CN111074538B - Multifunctional finishing auxiliary agent and preparation method and application thereof - Google Patents
Multifunctional finishing auxiliary agent and preparation method and application thereof Download PDFInfo
- Publication number
- CN111074538B CN111074538B CN201911279934.2A CN201911279934A CN111074538B CN 111074538 B CN111074538 B CN 111074538B CN 201911279934 A CN201911279934 A CN 201911279934A CN 111074538 B CN111074538 B CN 111074538B
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- Prior art keywords
- emulsion
- fabric
- finishing
- dosage
- titanium dioxide
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- 239000012752 auxiliary agent Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 239000004744 fabric Substances 0.000 claims abstract description 82
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000000839 emulsion Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 27
- 230000001804 emulsifying effect Effects 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 27
- 239000010936 titanium Substances 0.000 claims description 18
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 15
- 239000003999 initiator Substances 0.000 claims description 15
- 239000002243 precursor Substances 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 14
- 229910052719 titanium Inorganic materials 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 12
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 11
- 239000000178 monomer Substances 0.000 claims description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 239000004530 micro-emulsion Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000004094 surface-active agent Substances 0.000 claims description 10
- 238000005096 rolling process Methods 0.000 claims description 9
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 8
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 7
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 230000003197 catalytic effect Effects 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
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- 150000002829 nitrogen Chemical class 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 239000004064 cosurfactant Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 238000002390 rotary evaporation Methods 0.000 claims description 5
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- QUVMSYUGOKEMPX-UHFFFAOYSA-N 2-methylpropan-1-olate;titanium(4+) Chemical compound [Ti+4].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-] QUVMSYUGOKEMPX-UHFFFAOYSA-N 0.000 claims description 4
- URDOJQUSEUXVRP-UHFFFAOYSA-N 3-triethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CCO[Si](OCC)(OCC)CCCOC(=O)C(C)=C URDOJQUSEUXVRP-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
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- 238000007598 dipping method Methods 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 4
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 3
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 3
- MUHFRORXWCGZGE-KTKRTIGZSA-N 2-hydroxyethyl (z)-octadec-9-enoate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCCO MUHFRORXWCGZGE-KTKRTIGZSA-N 0.000 claims description 2
- SYBYTAAJFKOIEJ-UHFFFAOYSA-N 3-Methylbutan-2-one Chemical compound CC(C)C(C)=O SYBYTAAJFKOIEJ-UHFFFAOYSA-N 0.000 claims description 2
- CDOUZKKFHVEKRI-UHFFFAOYSA-N 3-bromo-n-[(prop-2-enoylamino)methyl]propanamide Chemical compound BrCCC(=O)NCNC(=O)C=C CDOUZKKFHVEKRI-UHFFFAOYSA-N 0.000 claims description 2
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 claims description 2
- KEZMLECYELSZDC-UHFFFAOYSA-N 3-chloropropyl-diethoxy-methylsilane Chemical compound CCO[Si](C)(OCC)CCCCl KEZMLECYELSZDC-UHFFFAOYSA-N 0.000 claims description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- LWZFANDGMFTDAV-BURFUSLBSA-N [(2r)-2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O LWZFANDGMFTDAV-BURFUSLBSA-N 0.000 claims description 2
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- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- ZRHOFLXFAAEXEE-UHFFFAOYSA-J butanoate;titanium(4+) Chemical compound [Ti+4].CCCC([O-])=O.CCCC([O-])=O.CCCC([O-])=O.CCCC([O-])=O ZRHOFLXFAAEXEE-UHFFFAOYSA-J 0.000 claims description 2
- 235000019329 dioctyl sodium sulphosuccinate Nutrition 0.000 claims description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
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- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 2
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- UDUKMRHNZZLJRB-UHFFFAOYSA-N triethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OCC)(OCC)OCC)CCC2OC21 UDUKMRHNZZLJRB-UHFFFAOYSA-N 0.000 claims description 2
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
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Abstract
The invention relates to a multifunctional finishing auxiliary agent, a preparation method and application thereof, wherein the auxiliary agent is hydrophobically modified nitrogen-doped titanium dioxide. The preparation process comprises the steps of preparing titanium dioxide nano particles by adopting a shah micro-emulsion method, then carrying out nitrogen doping and hydrophobic modification on titanium dioxide, and finally emulsifying the prepared modified titanium dioxide to obtain emulsion. The invention can endow the fabric with the water resistance, ultraviolet resistance and light response directional moisture conduction versatility, improves the wearing comfort, has good composite function after finishing the garment fabrics with different fiber components and different organizational structures, and has universal applicability.
Description
Technical Field
The invention belongs to the field of intelligent textile fabrics, and particularly relates to a multifunctional finishing auxiliary agent, and a preparation method and application thereof.
Background
The wearing comfort of the textile is the first requirement of people on the garment fabric, and the damp-heat comfort of the textile fabric is the most important factor influencing the wearing comfort of the garment. The fabric with the damp-heat comfort function comprises a waterproof moisture-permeable function and a directional moisture-conducting quick-drying function.
The waterproof and moisture permeable function is widely used as a fabric protection technology. The waterproof fabric is prepared by using a waterproof agent in a post-finishing process, wherein the waterproof agent comprises two types of acrylate fluorine-containing waterproof agents and fluorine-free waterproof agents. Among them, fluorocarbon compounds have the best water repellent effect, but the C8 water repellent is banned by countries such as Europe and America because it contains potential carcinogenic substances such as perfluorooctanoic acid (PFOA) and perfluorooctane sulfonyl compound (PFOS) and brings harm to human health and environment. Therefore, the development of new environment-friendly C6, C4 and fluorine-free finishing technologies becomes a research hotspot of water repellent finishing at present.
The directional moisture-conducting and quick-drying function is applied to summer clothing and sportswear fabrics as a technology for improving the heat and humidity comfort of textile wearing. When people exercise vigorously or are in a sultry and humid environment, a high-temperature and high-humidity environment is formed on the surface of the skin due to a large amount of sweating of a human body, so that clothes are adhered to the skin, a wearer feels sultry, even bacteria are bred, and the health of people is harmed. At present, two methods are commonly used for realizing the directional moisture-conducting function of the fabric, one method is the design of the fabric structure, and the additional pressure difference is formed between the inner side and the outer side of the fabric by interweaving warp yarns and weft yarns with different hydrophilicity and hydrophobicity, so that the directional moisture conduction is realized. According to the method, the inner layer fiber is made of hydrophobic yarn, polypropylene fiber is commonly used, the outer layer is made of fibers such as polyester or cotton, the one-way moisture-conducting effect can be achieved, but the polypropylene fiber is poor in dyeing property and incomplete in color spectrum, the color is limited when the polypropylene fiber is blended with other fibers, the polypropylene fiber is hard in hand feeling, high temperature resistance and ironing resistance are avoided, and therefore low temperature is suitable for post-finishing, drying and shaping, and production efficiency is affected. Meanwhile, the chemical fiber is difficult to meet the requirements of consumers on the comfort and natural environment protection of clothes. Another method is to finish the fabric in post-finishing to make one side of the fabric discontinuous hydrophobic and the other side hydrophilic, and form directional moisture conduction under the action of wettability gradient. At present, the method mainly aims at natural fibers, such as cotton and the like. The function is mainly used for sportswear and summer clothing, the fabric is light and thin, the hydrophilic and hydrophobic finishing agents are easy to permeate and contact at critical positions during finishing, the moisture-conducting effect is damaged, and the operation difficulty is high.
Patent CN208403362U has represented this kind of research that adopts the blending method of interweaving to prepare one-way moisture guide fabric, discloses one-way moisture guide fabric, and for double-deck two-sided mesh structure, the face next to the shin is the hydrophobic layer, and the top layer is hydrophilic layer, and this patent adopts polypropylene fibre and Coolmax polyester fiber blending, combines the mode of waterproof arrangement to prepare one-way moisture guide fabric simultaneously, and this surface fabric uses the chemical fibre to be given first place to and be double-deck surface fabric, and gram is great, and thickness is big, wears to influence human heat dissipation summer.
Patent CN101962885B represents the research of adopting the second preparation method of unidirectional moisture-conducting fabric, and discloses a method for preparing fabric with unidirectional moisture-conducting function, which comprises the steps of performing hydrophilization pretreatment on fabric, and then performing single-side spraying processing on the treated fabric by using working solution of water-repellent finishing agent to form discontinuous water-repellent surface, thereby obtaining the fabric with unidirectional moisture-conducting function.
At present, some reports report that the fabric has two functions which are combined to better improve the damp-heat comfort, but the technical routes adopted by different researchers are different.
Patent CN103821000B reports that a form that passes through the printing respectively inside and outside the hydrophilic surface fabric prints the waterproof pattern of different hydrophilic and hydrophobic areas, realizes the one-way wet guide of garment materials to form waterproof performance on the surface, have waterproof grease proofing antifouling function, provide quick sweat releasing mechanism for human motion sweat, provide dry and comfortable body surface environment. The fabric on the outer surface of the technical scheme of the patent only achieves partial water resistance, and the water-proof area is 50-80%.
The research of Lihuizian and the like is reported in No. 35 and No. 1 of Tianjin university of Industrial science, and the literature shows that titanium dioxide sol is prepared by using butyl titanate as a precursor through a sol-gel method, cotton and viscose fabrics are finished, contact angles after finishing are 135 degrees and 139 degrees, the contact angle is reduced to zero after the cotton and the viscose fabrics are irradiated by ultraviolet rays for 2 hours, and the unidirectional moisture-conducting capacity can be realized. However, the report also indicates that the fabric cannot meet the requirements of practical use because of its slow wettability switching speed. Meanwhile, the hydrophobic contact angle of 130-140 degrees reported in the document cannot achieve the super-hydrophobic effect, and the hydrophobic effect is poor. Meanwhile, the processing mode of the fabric adopts an organic solvent to directly pad the target fabric, and the difficulties of VOC pollution, processing cost, inflammable finishing agent and the like which are difficult to apply industrially exist.
The harm of ultraviolet radiation arouses people's attention more and more, and the mechanism of action of anti ultraviolet fabrics has two kinds: absorption and reflection, and accordingly there are two main approaches to uv protection: one is an anti-ultraviolet product obtained by increasing the reflection and scattering of ultraviolet rays by textiles, which is called an ultraviolet screening agent; another product that increases the uv absorption of textiles is uv absorbers. The absorbent and the shielding agent can be used alone or in combination.
The multifunctional composite finishing of the textile enables the textile to develop towards higher grade. At present, the traditional means of complex function finishing is mainly to realize different functions by carrying out one-bath treatment or step-by-step padding on a plurality of auxiliary agents through function finishing. Therefore, in the multifunctional composite finishing, the mutual contradiction between different functions and the influence of many factors such as the coordination compounding and compatibility among the auxiliary agents, the process and the like are considered, and the different functional effects of the composite functional finishing can be influenced mutually due to the compounding. The waterproof finishing is the compounding of waterproof finishing and other functions, the waterproof principle is that the surface of the fabric is covered by a high polymer with low surface tension to prevent wetting of water and other liquids, the hydrophobic chain segments with low surface energy are required to be vertically and tightly arranged on the outermost layer of the fabric to obtain the best waterproof effect, and when other functions are compounded, film forming of other finishing agents and arrangement of the hydrophobic chain segments of the waterproof agent on the surface of the fabric form a competition and a covering relation, so that the waterproof effect is greatly influenced.
The three functions of water resistance, directional moisture conduction and ultraviolet resistance are greatly helpful for improving the wearing comfort of damp and heat and protecting human bodies on summer clothing and sports clothing, but research reports and clothing sales integrating the three functions are difficult to find at present.
Patent CN101768854A discloses a method for preparing super-hydrophobic and ultraviolet-resistant cotton fabric by using titanium dioxide and a fluorine-free waterproof agent, and adopts the technical scheme that the method comprises two steps, namely, the prepared titanium dioxide sol is used for ultraviolet-resistant finishing, and then the waterproof agent is used for hydrophobic finishing. According to the method, the ethanol sol is used for finishing the cotton fabric, and the ethanol is used for replacing water as the sol for dissolving titanium dioxide, so that the problems of VOC pollution, cost, flammability and the like exist in the processing process, the method cannot realize industrial application at all from any angle, and the fluorine-free hydrophobic finishing is carried out on the cotton fabric finished by using the titanium dioxide, so that the hydrophobic property is greatly influenced. The combination of the ultraviolet resistance function and the super-hydrophobic function can not be realized.
TiO 2 The material is an inorganic nano semiconductor material with wide forbidden band, and has stable property, no toxicity and high-efficiency photocatalytic activity, so that the material is widely applied to the fields of photocatalytic degradation of printing and dyeing wastewater, degradation of waste gas pollutants, antibiosis, deodorization, ultraviolet ray prevention, addition of additives, self-cleaning and the like in the textile field. However, because the band gap of titanium dioxide is wide and the response to visible light is weak, ion doping is an effective way for improving the photocatalytic activity of titanium dioxide in the visible light region.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a finishing auxiliary agent with waterproof, ultraviolet-resistant and light-responsive directional moisture-conducting functions, the difficulty that the three functions are mutually influenced and cannot obtain good functional effects when finishing is carried out by compounding the auxiliary agent is solved, and the wearing comfort of summer clothes and sports clothes is improved.
The invention provides a multifunctional finishing auxiliary agent, which is hydrophobically modified nitrogen-doped titanium dioxide.
The invention provides a preparation method of a multifunctional finishing auxiliary agent, which comprises the following steps:
(1) uniformly mixing a surfactant, a cosurfactant, an oil phase and a modified monomer at room temperature, adding deionized water with the mass fraction of 5-15% into the mixed solution, and stirring until a transparent and uniform micro-emulsion is formed, wherein the micro-emulsion is recorded as emulsion A;
(2) mixing the titanium source precursor, the catalytic acid and the modified nitrogen source at room temperature, uniformly stirring, and recording as a solution B;
(3) dripping the solution B into the emulsion A at a speed of 1-5g/min, and introducing N after the addition is finished 2 Protecting, heating to 40-90 ℃, stirring for 5-30min, adding an initiator and a silane coupling agent (dropwise adding is completed within 0.5-2h under the control of the adding speed), reacting for 1-10h under heat preservation, cooling to room temperature, adjusting the pH to be neutral, taking out a reactant, adding pure water, removing the solvent, adding a surfactant, stirring and emulsifying to obtain the hydrophobically modified nitrogen-doped titanium dioxide emulsion.
The surfactant in the step (1) is one of dioctyl sodium sulfosuccinate, sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, dodecyl trimethyl ammonium bromide DTAB, cetyl trimethyl ammonium bromide CTAB, fatty alcohol-polyoxyethylene ether, span 20 and polyethylene glycol monooleate, and the dosage is 1-10% by mass fraction.
The cosurfactant in the step (1) is one of acetone, methyl butanone, methyl isobutyl ketone, butanone, ethyl acetate, n-hexanol, ethanol, ethylene glycol, n-propanol and isopropanol, and the dosage is 1-10% by mass.
The oil phase in the step (1) is one or two of n-heptane, n-hexane, cyclohexane, n-pentane and liquid paraffin, and the dosage is 5-30% by mass.
The modified monomer in the step (1) is one or two of acrylate monomer, organic siloxane and fluorine-containing acrylate monomer, and the using amount is 0.5-5% by mass fraction.
The titanium source precursor in the step (2) is one of titanium butyrate, titanium tetrachloride, tetraisobutyl titanate and tetraisopropyl titanate, and the dosage of the titanium source precursor is 5-25% of the total amount of the emulsion A by mass fraction.
The catalytic acid in the step (2) is one of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, oxalic acid, acetic acid and oxalic acid, and the dosage of the catalytic acid is 0.01-0.5% of the total amount of the emulsion A by mass fraction.
The modified nitrogen source in the step (2) is one of triethylamine, urea and thiourea, and the using amount of the modified nitrogen source is 1-10% of that of the titanium source precursor by mass fraction.
The initiator in the step (3) is one or more of a sulfate initiator, an azo initiator (such as AIBN) and a redox initiator, and the dosage of the initiator is 0.1 to 0.5 percent of the total weight of the modified monomer by mass fraction.
The silane coupling agent in the step (3) is one or more of 3-aminopropyltriethoxysilane KH550, 3-chloropropylmethyldiethoxysilane, 3-chloropropyltriethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltriethoxysilane, vinyltriethoxysilane KH151 and 3- (methacryloyloxy) propyltriethoxysilane KH-570, and the using amount of the silane coupling agent is 0.05-0.5% of that of the titanium source precursor by mass fraction.
The invention provides an application of a multifunctional finishing auxiliary agent, which comprises the following specific steps:
applying the multifunctional finishing auxiliary agent to the prepared fabric by one-dipping one-rolling or two-dipping one-rolling, and then carrying out high-temperature baking on the fabric by a setting machine; wherein the liquid carrying rate is controlled to be 20-100%, the concentration of the auxiliary agent is 10-100 g/L, the drying temperature of the setting machine is controlled to be 100-180 ℃, and the vehicle speed is 10-60 m/min.
The fabric can be a knitted fabric woven by natural fibers (cotton, hemp, silk fibers and the like), chemical fibers (including terylene, chinlon, acrylic fibers, regenerated cellulose fibers and the like), a knitted fabric woven by the blended fibers (such as terylene/cotton blended fabric, chinlon/cotton blended fabric, terylene/nylon blended fabric and the like) and a woven fabric.
According to the selected fabrics with different components, the fabric is subjected to desizing, scouring and bleaching pretreatment, dyeing, full washing, dehydration and drying for later use according to the conventional preparation process.
The invention adopts a microemulsion method to treat TiO 2 The N doping is carried out to improve the response capability of the material to visible light, and meanwhile, the hydrophobic modification is carried out to improve the prepared materialThe water emulsion can be directly used in the textile printing and dyeing after-finishing process, and the method for preparing the intelligent fabric with the waterproof, directional moisture-conducting and ultraviolet-resistant composite functions by utilizing the material in the textile after-finishing stage is realized.
The fabric treated by the method has the functions of ultraviolet resistance and water resistance, and when the fabric is irradiated by sunlight for a certain time in the outdoor wearing process, the surface of the fabric becomes hydrophilic under the stimulation of light by the surface-modified titanium dioxide, so that the garment has the function of directional moisture conduction. In the finishing process of the fabric, the high-temperature shaping action enables unreacted hydroxyl connected to Ti atoms to generate self-polycondensation and react with reactive groups on the surface of the fiber, hydrophilic groups are sealed, and the grafted and modified hydrophobic acrylate or siloxane groups have combined action to form a hydrophobic structure on the surface of the fabric. Meanwhile, the acrylate partially undergoes polycondensation film forming reaction, so that the washing resistance effect is improved. When the fabric is illuminated, TiO 2 Electrons in the valence band are excited to the conduction band, electron holes are generated in the valence band, and the photogenerated electrons and holes migrate to the surface where they are trapped in the TiO 2 The surface generates electron-hole pairs. Electrons and Ti 4+ Reacting, the cavity reacts with other cations on the surface of the material to respectively form Ti 3+ And oxygen vacancies. The hydrolytic ions in the air are adsorbed in the oxygen vacancies to form chemically adsorbed water, and the chemically adsorbed water further adsorbs the moisture in the air and is in the Ti 3+ Hydrophilic micro-areas are formed around the surface, and the dropped water drops are adsorbed by the hydrophilic micro-areas to wet the surface. After the light irradiation is stopped, the chemisorbed hydroxyl groups are replaced by oxygen in the air, and the hydrophobic state is recovered. The change in wettability of the fabric is a gradual transition and is not instantaneous.
Advantageous effects
(1) The fabric can be endowed with the water resistance, ultraviolet resistance and directional moisture conduction versatility, and the wearing comfort is improved;
(2) the titanium dioxide prepared by the invention exists in the form of emulsion, so that the application of after-finishing of textiles is facilitated, the hydrophobic modification is carried out on the titanium dioxide, the hydrophobic property is improved, meanwhile, the utilization rate of the titanium dioxide to visible light is enhanced by doping N element, the ultraviolet resistance function is enhanced, and the response time of the material to the light is greatly shortened, so that the wettability change of the finished fabric can be realized in a short time when the finished fabric is irradiated by sunlight;
(3) the invention solves the difficulty that three functions of water resistance, ultraviolet resistance and directional moisture conduction are mutually influenced when finishing by compounding the auxiliary agent, and a good functional effect cannot be obtained;
(4) the invention has good composite function after finishing the garment materials with different fiber components and different organizational structures, and has universal applicability.
Drawings
FIG. 1 is a graph showing the change of contact angle of a finished fabric with illumination time under illumination conditions.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
The preparation method of the hydrophobic modified nitrogen-doped titanium dioxide emulsion functional finishing auxiliary agent comprises the following steps:
(1) adding dodecyl trimethyl ammonium bromide DTAB, n-hexanol, n-hexane, hexafluorobutyl acrylate and hydroxyethyl methacrylate into a reaction beaker at room temperature according to the mass ratio of 3%, 4%, 25%, 3% and 0.5%, respectively, starting stirring to mix uniformly, slowly adding deionized water with the mass fraction of 7% into the mixed solution, violently stirring until a transparent and uniform micro-emulsion is formed, and weaving the micro-emulsion into emulsion A.
(2) Respectively mixing titanium source precursor butyl titanate and nitric acid (36%) by mass percent of 20% and 0.8% of the total amount of the emulsion A, adding triethylamine with the amount of 1% of the butyl titanate, uniformly stirring and weaving the solution into a solution B.
(3) Transferring the emulsion A into a three-neck flask reaction kettle, slowly dripping the solution B into the emulsion A at the speed of 5mL/min by using a syringe pump, and continuously stirring. Introducing N after the addition is finished 2 Protecting and heating to 70 ℃, stirring for 20min, adding 0.1% of initiator azobisisobutyronitrile and 0.3% of silane coupling agent 3- (methacryloyloxy) propyltriethoxysilane KH-570 (the adding speed is controlled to be within 1.5h, dropwise adding), keeping the temperature for reaction for 6h, then cooling to room temperature, dropwise adding ammonia water to adjust the pH to be neutral, taking out the reactant, adding pure water, removing the solvent by rotary evaporation on a rotary evaporator, adding 0.4% DTAB, stirring at high speed and emulsifying to obtain the hydrophobic modified N-titanium dioxide emulsion.
The selection specification is 180g/m 2 The 40S all-cotton combed single-sided single jersey gray fabric is subjected to desizing and scouring bleaching pretreatment for 30-45min on equipment according to a conventional preparation process at a bath ratio of 1:10, is dyed by reactive dye according to required colors, the water bath temperature is controlled to be 55-60 ℃, the heat preservation time is 45-60min, after the color fixation of soda, the fabric is fully washed before being taken out of a cylinder to ensure the subsequent function finishing effect, the fabric is subjected to one-dipping-one-rolling after scutching and drying, the concentration of a titanium dioxide nano function finishing agent is 60g/L, 10g/L of a polyurethane cross-linking agent is added at the same time, the padder pressure of a setting machine is 3kg, the drying temperature is 170 ℃, and the vehicle speed is 30 m/min. The fabric is irradiated by sunlight for a certain time in the outdoor wearing process, and the surface of the fabric becomes hydrophilic under the stimulation of light by the surface modified titanium dioxide, so that the garment has the function of directional moisture conduction.
Example 2
The preparation method of the hydrophobic modified nitrogen-doped titanium dioxide emulsion functional finishing auxiliary agent comprises the following steps:
(1) adding sodium dodecyl benzene sulfonate, n-hexanol, n-heptane, octadecyl methacrylate and hydroxyethyl methacrylate into a reaction beaker according to the mass ratio of 4%, 20%, 4% and 0.5% respectively at room temperature, starting stirring simultaneously to mix uniformly, slowly adding deionized water with the mass fraction of 10% into the mixed solution, stirring vigorously until a transparent and uniform micro-emulsion is formed, and weaving the micro-emulsion into emulsion A.
(2) Respectively mixing titanium tetrachloride serving as a titanium source precursor and hydrochloric acid (20%) by mass percent to 20% and 0.3% of the total amount of the emulsion A, adding urea with the amount of 2% of the titanium tetrachloride, and uniformly stirring to obtain a solution B.
(3) Transferring the emulsion A into a three-neck flask reaction kettle, slowly dripping the solution B into the emulsion A at the speed of 2mL/min by using a syringe pump, and continuously stirring. Introducing N after the addition is finished 2 Protecting and heating to 70 ℃, stirring for 20min, adding 0.4% of initiator ammonium persulfate and 0.3% of silane coupling agent 3-aminopropyltriethoxysilane KH550 (the adding speed is controlled to be finished within 1 h), continuing to react at 70 ℃ for 5h, then cooling to room temperature, dropwise adding ammonia water to adjust the pH to be neutral, taking out the reactant, adding pure water, performing rotary evaporation on a rotary evaporator to remove the solvent, adding 0.4% of sodium dodecyl benzene sulfonate surfactant, and stirring at high speed for emulsification.
Selecting a yarn count of 300T with the specification of 50D and the gram weight of 80g/m 2 The dacron kasugan fabric is subjected to desizing, refining and bleaching pretreatment for 30-45min on equipment according to a conventional preparation process in a bath ratio of 1:10, is dyed with disperse dyes according to required colors, is subjected to reduction cleaning at a water bath temperature of 120-130 ℃ for a heat preservation time of 45-60min, is fully washed before being taken out of a cylinder to ensure the subsequent function finishing effect, is subjected to hydrophilic soft finishing after being dried to ensure the directional moisture conducting effect and hand feeling after finishing, is subjected to secondary soaking and primary rolling, has a titanium dioxide nano function finishing agent concentration of 50g/L, is added with 10g/L of an end-sealed isocyanate polyurethane cross-linking agent, has a rolling machine pressure of 3kg, a liquid carrying rate of 70%, a drying temperature of 180 ℃ and a vehicle speed of 65 m/min. The fabric is irradiated by sunlight for a certain time in the outdoor wearing process, and the surface of the fabric becomes hydrophilic under the stimulation of light by the surface modified titanium dioxide, so that the garment has the function of directional moisture conduction.
Example 3
The preparation method of the hydrophobic modified nitrogen-doped titanium dioxide emulsion functional finishing auxiliary agent comprises the following steps:
(1) adding nonionic surfactants of fatty alcohol-polyoxyethylene ether AEO-9, n-propanol, n-heptane, methyl trimethoxy silane and hexadecyl dimethyl silane into a reaction beaker according to the mass ratio of 3%, 4%, 25%, 4% and 0.5% respectively at room temperature, starting stirring simultaneously to mix uniformly, slowly adding deionized water with the mass fraction of 7% into the mixed solution, violently stirring until a transparent and uniform micro-emulsion is formed, and weaving the emulsion into emulsion A.
(2) Respectively mixing titanium source precursor tetrabutyl titanate and nitric acid (38%) which account for 25% and 0.3% of the total amount of the emulsion A in terms of mass fraction, adding urea with the amount of 1% of the tetrabutyl titanate, uniformly stirring, and weaving into a solution B.
(3) The solution A is transferred to a three-neck flask reaction kettle, the solution B is slowly dropped into the solution A by using a syringe pump at the speed of 2mL/min, and the stirring is continued. Introducing N after the addition is finished 2 Protecting and heating to 70 ℃, stirring for 20min, adding 0.4% of initiator ammonium persulfate and 0.6% of silane coupling agent 3-aminopropyltriethoxysilane KH550 (the adding speed is controlled to be finished within 1 h), continuing to perform heat preservation reaction at 70 ℃ for 6h, then cooling to room temperature, adding ammonia water to adjust the pH to be neutral, performing rotary evaporation on a rotary evaporator to remove the solvent, adding 0.4% of AEO-9 surfactant, and stirring at high speed for emulsification to obtain the hydrophobic modified N-titanium dioxide emulsion.
Selecting 40 cotton ammonia 95/5 blended knitted grey cloth with gram weight of 180g/m 2 Performing desizing and refining bleaching pretreatment for 30-45min on equipment according to a conventional preparation process at a bath ratio of 1:10, dyeing with reactive dye according to a required color, controlling the water bath temperature to be 55-60 ℃, keeping the temperature for 45-60min, fully washing with water before discharging from a cylinder after fixation of soda to ensure the effect of subsequent function finishing, performing one-dipping-one-rolling after scutching and drying, wherein the concentration of a titanium dioxide nano function finishing agent is 60g/L, 10g/L of a polyurethane crosslinking agent is added at the same time, the pressure of a padder of a setting machine is 3kg, the drying temperature is 170 ℃, and the vehicle speed is 30 m/min. Thereby endowing the fabric with ultraviolet resistance and water resistanceWhen the fabric is irradiated by sunlight for a certain time, the surface of the fabric becomes hydrophilic under the stimulation of the light by the surface modified titanium dioxide, so that the garment has the function of directional moisture conduction.
Example 4
The preparation method of the hydrophobic modified nitrogen-doped titanium dioxide emulsion functional finishing auxiliary agent comprises the following steps:
(1) cetyl trimethyl ammonium bromide CTAB, butanone, cyclohexane, hexafluorobutyl acrylate and hydroxyethyl methacrylate are added into a reaction beaker according to the mass ratio of 3%, 4%, 25%, 3% and 0.5% respectively at room temperature, stirring is started simultaneously to mix uniformly, deionized water with the mass fraction of 7% is slowly added into the mixed solution, stirring is vigorously carried out until a transparent and uniform micro-emulsion is formed, and the emulsion A is prepared.
(2) Respectively mixing titanium source precursors of tetraisobutyl titanate and nitric acid (36 percent) which account for 25 percent and 0.3 percent of the total amount of the emulsion A in terms of mass fraction, adding triethylamine, wherein the dosage of the triethylamine is 2 percent of the tetraisobutyl titanate, and uniformly stirring to obtain a solution B.
(3) Transferring the emulsion A into a three-neck flask reaction kettle, slowly dripping the solution B into the emulsion A by using a syringe pump at the speed of 5mL/min, and continuously stirring. Introducing N after the addition is finished 2 Protecting, heating to 80 ℃, stirring for 15min, adding an initiator azobisisobutyronitrile and a silane coupling agent 3- (methacryloyloxy) propyltriethoxysilane KH-570 (the adding speed is controlled to be within 1.5h, dropwise adding the initiator and the silane coupling agent, keeping the temperature, reacting for 5h, then cooling to room temperature, dropwise adding ammonia water to adjust the pH value to be neutral, taking out a reactant, adding pure water, performing rotary evaporation on the reactant to remove a solvent, adding 0.4% CTAB surfactant, stirring at a high speed, and emulsifying to obtain the hydrophobically modified N-titanium dioxide emulsion.
Selecting the gram weight of polyester-cotton blended 65/35 proportional fabric as 200g/m 2 Performing desizing and refining bleaching pretreatment for 30-45min on equipment according to a conventional preparation process at a bath ratio of 1:10, dyeing terylene with disperse dye according to the required color, controlling the water bath temperature at 120-130 ℃, keeping the temperature for 45-60min, reducing and cleaning, dyeing cotton with reactive dye according to the required color, controlling the water bath temperature at 55-60 DEG CThe heat preservation time is 45-60min, the mixture is fully washed before being taken out of a cylinder after the color fixation of the soda ash so as to ensure the effect of subsequent functional finishing, hydrophilic soft finishing is firstly carried out after drying, the directional moisture-conducting effect and the hand feeling after finishing are ensured, then one-dipping-one-rolling is carried out, the concentration of the titanium dioxide nano functional finishing agent is 50g/L, 10g/L of end-capped isocyanate polyurethane crosslinking agent is added, the padder pressure of the setting machine is 3kg, the liquid carrying rate is 75%, the drying temperature is 180 ℃, and the vehicle speed is 50 m/min. The fabric is irradiated by sunlight for a certain time in the outdoor wearing process, and the surface of the fabric becomes hydrophilic under the stimulation of light by the surface modified titanium dioxide, so that the garment has the function of directional moisture conduction.
And (3) testing results:
remarking: before the water drop contact angle test, the fabric is placed in a constant-temperature constant-humidity room for 24 hours under the dark condition.
The data of the above examples were tested according to: the ultraviolet protection coefficient UPF of the ultraviolet resistance is determined according to the test standard GB18830-2009, the dynamic transmission comprehensive index M of the liquid water test standard GB/T21655.2-2009
The data of different examples show that the prepared fabrics of different types have waterproof and ultraviolet-resistant effects, and the fabrics show directional moisture-conducting capability after being respectively irradiated for different times.
Claims (7)
1. A method for preparing a multifunctional finishing aid, comprising:
(1) uniformly mixing a surfactant, a cosurfactant, an oil phase and a modified monomer at room temperature, adding deionized water with the mass fraction of 5-15% into the mixed solution, and stirring until a transparent and uniform micro-emulsion is formed, wherein the micro-emulsion is recorded as emulsion A; wherein the surfactant is one of dioctyl sodium sulfosuccinate, sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, dodecyl trimethyl ammonium bromide DTAB, cetyl trimethyl ammonium bromide CTAB, fatty alcohol-polyoxyethylene ether, span 20 and polyethylene glycol monooleate; the cosurfactant is one of acetone, methyl butanone, methyl isobutyl ketone, butanone, ethyl acetate, n-hexanol, ethanol, ethylene glycol, n-propanol and isopropanol; the oil phase is one or two of n-heptane, n-hexane, cyclohexane, n-pentane and liquid paraffin; the modified monomer is one or two of acrylate monomer, organic siloxane and fluorine-containing acrylate monomer;
(2) mixing the titanium source precursor, the catalytic acid and the modified nitrogen source at room temperature, uniformly stirring, and recording as a solution B; wherein the titanium source precursor is one of titanium butyrate, titanium tetrachloride, tetraisobutyl titanate and tetraisopropyl titanate; the catalytic acid is one of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, oxalic acid, acetic acid and oxalic acid; the modified nitrogen source is one of triethylamine, urea and thiourea
(3) Dripping the solution B into the emulsion A at a speed of 1-5g/min, and introducing N after the addition is finished 2 Protecting, heating to 40-90 ℃, stirring for 5-30min, adding an initiator and a silane coupling agent, reacting for 1-10h under heat preservation, cooling to room temperature, adjusting the pH to be neutral, taking out the reactant, adding pure water, removing the solvent by rotary evaporation, adding a surfactant, stirring and emulsifying to obtain a hydrophobically modified nitrogen-doped titanium dioxide emulsion; wherein the initiator is one or more of sulfate initiator, azo initiator and redox initiator; the silane coupling agent is one or more of 3-aminopropyltriethoxysilane KH550, 3-chloropropylmethyldiethoxysilane, 3-chloropropyltriethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltriethoxysilane, vinyltriethoxysilane KH151 and 3- (methacryloyloxy) propyltriethoxysilane KH-570.
2. The method of claim 1, wherein: the dosage of the surfactant in the step (1) is 1-10% by mass; the dosage of the cosurfactant in the step (1) is 1-10% by mass fraction.
3. The method of claim 1, wherein: the dosage of the oil phase in the step (1) is 5-30% by mass; the amount of the modified monomer in the step (1) is 0.5-5% by mass.
4. The method of claim 1, wherein: the using amount of the titanium source precursor in the step (2) is 5-25% of the total amount of the emulsion A in mass fraction; the dosage of the catalytic acid in the step (2) is 0.01 to 0.5 percent of the total amount of the emulsion A in mass fraction; the modified nitrogen source dosage in the step (2) is 1-10% of the titanium source precursor dosage in mass fraction.
5. The method of claim 1, wherein: the initiator in the step (3) accounts for 0.1-0.5% of the total amount of the modified monomer by mass fraction; the dosage of the silane coupling agent in the step (3) is 0.05-0.5% of the dosage of the titanium source precursor by mass fraction.
6. The method of claim 1, wherein: the obtained multifunctional finishing auxiliary is applied to fabric finishing.
7. The method of claim 6, wherein: the method comprises the following specific steps: applying the multifunctional finishing auxiliary agent to the prepared fabric by one-dipping one-rolling or two-dipping one-rolling, and then carrying out high-temperature baking on the fabric by a setting machine; wherein the liquid carrying rate is controlled to be 20-100%, the concentration of the auxiliary agent is 10-100 g/L, the drying temperature of the setting machine is controlled to be 100-180 ℃, and the vehicle speed is 10-60 m/min.
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