CN108004775A - A kind of water-proof antibiotic finishing agent - Google Patents
A kind of water-proof antibiotic finishing agent Download PDFInfo
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- CN108004775A CN108004775A CN201711489674.2A CN201711489674A CN108004775A CN 108004775 A CN108004775 A CN 108004775A CN 201711489674 A CN201711489674 A CN 201711489674A CN 108004775 A CN108004775 A CN 108004775A
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- Prior art keywords
- parts
- water
- emulsion
- ammonium chloride
- finishing agent
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- 230000003115 biocidal effect Effects 0.000 title claims abstract description 17
- 239000000839 emulsion Substances 0.000 claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 239000003999 initiator Substances 0.000 claims abstract description 11
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 238000004945 emulsification Methods 0.000 claims abstract description 8
- 238000009413 insulation Methods 0.000 claims abstract description 8
- 239000000178 monomer Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000010792 warming Methods 0.000 claims abstract description 4
- -1 acrylyl oxy-ethyl-propyl group Chemical group 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 150000001252 acrylic acid derivatives Chemical class 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 6
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- IVKNZCBNXPYYKL-UHFFFAOYSA-N 2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[4-(2,4,4-trimethylpentan-2-yl)phenoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethanol Chemical compound CC(C)(C)CC(C)(C)C1=CC=C(OCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO)C=C1 IVKNZCBNXPYYKL-UHFFFAOYSA-N 0.000 claims description 3
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 3
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 3
- 239000012295 chemical reaction liquid Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 3
- 238000005292 vacuum distillation Methods 0.000 claims description 3
- 239000007822 coupling agent Substances 0.000 claims description 2
- PGQAXGHQYGXVDC-UHFFFAOYSA-N dodecyl(dimethyl)azanium;chloride Chemical compound Cl.CCCCCCCCCCCCN(C)C PGQAXGHQYGXVDC-UHFFFAOYSA-N 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims 3
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- HFBMWMNUJJDEQZ-UHFFFAOYSA-N acryloyl chloride Chemical class ClC(=O)C=C HFBMWMNUJJDEQZ-UHFFFAOYSA-N 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- 210000000481 breast Anatomy 0.000 claims 1
- 230000004048 modification Effects 0.000 claims 1
- 238000012986 modification Methods 0.000 claims 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims 1
- 150000004968 peroxymonosulfuric acids Chemical group 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 239000010936 titanium Substances 0.000 claims 1
- 239000004408 titanium dioxide Substances 0.000 claims 1
- 239000004753 textile Substances 0.000 description 12
- 230000000844 anti-bacterial effect Effects 0.000 description 9
- 239000004744 fabric Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 4
- 229920000742 Cotton Polymers 0.000 description 3
- DEQJNIVTRAWAMD-UHFFFAOYSA-N 1,1,2,4,4,4-hexafluorobutyl prop-2-enoate Chemical group FC(F)(F)CC(F)C(F)(F)OC(=O)C=C DEQJNIVTRAWAMD-UHFFFAOYSA-N 0.000 description 2
- BTERVQLEXBFOIO-UHFFFAOYSA-N C(C)O[SiH](OCC)OCC.C(C=C)(=O)OCCC[SiH2]OCC Chemical compound C(C)O[SiH](OCC)OCC.C(C=C)(=O)OCCC[SiH2]OCC BTERVQLEXBFOIO-UHFFFAOYSA-N 0.000 description 2
- FGSZZFKINHMRGG-UHFFFAOYSA-N CON(OC)OC.Cl Chemical compound CON(OC)OC.Cl FGSZZFKINHMRGG-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 description 2
- 230000000845 anti-microbial effect Effects 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
- 235000019394 potassium persulphate Nutrition 0.000 description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 210000000697 sensory organ Anatomy 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/356—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms
- D06M15/3568—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms containing silicon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
-
- 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
-
- 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
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention discloses a kind of water-proof antibiotic finishing agent, preparation method is：1) pre-emulsification, 100 parts of water, 12 parts of compound emulsifying agents, 64 parts of mix monomers are placed in emulsifier, and stirring, emulsification 30min, are made pre-emulsion；2) prepared by seed emulsion, 50 parts of water, 6 parts of compound emulsifying agents, 8 parts of surface-modified nano titanium dioxide are sequentially added in reaction kettle, stir evenly scattered, add the pre-emulsion of 1/3 volume, when being warming up to 75 DEG C, the solution of 0.2 part of initiator and 5 parts of water is added, insulation reaction 0.5h, obtains seed emulsion；3) complex emulsions react, in the remaining pre-emulsion of 2/3 volume of dropwise addition in 2h, the solution of 0.6 part of initiator and 15 parts of water, 4 parts of methacryloxypropyls, then heat to 82 DEG C, after continuing insulation reaction 2h, cooled to room temperature, filtering, agent emulsion is arranged up to water-proof antibiotic.
Description
Technical field
The present invention relates to a kind of textile function finishing agent, and in particular to a kind of water-proof antibiotic finishing agent, belongs to textile
Auxiliary agent field.
Background technology
With the continuous improvement of people's living standards, requirement of the people to functions of textile fabrics is more and more stronger, weaving face fabric
The comfort of the sense organs such as feel, appearance has not only been satisfied with, more focuses on the exploitation of functional product.Functional textile will be into
One step is expanded to fabric fields such as clothes, home textile, knitting, medical treatment, military project, style, environmental protection, space flight, and functional textile is opened
Hair is largely dependent upon the exploitation of textile function finishing agent and finishing technique.Textile function in present China market
Property finishing agent, it is either decontaminable or antifouling, antibacterial, anlistatig, be mostly the product of simple function, arrange
Technics comparing is complicated, it is desirable to which condition is harsh, and durability is poor, and applicable textile also has limitation.
The content of the invention
The object of the present invention is to provide a kind of water-proof antibiotic finishing agent, using emulsion polymerisation process, by waterproof, antibacterial monomer
It is graft-polymerized in nano-material surface, finishing agent is provided simultaneously with the functions such as good antibacterial, waterproof, UV resistance.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of water-proof antibiotic finishing agent, preparation method are：
1) pre-emulsification
100 parts of water, 12 parts of compound emulsifying agents, 64 parts of mix monomers are placed in emulsifier, stirring, emulsification 30min, are made
Pre-emulsion；
2) prepared by seed emulsion
50 parts of water, 6 parts of compound emulsifying agents, 8 parts of surface-modified nano titanium dioxide are sequentially added in reaction kettle, are stirred evenly
It is scattered, the pre-emulsion of 1/3 volume is added, when being warming up to 75 DEG C, adds the solution of 0.2 part of initiator and 5 parts of water, insulation is anti-
0.5h is answered, obtains seed emulsion；
3) complex emulsions react
In the remaining pre-emulsion of 2/3 volume of dropwise addition in 2h, the solution of 0.6 part of initiator and 15 parts of water, 4 parts of metering systems
Acryloxypropylethoxysilane triethoxysilane, then heats to 82 DEG C, after continuing insulation reaction 2h, cooled to room temperature, and filtering, i.e.,
Obtain water-proof antibiotic and arrange agent emulsion；
The mix monomer is by butyl acrylate, ethyl acrylate, fluorinated acrylate, acrylyl oxy-ethyl-propyl group
Trimethoxy silane-alkyl dimethyl ammonium chloride, methyl methacrylate, acrylic acid composition, mass ratio 15:3:5:4:4:1.
The preparation method of the acrylyl oxy-ethyl-propyl trimethoxy silicane-alkyl dimethyl ammonium chloride is：
Added in single-necked flask 1mol N, N- dimethylethanolamine, 1.05mol γ-r-chloropropyl trimethoxyl silane,
200mL acetonitriles, stirring, are slowly heated to 70 DEG C or so, after back flow reaction 36h, place reaction liquid into ice bath and cool down, to be crystallized
Separate out, filter, it is dry, white powder solid is obtained, i.e. propyl trimethoxy silicane-ethanol base-alkyl dimethyl ammonium chloride；
1mol propyl trimethoxy silicanes-ethanol base-alkyl dimethyl ammonium chloride, 1.1mol acryloyls are added in single-necked flask
Chlorine and a small amount of hydroquinone, 150mL ether, 5 DEG C of controlling reaction temperature, reacts 4h, after completion of the reaction, by the mixed liquor mistake in bottle
Filter, vacuum distillation remove unreacted reactant, obtain acrylyl oxy-ethyl-propyl trimethoxy silicane-alkyl dimethyl ammonium chloride.Reactional equation
Formula is as follows：
The preparation method of the surface-modified nano titanium dioxide is：Weigh 15 parts arrive equipped with 120mL absolute ethyl alcohols and
In the wide-mouth bottle of 40mL water, ultrasonic disperse 30min, pH value is adjusted to 6-6.5 with HCl, add 3 parts of coupling agent kh-570s with
9mL absolute ethyl alcohol mixed liquors, take out filtering, washing, obtained solid absolute ethyl alcohol soxhlet type 24h, then exists after reacting 2h
80 DEG C of vacuum drying chamber drying 12h, obtains surface-modified nano titanium dioxide.
The fluorinated acrylate is hexafluorobutyl acrylate, in acrylic acid trifluoro ethyl ester, dodecafluorhe-ptylacrylate
One kind.
The compound emulsifying agent is by methylacryoyloxyethyl trimethoxy ammonium chloride, dodecyl dimethyl chlorination
Ammonium, OP-10 compositions, mass ratio 3:1:2.
The initiator is potassium peroxydisulfate, one kind in ammonium persulfate, sodium peroxydisulfate.
The present invention arranges agent emulsion by acrylate, fluorinated acrylate, organic quaternary ammonium salt grafted nano titanium oxide shape
Into the functional finishing agent used for textiles with functional unifications such as waterproof, antibacterial, uvioresistants.Acryloyl-oxy with antibacterial functions
Ethyl-propyl trimethoxy silane-alkyl dimethyl ammonium chloride grafts on nano-titanium dioxide surface, forms inorganic-organic antibacterial and answers
Compound, had not only enhanced the dispersion stabilization of nano-titanium dioxide, but overcome organic quaternary ammonium salt as antiseptic chemistry it is steady
The defects of qualitative, poor heat resistance；Acrylyl oxy-ethyl-propyl trimethoxy silicane-alkyl dimethyl ammonium chloride can be with methacryl
Epoxide propyl-triethoxysilicane carries out cross-linking reaction by silicon-methoxyl group, enhances the fastness of high molecular polymer film forming.
Embodiment
Embodiment 1：
The preparation of acrylyl oxy-ethyl-propyl trimethoxy silicane-alkyl dimethyl ammonium chloride：
Added in single-necked flask 1mol N, N- dimethylethanolamine, 1.05mol γ-r-chloropropyl trimethoxyl silane,
200mL acetonitriles, stirring, are slowly heated to 70 DEG C or so, after back flow reaction 36h, place reaction liquid into ice bath and cool down, to be crystallized
Separate out, filter, it is dry, white powder solid is obtained, i.e. propyl trimethoxy silicane-ethanol base-alkyl dimethyl ammonium chloride；
1mol propyl trimethoxy silicanes-ethanol base-alkyl dimethyl ammonium chloride, 1.1mol acryloyls are added in single-necked flask
Chlorine and a small amount of hydroquinone, 150mL ether, 5 DEG C of controlling reaction temperature, reacts 4h, after completion of the reaction, by the mixed liquor mistake in bottle
Filter, vacuum distillation remove unreacted reactant, obtain acrylyl oxy-ethyl-propyl trimethoxy silicane-alkyl dimethyl ammonium chloride.
Embodiment 2：
A kind of water-proof antibiotic finishing agent, preparation method are：
1) pre-emulsification
100 parts of water, 12 parts of compound emulsifying agents, 64 parts of mix monomers are placed in emulsifier, stirring, emulsification 30min, are made
Pre-emulsion；
2) prepared by seed emulsion
50 parts of water, 6 parts of compound emulsifying agents, 8 parts of surface-modified nano titanium dioxide are sequentially added in reaction kettle, are stirred evenly
It is scattered, the pre-emulsion of 1/3 volume is added, when being warming up to 75 DEG C, adds the solution of 0.2 part of initiator and 5 parts of water, insulation is anti-
0.5h is answered, obtains seed emulsion；
3) complex emulsions react
In the remaining pre-emulsion of 2/3 volume of dropwise addition in 2h, the solution of 0.6 part of initiator and 15 parts of water, 4 parts of metering systems
Acryloxypropylethoxysilane triethoxysilane, then heats to 82 DEG C, after continuing insulation reaction 2h, cooled to room temperature, and filtering, i.e.,
Obtain water-proof antibiotic and arrange agent emulsion.
Wherein, mix monomer is by butyl acrylate, ethyl acrylate, fluorinated acrylate, acrylyl oxy-ethyl-propyl group three
Methoxy silane-alkyl dimethyl ammonium chloride, methyl methacrylate, acrylic acid composition, mass ratio 15:3:5:4:4:1；Composite Milk
Agent is made of methylacryoyloxyethyl trimethoxy ammonium chloride, dodecyl dimethyl ammonium chloride, OP-10, and mass ratio is
3:1:2；Fluorinated acrylate is hexafluorobutyl acrylate, acrylic acid trifluoro ethyl ester or dodecafluorhe-ptylacrylate；Initiator is
Potassium peroxydisulfate, ammonium persulfate or sodium peroxydisulfate.Application examples：
The arrangement agent emulsion of embodiment 2 is applied to by web surface by the method for final finishing
Antibacterial finishing agent in mass ratio:Water=3:50 proportional arrangement dressing liquid, is sufficiently stirred dissolving；By cotton fabric (40*
40/120*120) thorough impregnation impregnates 10 minutes, padding machine mangle in dressing liquid, pick-up rate 90-100%, 180 DEG C of drying.
Antibacterial, the water resistance of 1 cotton fabric of table
As shown in Table 1, cotton fabric has good waterproof, anti-microbial property.
Water resistance is pressed《The detection and evaluation of GB/T 4745-2012 textile water proof performances get wet method》Test.
Anti-microbial property is pressed《The evaluation third portion of GB/T 20944.3-2008 antibacterial textile performances:Succusion》Test.
Claims (6)
1. a kind of water-proof antibiotic finishing agent, preparation method are：
1) pre-emulsification
100 parts of water, 12 parts of compound emulsifying agents, 64 parts of mix monomers are placed in emulsifier, stirring, emulsification 30min, are made pre- breast
Change liquid；
2) prepared by seed emulsion
50 parts of water, 6 parts of compound emulsifying agents, 8 parts of surface-modified nano titanium dioxide are sequentially added in reaction kettle, are stirred evenly point
Dissipate, add the pre-emulsion of 1/3 volume, when being warming up to 75 DEG C, add the solution of 0.2 part of initiator and 5 parts of water, insulation reaction
0.5h, obtains seed emulsion；
3) complex emulsions react
In the remaining pre-emulsion of 2/3 volume of dropwise addition in 2h, the solution of 0.6 part of initiator and 15 parts of water, 4 parts of methacryloxypropyls
Base propyl-triethoxysilicane, then heats to 82 DEG C, after continuing insulation reaction 2h, cooled to room temperature, and filtering, up to anti-
Water antibiotic finish agent emulsion；
The mix monomer is by butyl acrylate, ethyl acrylate, fluorinated acrylate, acrylyl oxy-ethyl-propyl group front three
Oxysilane-alkyl dimethyl ammonium chloride, methyl methacrylate, acrylic acid composition, mass ratio 15:3:5:4:4:1.
A kind of 2. water-proof antibiotic finishing agent according to claim 1, it is characterised in that：The acrylyl oxy-ethyl-the third
The preparation method of base trimethoxy silane-alkyl dimethyl ammonium chloride is：
1mol N, N- dimethylethanolamine, 1.05mol γ-r-chloropropyl trimethoxyl silane, 200mL are added in single-necked flask
Acetonitrile, stirring, is slowly heated to 70 DEG C or so, after back flow reaction 36h, places reaction liquid into ice bath and cools down, precipitation to be crystallized,
Filter, it is dry, white powder solid is obtained, i.e. propyl trimethoxy silicane-ethanol base-alkyl dimethyl ammonium chloride；
Added in single-necked flask 1mol propyl trimethoxy silicanes-ethanol base-alkyl dimethyl ammonium chloride, 1.1mol acryloyl chlorides and
A small amount of hydroquinone, 150mL ether, 5 DEG C of controlling reaction temperature, reacts 4h, and after completion of the reaction, the mixed liquor in bottle is filtered,
Vacuum distillation removes unreacted reactant, obtains acrylyl oxy-ethyl-propyl trimethoxy silicane-alkyl dimethyl ammonium chloride.
A kind of 3. water-proof antibiotic finishing agent according to claim 1, it is characterised in that：The surface-modified nano titanium dioxide
The preparation method of titanium is：15 parts are weighed into the wide-mouth bottle equipped with 120mL absolute ethyl alcohols and 40mL water, ultrasonic disperse 30min, is used
HCl adjusts pH value to 6-6.5, adds 3 parts of coupling agent kh-570s and 9mL absolute ethyl alcohol mixed liquors, react take out after 2h filter,
Washing, obtained solid absolute ethyl alcohol soxhlet type 24h, then in 80 DEG C of vacuum drying chamber drying 12h, obtains surface modification and receives
Rice titanium dioxide.
A kind of 4. water-proof antibiotic finishing agent according to claim 1, it is characterised in that：The fluorinated acrylate is third
One kind in olefin(e) acid hexafluoro butyl ester, acrylic acid trifluoro ethyl ester, dodecafluorhe-ptylacrylate.
A kind of 5. water-proof antibiotic finishing agent according to claim 1, it is characterised in that：The compound emulsifying agent is by methyl
Acrylyl oxy-ethyl trimethoxy ammonium chloride, dodecyl dimethyl ammonium chloride, OP-10 compositions, mass ratio 3:1:2.
A kind of 6. water-proof antibiotic finishing agent according to claim 1, it is characterised in that：The initiator is persulfuric acid
One kind in potassium, ammonium persulfate, sodium peroxydisulfate.
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| CN115160486A (en) * | 2022-07-29 | 2022-10-11 | 同济大学 | Antibacterial fluorine-containing emulsifier and preparation method thereof |
| CN116695426A (en) * | 2023-05-10 | 2023-09-05 | 吴江市涂泰克纺织后整理有限公司 | Wear-resistant organic-inorganic multielement synergistic flame-retardant fabric and preparation method thereof |
| CN118441397A (en) * | 2024-05-27 | 2024-08-06 | 武汉爱帝针纺实业有限公司 | Ultraviolet-resistant breathable polyester fiber fabric and preparation method thereof |
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| CN102516477A (en) * | 2011-11-23 | 2012-06-27 | 华南理工大学 | Nano titanium dioxide/ acrylate composite emulsion and preparation method thereof |
| CN106479303A (en) * | 2016-08-31 | 2017-03-08 | 秦瑶 | A kind of water-proof antibiotic coating |
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| CN118441397A (en) * | 2024-05-27 | 2024-08-06 | 武汉爱帝针纺实业有限公司 | Ultraviolet-resistant breathable polyester fiber fabric and preparation method thereof |
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