CN108411638A - A kind of preparation method of weaving waterproofing agent - Google Patents

A kind of preparation method of weaving waterproofing agent Download PDF

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CN108411638A
CN108411638A CN201810287372.5A CN201810287372A CN108411638A CN 108411638 A CN108411638 A CN 108411638A CN 201810287372 A CN201810287372 A CN 201810287372A CN 108411638 A CN108411638 A CN 108411638A
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dried
added
mass ratio
temperature
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郭跃
徐扣华
丁正颖
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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
    • 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
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
    • D06M15/568—Reaction products of isocyanates with polyethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
    • C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/77—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 silicon or compounds thereof
    • D06M11/79—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 silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
    • D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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    • D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
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Abstract

The invention discloses a kind of preparation methods of weaving waterproofing agent, belong to weaving field of waterproof materials.The present invention is modified nano silicon dioxide by coupling agent, due to the small-size effect and macro quanta tunnel effect of nano silicon dioxide,, raising serous coat wear-resisting property damaged so as to effective lint, the dispersibility of nano silicon dioxide can also be improved simultaneously, and also utilize the absorption property of nano silicon dioxide, high mallow stem skin extracting solution is adsorbed, due to having many OH in extracting solution molecule, into in the institutional framework of real silk fabric, make to generate preferable caking property between fiber, to improve tensile property, the uvioresistant performance of fabric.The present invention solves waterproofing agent currently on the market and not can effectively solve the problem that waterproof problem, the problem of leading to low fabric tension performance, fibre beakage.

Description

A kind of preparation method of weaving waterproofing agent
Technical field
The invention belongs to waterproof fields of weaving, and in particular to a kind of preparation method of weaving waterproof.
Background technology
Weaving waterproofing agent, belongs to one of the product of textile material auxiliary agent class.With the raising required properties of textile, carry The auxiliary agent of high textile various aspects of performance is also developed in succession.In order to meet textile can daily life and rainy day, Normal use under the particular surroundings such as hot summer days, high temperature, field, the water-proofing treatment of textile is with regard to particularly important.Without water-proofing treatment Textile fabric after the absorbing sweat that absorbs water, water sweat penetrates into the textile back side, can influence the appearance and comfort of textile.At waterproof Reason is an important procedure of textile fabric final finishing, and waterproofing agent can assign textile surface hydrophobic property
Possess a variety of weaving waterproofing agent products on the market, but these waterproofing agents all have certain defect, are actually using In, waterproofing agent currently on the market not can effectively solve the problem that waterproof problem, lead to that fabric tension performance is low, fibre beakage.
Invention content
The technical problems to be solved by the invention：It not can effectively solve the problem that waterproof is asked for waterproofing agent currently on the market The problem of inscribing, leading to low fabric tension performance, fibre beakage provides a kind of preparation method of weaving waterproofing agent.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of preparation method of weaving waterproofing agent, the preparation method include the following steps：
（1）In mass ratio 1：100, nano silicon dioxide, the ethanol solution that volume fraction is 95% are mixed, stirred evenly, Sonic oscillation is added the titanate coupling agent of nano silicon dioxide quality 1 ~ 3%, is heated to reflux, obtains phegma, by phegma into Sediment is dried at 60 ~ 70 DEG C of temperature, grinds, obtain abrasive material by row centrifugation, taking precipitate；
（2）In mass ratio 1：6 ~ 8, abrasive material, extracting solution are mixed, impregnated, filtering obtains filter residue a, by filter residue a in temperature It is dried at 50 ~ 60 DEG C, obtains drying object, in mass ratio 1：5 ~ 7, Quaternary Ammonium Salt of Chitosan, acetic acid solution are mixed, stirs, adds The drying object for entering Quaternary Ammonium Salt of Chitosan quality 20 ~ 30%, stirs evenly, and spray drying obtains dried object；
（3）It counts in parts by weight, takes 70 ~ 80 parts of deionized waters, 10 ~ 15 parts of propylene glycol polyethers, 9 ~ 10 parts of phorone diisocyanates Ester, 2 ~ 4 parts of castor oil, 2 ~ 4 parts of dried objects, 2 ~ 4 parts of dihydromethyl propionic acids, 2 ~ 4 parts of trimethylolpropanes, 2 ~ 4 parts of 1,4- fourths two Alcohol, 1 ~ 3 part of triethylamine, 0.3 ~ 0.5 part of catalyst, by isophorone diisocyanate, propylene glycol polyethers, castor oil temperature 38 ~ It is mixed, is stirred at 40 DEG C, be warming up to 68 ~ 70 DEG C, catalyst is added, stand 1 ~ 3h, dihydromethyl propionic acid is added, stood, Trimethylolpropane, 1,4-butanediol is added, heat preservation is cooled to 38 ~ 40 DEG C, and triethylamine is added and neutralizes, is cooled to 28 ~ 30 DEG C, Deionized water, dried object is added, stirring obtains stirring liquid；
（4）In mass ratio 1：1：1, by γ-methacryloxypropyl trimethoxy silane, vinyltrimethoxysilane, Octamethylcy-clotetrasiloxane is mixed, and mixed liquor, in mass ratio 1 are obtained：5~7：0.1 ~ 0.3, by mixed liquor, stirring liquid, cause Agent is kept the temperature at 80 ~ 83 DEG C of temperature, is cooled to 40 ~ 50 DEG C, adjusts pH value, and filtering and discharging collects feed liquid to get weaving waterproof Agent.
The step（1）Middle titanate coupling agent is isopropyl three（Isostearoyl base）Titanate esters.
The step（2）Middle extracting solution is that high mallow stem skin is dried, and obtains dried object, dried object is washed with water, set In the deionized water of 7 ~ 9 times of dried object quality, 80 ~ 85 DEG C are heated to, is impregnated, filtering obtains filter residue, in mass ratio 1：5 ~ 7, it will Filter residue, hydrochloric acid solution at 70 ~ 80 DEG C of temperature refluxing extraction to get extracting solution.
The step（3）Middle catalyst is dibutyl tin dilaurate.
The step（4）Middle initiator be ammonium persulfate, potassium peroxydisulfate it is therein any one.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention is modified nano silicon dioxide by coupling agent, due to nano silicon dioxide small-size effect and Macro quanta tunnel effect, raising serous coat wear-resisting property damaged so as to effective lint, while nanometer two can also be improved The dispersibility of silica, and the absorption property of nano silicon dioxide is also utilized, high mallow stem skin extracting solution is adsorbed, due to carrying Taking in liquid molecule has very much-OH, into the institutional framework of real silk fabric, makes to generate preferable caking property between fiber, from And improve the tensile property of fabric, uvioresistant performance.
（2）The present invention is prepared aqueous polyurethane emulsion as raw material, and is utilized using propylene glycol polyethers, isophorone diisocyanate Castor oil modified, the long-chain fat segment in castor oil molecule assigns good hydrophobicity, so as to improve aqueous polyurethane coating The water resistance of fabric, and grain size is smaller, is easy to penetrate into inside fabric fibre, while and Zeta potential is positive value, be conducive to Increase the repulsive force of latex intergranular, improves emulsion intercalation method.
（3）The present invention is also in one layer of Quaternary Ammonium Salt of Chitosan film of the apparent package of nano silicon dioxide, Quaternary Ammonium Salt of Chitosan film In cation, on the one hand improves nano silicon dioxide and preferably combined with negatively charged fabric fibre surface, it is another The addition of aspect Quaternary Ammonium Salt of Chitosan changes the more regular close crystalline texture of aqueous polyurethane film, the crystallinity hair of blend film Variation is given birth to, and since Quaternary Ammonium Salt of Chitosan contains-OH ,-NH 2 Equal hydrophilic radicals, intermolecular combination become close, hydrone It is difficult to pass through, to which water proofing property increases, while Quaternary Ammonium Salt of Chitosan film also has antibiotic property, good anti-to assign fabric Water, anti-microbial property, are additionally added composite organic in addition, and since composite organic has unique chemical constitution, surface energy is low, from And further increase the water resistance of aqueous polyurethane film.
Specific implementation mode
Titanate coupling agent is isopropyl three（Isostearoyl base）Titanate esters.
Extracting solution is that high mallow stem skin is dried, and obtains dried object, dried object is washed with water, be placed in dried object quality 7 ~ In 9 times of deionized water, 80 ~ 85 DEG C are heated to, impregnates 8 ~ 10min, filtering obtains filter residue, in mass ratio 1：5 ~ 7, by filter residue, salt Acid solution at 70 ~ 80 DEG C of temperature 1 ~ 3h of refluxing extraction to get extracting solution.
Catalyst is dibutyl tin dilaurate.
Initiator be ammonium persulfate, potassium peroxydisulfate it is therein any one.
A kind of preparation method of weaving waterproofing agent, the preparation method include the following steps：
（1）In mass ratio 1：100, nano silicon dioxide, the ethanol solution that volume fraction is 95% are mixed, stirred evenly, 10 ~ 15min of sonic oscillation is added the titanate coupling agent of nano silicon dioxide quality 1 ~ 3%, is heated to reflux, obtains phegma, will Phegma is centrifuged, taking precipitate, and sediment is dried at 60 ~ 70 DEG C of temperature, grinds, obtains abrasive material；
（2）In mass ratio 1：6 ~ 8, abrasive material, extracting solution are mixed, 1 ~ 3h is impregnated, filtering obtains filter residue a, filter residue a is existed It is dried at 50 ~ 60 DEG C of temperature, obtains drying object, in mass ratio 1：5 ~ 7, Quaternary Ammonium Salt of Chitosan, acetic acid solution are mixed, stirred 25 ~ 30min is added the drying object of Quaternary Ammonium Salt of Chitosan quality 20 ~ 30%, stirs evenly, and is spray-dried, obtains dried object；
（3）It counts in parts by weight, takes 70 ~ 80 parts of deionized waters, 10 ~ 15 parts of propylene glycol polyethers, 9 ~ 10 parts of phorone diisocyanates Ester, 2 ~ 4 parts of castor oil, 2 ~ 4 parts of dried objects, 2 ~ 4 parts of dihydromethyl propionic acids, 2 ~ 4 parts of trimethylolpropanes, 2 ~ 4 parts of 1,4- fourths two Alcohol, 1 ~ 3 part of triethylamine, 0.3 ~ 0.5 part of catalyst, by isophorone diisocyanate, propylene glycol polyethers, castor oil temperature 38 ~ It is mixed at 40 DEG C, stirs 30 ~ 40min, be warming up to 68 ~ 70 DEG C, catalyst is added, stand 1 ~ 3h, dihydroxymethyl third is added Acid stands 1 ~ 3h, and trimethylolpropane, 1,4-butanediol is added, and keeps the temperature 80 ~ 100min, is cooled to 38 ~ 40 DEG C, and three second are added With 25 ~ 30min in amine, 28 ~ 30 DEG C are cooled to, deionized water, dried object is added, 25 ~ 30min is stirred, obtains stirring liquid；
（4）In mass ratio 1：1：1, by γ-methacryloxypropyl trimethoxy silane, vinyltrimethoxysilane, Octamethylcy-clotetrasiloxane is mixed, and mixed liquor, in mass ratio 1 are obtained：5~7：0.1 ~ 0.3, by mixed liquor, stirring liquid, cause Agent keeps the temperature the h of l ~ 3 at 80 ~ 83 DEG C of temperature, is cooled to 40 ~ 50 DEG C, adjusts pH value, and filtering and discharging collects feed liquid to get weaving Waterproofing agent.
Embodiment 1
Titanate coupling agent is isopropyl three（Isostearoyl base）Titanate esters.
Extracting solution is that high mallow stem skin is dried, and obtains dried object, dried object is washed with water, be placed in dried object quality 7 In deionized water again, 80 DEG C are heated to, impregnates 8min, filtering obtains filter residue, in mass ratio 1：5, filter residue, hydrochloric acid solution are existed Refluxing extraction 1h is to get extracting solution under temperature 70 C.
Catalyst is dibutyl tin dilaurate.
Initiator is ammonium persulfate.
A kind of preparation method of weaving waterproofing agent, the preparation method include the following steps：
（1）In mass ratio 1：100, nano silicon dioxide, the ethanol solution that volume fraction is 95% are mixed, stirred evenly, Sonic oscillation 10min is added the titanate coupling agent of nano silicon dioxide quality 1%, is heated to reflux, obtains phegma, by phegma It is centrifuged, taking precipitate, sediment is dried under temperature 60 C, ground, obtain abrasive material；
（2）In mass ratio 1：6, abrasive material, extracting solution are mixed, 1h is impregnated, filtering obtains filter residue a, by filter residue a in temperature It is dried at 50 DEG C, obtains drying object, in mass ratio 1：5, Quaternary Ammonium Salt of Chitosan, acetic acid solution are mixed, 25min is stirred, adds The drying object for entering Quaternary Ammonium Salt of Chitosan quality 20%, stirs evenly, and spray drying obtains dried object；
（3）It counts in parts by weight, takes 70 parts of deionized waters, 10 parts of propylene glycol polyethers, 9 parts of isophorone diisocyanates, 2 portions of castor-oil plants Oil, 2 parts of dried objects, 2 parts of dihydromethyl propionic acids, 2 parts of trimethylolpropanes, 2 parts of 1,4- butanediols, 1 part of triethylamine, 0.3 part urge Agent mixes isophorone diisocyanate, propylene glycol polyethers, castor oil at 38 DEG C of temperature, stirs 30min, heating To 68 DEG C, catalyst is added, stands 1h, dihydromethyl propionic acid is added, stands 1h, trimethylolpropane, 1,4-butanediol is added, 80min is kept the temperature, is cooled to 38 DEG C, is added in triethylamine and 25min, 28 DEG C is cooled to, deionized water, dried object, stirring is added 25min obtains stirring liquid；
（4）In mass ratio 1：1：1, by γ-methacryloxypropyl trimethoxy silane, vinyltrimethoxysilane, Octamethylcy-clotetrasiloxane is mixed, and mixed liquor, in mass ratio 1 are obtained：5：0.1, by mixed liquor, stirring liquid, initiator, in temperature Lh is kept the temperature at 80 DEG C of degree, is cooled to 40 DEG C, adjusts pH value, filtering and discharging collects feed liquid to get weaving waterproofing agent.
Embodiment 2
Titanate coupling agent is isopropyl three（Isostearoyl base）Titanate esters.
Extracting solution is that high mallow stem skin is dried, and obtains dried object, dried object is washed with water, be placed in dried object quality 9 In deionized water again, 85 DEG C are heated to, impregnates 10min, filtering obtains filter residue, in mass ratio 1：7, filter residue, hydrochloric acid solution are existed Refluxing extraction 3h is to get extracting solution at 80 DEG C of temperature.
Catalyst is dibutyl tin dilaurate.
Initiator is ammonium persulfate.
A kind of preparation method of weaving waterproofing agent, the preparation method include the following steps：
（1）In mass ratio 1：100, nano silicon dioxide, the ethanol solution that volume fraction is 95% are mixed, stirred evenly, Sonic oscillation 15min is added the titanate coupling agent of nano silicon dioxide quality 3%, is heated to reflux, obtains phegma, by phegma It is centrifuged, taking precipitate, sediment is dried under temperature 70 C, ground, obtain abrasive material；
（2）In mass ratio 1：8, abrasive material, extracting solution are mixed, 3h is impregnated, filtering obtains filter residue a, by filter residue a in temperature It is dried at 60 DEG C, obtains drying object, in mass ratio 1：7, Quaternary Ammonium Salt of Chitosan, acetic acid solution are mixed, 30min is stirred, adds The drying object for entering Quaternary Ammonium Salt of Chitosan quality 30%, stirs evenly, and spray drying obtains dried object；
（3）It counts in parts by weight, takes 80 parts of deionized waters, 15 parts of propylene glycol polyethers, 10 parts of isophorone diisocyanates, 4 parts of castors Sesame oil, 4 parts of dried objects, 4 parts of dihydromethyl propionic acids, 4 parts of trimethylolpropanes, 4 parts of 1,4- butanediols, 3 parts of triethylamines, 0.5 part Isophorone diisocyanate, propylene glycol polyethers, castor oil are mixed at 40 DEG C of temperature, stir 40min, risen by catalyst Catalyst is added to 70 DEG C in temperature, stands 3h, and dihydromethyl propionic acid is added, and stands 3h, and trimethylolpropane, Isosorbide-5-Nitrae-fourth two is added Alcohol keeps the temperature 100min, is cooled to 40 DEG C, is added in triethylamine and 30min, is cooled to 30 DEG C, deionized water, dried object is added, 30min is stirred, stirring liquid is obtained；
（4）In mass ratio 1：1：1, by γ-methacryloxypropyl trimethoxy silane, vinyltrimethoxysilane, Octamethylcy-clotetrasiloxane is mixed, and mixed liquor, in mass ratio 1 are obtained：7：0.3, by mixed liquor, stirring liquid, initiator, in temperature The h of l ~ 3 are kept the temperature at 83 DEG C of degree, are cooled to 50 DEG C, adjust pH value, and filtering and discharging collects feed liquid to get weaving waterproofing agent.
Embodiment 3
Titanate coupling agent is isopropyl three（Isostearoyl base）Titanate esters.
Extracting solution is that high mallow stem skin is dried, and obtains dried object, dried object is washed with water, be placed in dried object quality 8 In deionized water again, 82.5 DEG C are heated to, impregnates 9min, filtering obtains filter residue, in mass ratio 1：6, by filter residue, hydrochloric acid solution Refluxing extraction 2h is to get extracting solution at 75 DEG C of temperature.
Catalyst is dibutyl tin dilaurate.
Initiator is potassium peroxydisulfate.
A kind of preparation method of weaving waterproofing agent, the preparation method include the following steps：
（1）In mass ratio 1：100, nano silicon dioxide, the ethanol solution that volume fraction is 95% are mixed, stirred evenly, Sonic oscillation 12.5min is added the titanate coupling agent of nano silicon dioxide quality 2%, is heated to reflux, obtains phegma, will flow back Liquid is centrifuged, taking precipitate, and sediment is dried at 65 DEG C of temperature, grinds, obtains abrasive material；
（2）In mass ratio 1：7, abrasive material, extracting solution are mixed, 2h is impregnated, filtering obtains filter residue a, by filter residue a in temperature It is dried at 55 DEG C, obtains drying object, in mass ratio 1：6, Quaternary Ammonium Salt of Chitosan, acetic acid solution are mixed, 27.5min is stirred, The drying object of Quaternary Ammonium Salt of Chitosan quality 25% is added, stirs evenly, is spray-dried, obtains dried object；
（3）Count in parts by weight, take 75 parts of deionized waters, 12.5 parts of propylene glycol polyethers, 9.5 parts of isophorone diisocyanates, 3 parts Castor oil, 3 parts of dried objects, 3 parts of dihydromethyl propionic acids, 3 parts of trimethylolpropanes, 3 parts of 1,4- butanediols, 2 parts of triethylamines, 0.4 Isophorone diisocyanate, propylene glycol polyethers, castor oil are mixed at 39 DEG C of temperature, stir 35min by part catalyst, 69 DEG C are warming up to, catalyst is added, stands 2h, dihydromethyl propionic acid is added, stands 2h, trimethylolpropane, Isosorbide-5-Nitrae-fourth is added Glycol keeps the temperature 90min, is cooled to 39 DEG C, is added in triethylamine and 27.5min, is cooled to 29 DEG C, deionized water, drying is added Object stirs 27.5min, obtains stirring liquid；
（4）In mass ratio 1：1：1, by γ-methacryloxypropyl trimethoxy silane, vinyltrimethoxysilane, Octamethylcy-clotetrasiloxane is mixed, and mixed liquor, in mass ratio 1 are obtained：6：0.2, by mixed liquor, stirring liquid, initiator, in temperature 2 h are kept the temperature at 81.5 DEG C of degree, are cooled to 45 DEG C, adjust pH value, filtering and discharging collects feed liquid to get weaving waterproofing agent.
Comparative example：The weaving waterproofing agent of company of Liuzhou City production
Fabric seepage of water tester method of testing：Fabric seepage of water tester one, mainly for detection of waterproof garment, raincoat, tent, The product of waterproof bag, water-proof gloves series.4 pieces of material cloth of the same race, is divided into four groups, uses the anti-of embodiment and comparative example respectively Aqua carries out weaving waterproof after finishing.Sample is fixed on the test zone of standard required area, by air compressor machine by 0-5bar Air be added in a water pot full of distilled water, water pot connecting test head, by certain pressure transmission to sample.Pressure is bent Line real-time display is in operation display, by pressure size suffered by measured object known to pressure gauge and measured object in this pressure It is whether qualified under force effect.According to as follows
Technical parameter is as experimental standard：
Execution standard：Meet gb4744-84, also complies with iso-811
Measurement range：Waterproof fabrics, tent, down jackets, anorak, anorak, poly-bag, insulated cold wear, umbrella, raincoat, cloth etc.
Technical parameter：Sample is horizontal positioned, and pressure is born below sample
Pressure area：100cm2, d=11.28cm
Water-column：0-10000mmH2O(10000mmH2O or more needs customized)
The rate of climb：10±3mmH2O（Standard speed）60±20 mmH2O
Standard speed：100±30 mmH2O（It advances the speed）
Sensitivity：1mmH2O, maximum show value 10000mmH2O
Experimental result such as the following table 1：
Table 1
Experimental group Embodiment 1 Embodiment 2 Embodiment 3 Comparative example
Waterproof rate/% 92 97.2 95 85.7
Uvioresistant/% 89 93.5 91.4 79.3
Stretch-proof/% 95.4 98.3 97.1 88.7
In conclusion the weaving waterproofing agent of the present invention complies fully with requirement, it is worth promoting and uses.

Claims (5)

1. a kind of preparation method of weaving waterproofing agent, which is characterized in that the preparation method includes the following steps：
（1）In mass ratio 1：100, nano silicon dioxide, the ethanol solution that volume fraction is 95% are mixed, stirred evenly, Sonic oscillation is added the titanate coupling agent of nano silicon dioxide quality 1 ~ 3%, is heated to reflux, obtains phegma, by phegma into Sediment is dried at 60 ~ 70 DEG C of temperature, grinds, obtain abrasive material by row centrifugation, taking precipitate；
（2）In mass ratio 1：6 ~ 8, abrasive material, extracting solution are mixed, impregnated, filtering obtains filter residue a, by filter residue a in temperature It is dried at 50 ~ 60 DEG C, obtains drying object, in mass ratio 1：5 ~ 7, Quaternary Ammonium Salt of Chitosan, acetic acid solution are mixed, stirs, adds The drying object for entering Quaternary Ammonium Salt of Chitosan quality 20 ~ 30%, stirs evenly, and spray drying obtains dried object；
（3）It counts in parts by weight, takes 70 ~ 80 parts of deionized waters, 10 ~ 15 parts of propylene glycol polyethers, 9 ~ 10 parts of phorone diisocyanates Ester, 2 ~ 4 parts of castor oil, 2 ~ 4 parts of dried objects, 2 ~ 4 parts of dihydromethyl propionic acids, 2 ~ 4 parts of trimethylolpropanes, 2 ~ 4 parts of 1,4- fourths two Alcohol, 1 ~ 3 part of triethylamine, 0.3 ~ 0.5 part of catalyst, by isophorone diisocyanate, propylene glycol polyethers, castor oil temperature 38 ~ It is mixed, is stirred at 40 DEG C, be warming up to 68 ~ 70 DEG C, catalyst is added, stand 1 ~ 3h, dihydromethyl propionic acid is added, stood, Trimethylolpropane, 1,4-butanediol is added, heat preservation is cooled to 38 ~ 40 DEG C, and triethylamine is added and neutralizes, is cooled to 28 ~ 30 DEG C, Deionized water, dried object is added, stirring obtains stirring liquid；
（4）In mass ratio 1：1：1, by γ-methacryloxypropyl trimethoxy silane, vinyltrimethoxysilane, Octamethylcy-clotetrasiloxane is mixed, and mixed liquor, in mass ratio 1 are obtained：5~7：0.1 ~ 0.3, by mixed liquor, stirring liquid, cause Agent is kept the temperature at 80 ~ 83 DEG C of temperature, is cooled to 40 ~ 50 DEG C, adjusts pH value, and filtering and discharging collects feed liquid to get weaving waterproof Agent.
2. the preparation method for waterproofing agent of weaving according to claim 1, which is characterized in that the step（1）Middle titanate esters are even It is isopropyl three to join agent（Isostearoyl base）Titanate esters.
3. the preparation method for waterproofing agent of weaving according to claim 1, which is characterized in that the step（2）Middle extracting solution is High mallow stem skin is dried, dried object is obtained, dried object is washed with water, is placed in the deionized water of 7 ~ 9 times of dried object quality, 80 ~ 85 DEG C are heated to, is impregnated, filtering obtains filter residue, in mass ratio 1：5 ~ 7, by filter residue, hydrochloric acid solution 70 ~ 80 DEG C of temperature next time Stream extraction is to get extracting solution.
4. the preparation method for waterproofing agent of weaving according to claim 1, which is characterized in that the step（3）Middle catalyst is Dibutyl tin dilaurate.
5. the preparation method for waterproofing agent of weaving according to claim 1, which is characterized in that the step（4）Middle initiator is Ammonium persulfate, potassium peroxydisulfate it is therein any one.
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CN111379170A (en) * 2018-12-27 2020-07-07 苏州迪塔杉针织有限公司 Preparation method of coating liquid for enhancing wear resistance of textile fiber yarns
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CN112323479A (en) * 2020-10-29 2021-02-05 长兴卓恒新材料科技有限公司 Preparation method of environment-friendly nano waterproof agent for textiles
CN112280262A (en) * 2020-11-12 2021-01-29 浙江贝隆纺织有限公司 Preparation method of ultraviolet-resistant flame-retardant polyester fiber master batch
CN112281255A (en) * 2020-11-12 2021-01-29 浙江贝隆纺织有限公司 Preparation method of anti-ultraviolet flame-retardant polyester filament yarn

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