether and 4.5g ammonium persulfate aqueous solution are added in three-necked flask, are stirred evenly, and then heating water bath is to 80 DEG C, reaction 15min;0.9g acrylic acid, 0.2g allyl glycidyl ether and 4.5g ammonium persulfate aqueous solution are added dropwise again, reacts 15min;Again Secondary dropwise addition 0.9g acrylic acid, 0.2g allyl glycidyl ether, 4.5g ammonium persulfate aqueous solution, after insulated and stirred reacts 4.0h, Room temperature is down to get QAS polymer solution.
Embodiment 5
(1) preparation of nano-zinc oxide compound solution: by 1.0g nano zine oxide, 40g ethyl alcohol, 18g water and 4g γ-first Base acryloyloxypropyltrimethoxysilane is uniformly mixed, after ultrasonic disperse 1h, in 60 DEG C of water-bath back flow reaction 12h, then It is down to room temperature, product obtains active nano-ZnO by centrifuge separation and washing.4g ammonium persulfate is dissolved in 10g deionization In water, two parts are divided into, later by 4.0g active nano-ZnO, 50g deionized water, 12g acrylic acid, 4.0g allyl glycidyl Glycerin ether and 7g potassium persulfate solution are added in three-necked flask, are stirred evenly, and then heating water bath reacts 20min to 80 DEG C; 12g acrylic acid, 4.0g allyl glycidyl ether and 7g potassium persulfate solution are added dropwise again to be down to after insulated and stirred reacts 4.0h Room temperature is to get nano-zinc oxide compound solution.
(2) synthesis of QAS polymer solution: 3.5g ammonium persulfate is dissolved in 10g deionized water first, is divided into Three parts.Then by 30g dimethyl diallyl ammonium chloride, 53.2g deionized water 0.8g methacrylic acid, 0.3g allyl glycidyl Glycerin ether and 4.5g ammonium persulfate aqueous solution are added in three-necked flask, are stirred evenly, and then heating water bath is to 80 DEG C, reaction 15min;0.9g acrylic acid, 0.2g allyl glycidyl ether and 4.5g ammonium persulfate aqueous solution are added dropwise again, reacts 15min;Again Secondary dropwise addition 0.9g acrylic acid, 0.2g allyl glycidyl ether, 4.5g ammonium persulfate aqueous solution, after insulated and stirred reacts 4.0h, Room temperature is down to get QAS polymer solution.
Embodiment 6
(1) preparation of nano-zinc oxide compound solution: by 1.0g nano zine oxide, 40g ethyl alcohol, 18g water and 4g γ-first Base acryloyloxypropyltrimethoxysilane is uniformly mixed, after ultrasonic disperse 1h, in 60 DEG C of water-bath back flow reaction 12h, then It is down to room temperature, product obtains active nano-ZnO by centrifuge separation and washing.4g ammonium persulfate is dissolved in 10g deionization In water, two parts are divided into, later by 4.0g active nano-ZnO, 50g deionized water, 10g methacrylic acid, 6.0g allyl Glycidol ether and 7g potassium persulfate solution are added in three-necked flask, are stirred evenly, and then heating water bath is to 80 DEG C, reaction 20min;12g acrylic acid, 4.0g allyl glycidyl ether and 7g potassium persulfate solution are added dropwise again, insulated and stirred reacts 4.0h Afterwards, room temperature is down to get nano-zinc oxide compound solution.
(2) synthesis of QAS polymer solution: 3.5g ammonium persulfate is dissolved in 10g deionized water first, is divided into Three parts.Then by 30g dimethyl diallyl ammonium chloride, 53.2g deionized water, 0.9g acrylic acid, 0.2g allyl glycidyl are sweet Oily ether and 4.5g ammonium persulfate aqueous solution are added in three-necked flask, are stirred evenly, and then heating water bath is to 80 DEG C, reaction 15min;0.9g acrylic acid, 0.2g allyl glycidyl ether and 4.5g ammonium persulfate aqueous solution are added dropwise again, reacts 15min;Again Secondary dropwise addition 0.9g acrylic acid, 0.2g allyl glycidyl ether, 4.5g ammonium persulfate aqueous solution, after insulated and stirred reacts 4.0h, Room temperature is down to get QAS polymer solution.
Embodiment 7
(1) preparation of nano-zinc oxide compound solution: by 1.0g nano zine oxide, 40g ethyl alcohol, 18g water and 4g γ-first Base acryloyloxypropyltrimethoxysilane is uniformly mixed, after ultrasonic disperse 1h, in 60 DEG C of water-bath back flow reaction 12h, then It is down to room temperature, product obtains active nano-ZnO by centrifuge separation and washing.4g ammonium persulfate is dissolved in 10g deionization In water, two parts are divided into, later by 4.0g active nano-ZnO, 50g deionized water, 12g acrylic acid, 4.0g allyl glycidyl Glycerin ether and 7g potassium persulfate solution are added in three-necked flask, are stirred evenly, and then heating water bath reacts 20min to 80 DEG C; 12g acrylic acid, 4.0g allyl glycidyl ether and 7g potassium persulfate solution are added dropwise again to be down to after insulated and stirred reacts 4.0h Room temperature is to get nano-zinc oxide compound solution.
(2) synthesis of QAS polymer solution: 4.1g ammonium persulfate is dissolved in 10g deionized water obtains over cure first 1.1g sodium hydrogensulfite is dissolved in 10g deionized water and obtains bisulfite aqueous ammonium by sour aqueous ammonium, by ammonium persulfate water Solution and bisulfite aqueous ammonium are divided into three parts respectively.Then by 30g dimethyl diallyl ammonium chloride, 41.5g go from Sub- water, 0.9g acrylic acid, 0.2g allyl glycidyl ether, 4.7g persulfate aqueous solution and 3.7g aqueous solution of sodium bisulfite It is added in three-necked flask, stirs evenly, then heating water bath reacts 15min to 80 DEG C;0.9g acrylic acid, 0.2g are added dropwise again Allyl glycidyl ether, 4.7g persulfate aqueous solution and 3.7g aqueous solution of sodium bisulfite react 15min;It is added dropwise again 0.9g acrylic acid, 0.2g allyl glycidyl ether, 4.7g persulfate aqueous solution and 3.7g aqueous solution of sodium bisulfite, heat preservation After being stirred to react 4.0h, room temperature is down to get QAS polymer solution.
Embodiment 8
(1) preparation of composite antibacterial finishing fluid: nano-zinc oxide compound solution and quaternary ammonium salt prepared by embodiment 1 are gathered Polymer solution is mixed to get zinc oxide-QAS polymer complex antimicrobials by weight 1:1, adds water and stirs uniformly, obtains The antibiotic finishing solution of 100g/L;
(2) leaching-baking of cotton fabric-roasting processing: cotton fabric is padded into processing in composite antibacterial finishing fluid, using two leachings two The mode rolled, padding pressure is 3kg/cm2, pick-up 80%.Then in 90 DEG C of preliminary drying 10min, then by cotton fabric at 130 DEG C Under bake 5min after, the cotton fabric (1# anti-bacteria cloth) after obtaining antibiotic finish.
Embodiment 9
(1) preparation of composite antibacterial finishing fluid: nano-zinc oxide compound solution and quaternary ammonium salt prepared by embodiment 1 are gathered Polymer solution is mixed to get zinc oxide-QAS polymer complex antimicrobials by weight 1:10, adds water and stirs uniformly, obtains The antibiotic finishing solution of 100g/L;
(2) leaching-baking of cotton fabric-roasting processing: cotton fabric is padded into processing in composite antibacterial finishing fluid, using two leachings two The mode rolled, padding pressure is 3kg/cm2, pick-up 80%.Then in 90 DEG C of preliminary drying 10min, then by cotton fabric at 130 DEG C Under bake 5min after, the cotton fabric (2# anti-bacteria cloth) after obtaining antibiotic finish.
Embodiment 10
(1) preparation of composite antibacterial finishing fluid: nano-zinc oxide compound solution and quaternary ammonium salt prepared by embodiment 1 are gathered Polymer solution is mixed to get zinc oxide-QAS polymer complex antimicrobials by weight 1:5, adds water and stirs uniformly, obtains The antibiotic finishing solution of 100g/L;
(2) leaching-baking of cotton fabric-roasting processing: cotton fabric is padded into processing in composite antibacterial finishing fluid, using two leachings two The mode rolled, padding pressure is 3kg/cm2, pick-up 80%.Then in 90 DEG C of preliminary drying 10min, then by cotton fabric at 130 DEG C Under bake 5min after, the cotton fabric (3# anti-bacteria cloth) after obtaining antibiotic finish.
Embodiment 11
(1) preparation of composite antibacterial finishing fluid: the nano-zinc oxide compound solution and quaternary ammonium salt that embodiment 2 will be prepared Polymer solution is mixed to get zinc oxide-QAS polymer complex antimicrobials by weight 1:5, adds water and stirs uniformly, obtains The antibiotic finishing solution of 500g/L;
(2) leaching-baking of cotton fabric-roasting processing: cotton fabric is padded into processing in composite antibacterial finishing fluid, using two leachings two The mode rolled, padding pressure is 3kg/cm2, pick-up 80%.Then in 85 DEG C of preliminary drying 15min, then by cotton fabric at 125 DEG C Under bake 15min after, the cotton fabric (4# anti-bacteria cloth) after obtaining antibiotic finish.
Embodiment 12
(1) preparation of composite antibacterial finishing fluid: nano-zinc oxide compound solution and quaternary ammonium salt prepared by embodiment 3 are gathered Polymer solution is mixed to get zinc oxide-QAS polymer complex antimicrobials by weight 1:5, adds water and stirs uniformly, obtains The antibiotic finishing solution of 100g/L;
(2) leaching-baking of cotton fabric-roasting processing: cotton fabric is padded into processing in composite antibacterial finishing fluid, using two leachings two The mode rolled, padding pressure is 3kg/cm2, pick-up 80%.Then in 95 DEG C of preliminary drying 7min, then by cotton fabric at 135 DEG C Under bake 3min after, the cotton fabric (5# anti-bacteria cloth) after obtaining antibiotic finish.
Embodiment 13
(1) preparation of composite antibacterial finishing fluid: nano-zinc oxide compound solution and quaternary ammonium salt prepared by embodiment 4 are gathered Polymer solution is mixed to get zinc oxide-QAS polymer complex antimicrobials by weight 1:5, adds water and stirs uniformly, obtains The antibiotic finishing solution of 200g/L;
(2) leaching-baking of cotton fabric-roasting processing: processing is padded in composite antibacterial finishing fluid, using the side of second dipping and rolling Formula, padding pressure is 3.5kg/cm2, pick-up 60%.Then in 85 DEG C of preliminary drying 15min, then cotton fabric roasted at 125 DEG C After drying 15min, the cotton fabric (6# anti-bacteria cloth) after obtaining antibiotic finish.
Identical pure cotton knitting cloth is compared without any processing as blank anti-bacteria cloth.
According to the National Standard of the People's Republic of China GB8629-2001 " home washings that are used when Textile Test and dry Dry program " regulation, Type B stirred type washing machine and washing procedure 8B are selected, respectively to 1#-6# anti-bacteria cloth, commercial antimicrobial cloth and not Processed pure cotton knitting cloth (blank anti-bacteria cloth) does carrying out washing treatment, and each sample is 10 times washed, 20 times, 50 times, measurement washing The anti-microbial property of sample afterwards.
According to National Standard of the People's Republic of China GB1759-2002 " Disposable Sanitary Accessory sanitary standard " product The anti-microbial property of sample after the test method measurement washing of anti-microbial property, test strain is bacterium: staphylococcus aureus (ATCC 6538), Escherichia coli (ATCC 25922), fungi: Candida albicans (ATCC 10231).Test result such as table 1:
Table 1
Note: bacteriostasis rate " * * * " represents>=99%, and " * * " represents>=90%, and " * " represents>=50%, and " -- " represents<50%.
By measurement result it is found that 1#-6# anti-bacteria cloth has good antibiotic property, good resist is able to maintain by repeatedly washing Bacterium property, it is seen that zinc oxide-QAS polymer complex antimicrobials and cotton fabric binding strength are good, and wash resistant is knitted using above-mentioned cotton The cotton fabric of object antibiotic finishing method processing can have long-term preferably antibacterial effect.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.

Claims (8)

1. a kind of antibiotic finishing method of cotton fabric, which comprises the following steps:
It prepares nano-zinc oxide compound solution: the first reaction raw materials is provided, first reaction raw materials contain according to quality percentage Meter includes: 1%~5% active nano-ZnO, 20%~30% carboxy acrylic class monomer, 5%~10% alkene Propyl glycidyl ether, 3%~6% the first initiator and water, the active nano-ZnO is that silane containing double bonds is even Join the modified nano zine oxide of agent, using the water as solvent, the active nano-ZnO, the carboxy acrylic class monomer and Polymerization reaction occurs under the initiation of first initiator and obtains nano-zinc oxide compound for the allyl glycidyl ether Solution, the silane coupling agent containing double bonds are γ-methacryloxypropyl trimethoxy silane, the active nano Zinc oxide is prepared by following steps: nano zine oxide, γ-methacryloxypropyl trimethoxy silane and solvent are mixed After conjunction, ultrasonic disperse obtains dispersion liquid;And active nano oxidation was obtained by the dispersion liquid back flow reaction 10 hours~20 hours The mass ratio of zinc, the nano zine oxide and the γ-methacryloxypropyl trimethoxy silane is 1:1~1:5;
It prepares QAS polymer solution: providing the second reaction raw materials, second reaction raw materials are according to mass percentage meter It include: 25%~35% dimethyl diallyl ammonium chloride, 1%~3% carboxy acrylic class monomer, 0.5%~1% Allyl glycidyl ether, 3%~6% the second initiator and water, using the water as solvent, the dimethyl diallyl chlorine Change ammonium, the carboxy acrylic class monomer and the allyl glycidyl ether to occur to gather under the initiation of second initiator It closes reaction and obtains QAS polymer solution;
The nano-zinc oxide compound solution and the QAS polymer solution are mixed to get zinc oxide-quaternary ammonium salt polymerization Object complex antimicrobials;
The zinc oxide-QAS polymer complex antimicrobials and water are mixed to get the antibacterial that concentration is 50g/L~500g/L Finishing fluid;
Cotton fabric is carried out using the antibiotic finishing solution to pad processing;And
To padding that treated, the cotton fabric is dried.
2. the antibiotic finishing method of cotton fabric according to claim 1, which is characterized in that the nano zine oxide is compound The mass ratio of object solution and the QAS polymer solution is that 1:1~1:10 is mixed to get the zinc oxide-quaternary ammonium salt polymerization Object complex antimicrobials.
3. the antibiotic finishing method of cotton fabric according to claim 1, which is characterized in that described to use the antibiotic finish Liquid carries out in the step of padding processing cotton fabric, is carried out by the way of second dipping and rolling, and the pressure for padding processing is 2kg/cm2~4kg/cm2, the pick-up for padding processing is 50%~90%.
4. the antibiotic finishing method of cotton fabric according to claim 1, which is characterized in that described pair of institute of padding that treated State in the withering step of cotton fabric, the cotton fabric that will pad that treated 80 DEG C~100 DEG C preliminary drying 5min~ 20min, then 2min~20min is baked at 120 DEG C~140 DEG C.
5. the antibiotic finishing method of cotton fabric according to claim 1, which is characterized in that the solvent include ethyl alcohol and Water, the matter of the nano zine oxide, the ethyl alcohol, the water and the γ-methacryloxypropyl trimethoxy silane Amount is than being 1:30~60:10~20:1~5.
6. the antibiotic finishing method of cotton fabric according to claim 1, which is characterized in that first initiator was selected from At least one of sodium sulphate, potassium peroxydisulfate and ammonium persulfate, or, first initiator includes sodium peroxydisulfate, potassium peroxydisulfate And at least one of ammonium persulfate and sodium hydrogensulfite;Second initiator is selected from sodium peroxydisulfate, potassium peroxydisulfate and over cure At least one of sour ammonium, or, second initiator includes at least one of sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate And sodium hydrogensulfite.
7. the antibiotic finishing method of cotton fabric according to claim 1, which is characterized in that it is described using the water as solvent, The active nano-ZnO, the carboxy acrylic class monomer and the allyl glycidyl ether are in first initiator Initiation under polymerization reaction the step of obtaining nano-zinc oxide compound solution occurs specifically:
By the active nano-ZnO, the water, the half of the carboxy acrylic class monomer, the allyl glycidyl The half of glycerin ether and the first initiator solution containing the half in first initiator are uniformly mixed, and are added Heat is stirred to react 15 minutes~20 minutes to 70 DEG C~85 DEG C and obtains mixed liquor;
By the half of the carboxy acrylic class monomer, the half of the allyl glycidyl ether and containing described First initiator solution of the half in the first initiator is added dropwise in the mixed liquor, is stirred at 70 DEG C~85 DEG C anti- It answers 3 hours~4.5 hours and obtains nano-zinc oxide compound solution.
8. the antibiotic finishing method of cotton fabric according to claim 1, which is characterized in that described using the water as solvent Dimethyl diallyl ammonium chloride, the carboxy acrylic class monomer and the allyl glycidyl ether cause described second The step of polymerization reaction obtains QAS polymer solution occurs under the initiation of agent specifically:
The dimethyl diallyl ammonium chloride, the water, second containing the one third in second initiator are drawn Send out agent aqueous solution, the one third in the allyl glycidyl ether and the one third in the carboxy acrylic class monomer It is heated to 70 DEG C~85 DEG C after mixing, is stirred to react 8 minutes~15 minutes and obtains the first reaction solution;
It will be in the second initiator solution containing the one third in second initiator, the allyl glycidyl ether One third and the carboxy acrylic class monomer in one third be added dropwise in first reaction solution, 70 DEG C~85 DEG C Under be stirred to react 10 minutes~20 minutes and obtain the second reaction solution;And
It will be in the second initiator solution containing the one third in second initiator, the allyl glycidyl ether One third and the carboxy acrylic class monomer in one third be added dropwise in second reaction solution, 70 DEG C~85 DEG C Under be stirred to react 3 hours~5 hours and obtain the QAS polymer solution.
CN201710597050.6A 2017-07-20 2017-07-20 The antibiotic finishing method of cotton fabric Active CN107287899B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710597050.6A CN107287899B (en) 2017-07-20 2017-07-20 The antibiotic finishing method of cotton fabric

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710597050.6A CN107287899B (en) 2017-07-20 2017-07-20 The antibiotic finishing method of cotton fabric

Publications (2)

Publication Number Publication Date
CN107287899A CN107287899A (en) 2017-10-24
CN107287899B true CN107287899B (en) 2019-08-13

Family

ID=60101963

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710597050.6A Active CN107287899B (en) 2017-07-20 2017-07-20 The antibiotic finishing method of cotton fabric

Country Status (1)

Country Link
CN (1) CN107287899B (en)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109680495A (en) * 2018-12-27 2019-04-26 中广核达胜加速器技术有限公司 A kind of preparation method and antibacterial fabric of nano particle antibacterial fabric
CN114680106B (en) * 2020-12-29 2022-09-20 中国科学院化学研究所 Antibacterial liquid, preparation method and application thereof, and antibacterial product
CN113832707A (en) * 2021-09-10 2021-12-24 宿迁金楠织造有限公司 Antibacterial light textile fabric and preparation method thereof
CN113638226B (en) * 2021-09-17 2024-04-02 四川华纺银华有限责任公司 Finishing method of antibacterial fiber, fiber and textile thereof
CN115839027B (en) * 2023-02-21 2023-04-14 汕头市富莱美服饰实业有限公司 Moisture-absorbing and breathable chemical fiber fabric containing fine denier polyester filaments and production process thereof
CN117107416B (en) * 2023-10-24 2024-01-12 广东欣薇尔服装有限公司 Fabric containing polyamide hollow fibers and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102787497A (en) * 2012-09-05 2012-11-21 陕西科技大学 Method for preparing novel quaternary ammonium salt copolymer/nanometer ZnO composite antimicrobial for fabric
CN103130957A (en) * 2013-03-15 2013-06-05 陕西科技大学 Method for preparing polymer/nano ZnO composite antimicrobial for textiles through in-situ polymerization method
CN104650290A (en) * 2015-02-05 2015-05-27 陕西科技大学 Polymer nano ZnO compound antibacterial agent for synthetic leathers based on in-situ polymerization process and preparation method of polymer nano ZnO compound antibacterial agent
CN105648745A (en) * 2016-04-01 2016-06-08 陕西科技大学 Polymer-based cerium-doped nano zinc oxide compound antibacterial agent for fabric and preparation method thereof
CN106283617A (en) * 2016-09-13 2017-01-04 陕西科技大学 Bafta polymer/Ag dopen Nano ZnO long acting antibiotic mildew-proofing finishing agent and preparation method thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101187276B1 (en) * 2010-06-29 2012-10-02 주식회사 삼광염직 Antibacterial Finish Of Polypropylene fabrics Using Cardanol Antibacterial-agents

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102787497A (en) * 2012-09-05 2012-11-21 陕西科技大学 Method for preparing novel quaternary ammonium salt copolymer/nanometer ZnO composite antimicrobial for fabric
CN103130957A (en) * 2013-03-15 2013-06-05 陕西科技大学 Method for preparing polymer/nano ZnO composite antimicrobial for textiles through in-situ polymerization method
CN104650290A (en) * 2015-02-05 2015-05-27 陕西科技大学 Polymer nano ZnO compound antibacterial agent for synthetic leathers based on in-situ polymerization process and preparation method of polymer nano ZnO compound antibacterial agent
CN105648745A (en) * 2016-04-01 2016-06-08 陕西科技大学 Polymer-based cerium-doped nano zinc oxide compound antibacterial agent for fabric and preparation method thereof
CN106283617A (en) * 2016-09-13 2017-01-04 陕西科技大学 Bafta polymer/Ag dopen Nano ZnO long acting antibiotic mildew-proofing finishing agent and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
纳米ZnO的表面改性研究;石振等;《上海涂料》;20080530;第46卷(第5期);第1-4页

Also Published As

Publication number Publication date
CN107287899A (en) 2017-10-24

Similar Documents

Publication Publication Date Title
CN107287899B (en) The antibiotic finishing method of cotton fabric
CN107401051B (en) Zinc oxide-QAS polymer complex antimicrobials and preparation method thereof
CN107287900B (en) The preparation method of composite antibacterial finishing agent
CN105648646B (en) Anti-mite antibacterial healthy knitted fabric of one kind and preparation method thereof
CN106565912A (en) Polyquaternium polymer emulsion antibacterial agent, preparation method thereof and application thereof
CN103130957B (en) Method for preparing polymer/nano ZnO composite antimicrobial for textiles through in-situ polymerization method
CN107419434B (en) A kind of preparation method of preservative free non-woven fabrics facial mask
CN107237122A (en) The durable antibiotic noniron finish liquid and finishing technique of a kind of cotton fabric
CN104727150A (en) Waterproof moisture-penetrable antibacterial anti-ultraviolet waterborne polyurethane material and preparation method thereof
EP2558637A2 (en) Antimicrobial treatment of synthetic nonwoven textiles
CN101349011A (en) High-efficiency antibiotic, anti-crease, anti-ultraviolet full cotton and polyester cotton special finishing method
CN1702232A (en) Preparation method for antibacterial and stinking-proof fabric
AU2020101333A4 (en) An ultraviolet-resistant and electromagnetic-radiation-resistant multifunctional textile preparation method
CN103924444A (en) Preparation method and application of hydrophilic anti-bacteria conditioner for fabric
CN109295706A (en) A kind of preparation method of antibacterial crease-resistant linen-cotton fabric
CN104172479A (en) Antibacterial underwear material
CN106592006B (en) A kind of Antistatic polyester cotton face fabric and preparation method thereof
CN105862417A (en) Novel antibacterial cotton fabric and preparation method thereof
CN107354715A (en) A kind of anti-sweat mark noniron finish liquid of the durable antibiotic of cotton fabric and finishing technique
CN110424160A (en) A kind of ready-made non-ironing garment three-prevention finishing method
CN112160155B (en) Flame-retardant antibacterial fabric
CN106702749A (en) Textile fabric surface modification treatment agent and preparation method thereof
CN106637950A (en) Finishing agent having function of reinforcing air permeability of textiles and preparation method of finishing agent
CN107663771A (en) A kind of fabric radiation agent and preparation method thereof
CN1710187B (en) Nano composite metal coated fabric and its preparing process

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant