CN101302718B - Method for preparing temperature sensitive intelligent anti-dip facing material and product thereof - Google Patents
Method for preparing temperature sensitive intelligent anti-dip facing material and product thereof Download PDFInfo
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- CN101302718B CN101302718B CN2008100536206A CN200810053620A CN101302718B CN 101302718 B CN101302718 B CN 101302718B CN 2008100536206 A CN2008100536206 A CN 2008100536206A CN 200810053620 A CN200810053620 A CN 200810053620A CN 101302718 B CN101302718 B CN 101302718B
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Abstract
The invention relates to a preparation method for an intelligent temperature-variable and immersion-proof shell fabric and a product thereof. The preparation method comprises the following steps: 1. temperature-variable copolymer of N-tert-butyl-acrylamide and acrylamide is obtained through the composition with a to b as the mole ratio of incoming stocks; wherein, the a lies between 60 and 40, andthe b lies between 40 and 60; 2. a coating layer liquid is prepared according to the following concentration formulation by mass: 8 to 15 percent of the copolymer, 2.0 to 5.0 percent of a crosslinking agent that is 1,2,3,4-butane tetrabasic carboxylic acid and 0.5 to 2.5 percent of a catalyst that is sodium hypophosphite; 3.the coating layer liquid is used for coating a preprocessed fabric; 4. the immersion-proof shell fabric can be obtained through post processing. The product is produced by adopting the preparation method of the intelligent temperature-variable and immersion-proof fabric ofthe invention.
Description
Technical field
The present invention relates to weaving face fabric finishing functions technology, be specially a kind of preparation method and goods thereof that are applied to the temperature sensitive intelligent anti-dip facing material of anti-exposure suit, international monopoly Main classification number plan is Int.Cl.DO6M13/00 (2006.01) I.
Background technology
Anti-exposure suit claims the winter protection anti-exposure suit again, is to have warming, the anti-special protective garment dress that soaks effect, is mainly used in river, river, lake and marine lifesaving.Anti-exposure suit is a kind of equipment of aircrew and waters operating personnel (as sailor, oil drilling platform staff etc.) indispensability, causes injury and even death because of intimate heat scatters and disappears at short notice in a large number in order to prevent the personnel of the wearing back of falling into water in danger.Anti-dip facing material is exactly the anti-special-purpose lining that soaks layer of making anti-exposure suit, plays a part that waterproof is anti-soaks.
Just wear when in danger temporarily, still be used as protective clothing and often wear, anti-exposure suit can be divided into two kinds of the anti-exposure suit of A type and Type B anti-exposure suits.Anti-dip facing material divides two classes, is applicable to anti-exposure suit of A type and Type B anti-exposure suit respectively.The anti-dip facing material that is applicable to the anti-exposure suit of A type has neoprene coated fabric and pvc coating fabric, and this type of lining is anti-to soak superior performance, but airtight, not wet thoroughly, wearing comfortableness is poor, influences task performance.The anti-dip facing material that is applicable to the Type B anti-exposure suit has high density COTTON FABRIC (Ventile), expanded microporous polytetra fluoroethylene-EPTEE laminated fabric Ge Er Tekes (Gore-tex) and atresia polyurethane coating fabric, this type of lining Waterproof Breathable, improve the universal and the comfortableness of anti-exposure suit, but had anti-problem of soaking the performance deficiency.Therefore, how improving the anti-performance of soaking is to improve the anti-main attack research topic of soaking (clothes) lining quality of Type B.
Summary of the invention
At the deficiency that prior art exists, the technical problem that quasi-solution of the present invention is determined provides a kind of preparation method and goods thereof of temperature sensitive intelligent anti-dip facing material.This preparation method is simple, and is easy to operate, is suitable for suitability for industrialized production.This preparation method's goods are that prepared anti-dip facing material has temperature sensitive property, and not only waterproof is anti-soaks effectively, and poisture-penetrability might as well.
The technical scheme that the present invention solves described preparation method's technical problem is: design a kind of preparation method of temperature sensitive intelligent anti-dip facing material, this preparation method may further comprise the steps:
1. synthetic temperature sensitive property N tert butyl acrylamide and acrylamide copolymer; Adopting raw materials components mole ratio is that 60～40: 40～60 N tert butyl acrylamide and acrylamide are initator generation radical polymerization with ammonium persulfate or azodiisobutyronitrile in methyl alcohol; Reacted mixed liquor goes out copolymer with acetone precipitation under vigorous stirring, through 3-5 dissolution precipitation, obtain N tert butyl acrylamide and acrylamide copolymer pure, white solid;
2. preparation coating liquid: be the crosslinking agent 1,2,3 of the described copolymer of coating liquid: 8-15,2.0-5.0, the catalyst sodium hypophosphite of 4-BTCA and 0.5-2.5 by the following mass percentage concentration formulated aqueous solution that becomes to be mixed;
3. fabric coating: to the fabric coating through pre-treatment, the fabric after the coating cures 1-5min at 180-200 ℃ then at 100-130 ℃ of oven dry 4-8min down, obtains coated fabric with described coating liquid; Described fabric is COTTON FABRIC, viscose fabric, sticking/cotton blended fabric and other cellulose base fiber fabric;
4. post processing was soaked the gained coated fabric 2-5 days in water, during changed water one time every 5-10 hour, take out at last at 60-90 ℃ down after the oven dry, can obtain described anti-dip facing material.
The technical scheme that the present invention solves described goods technical problem is: design a kind of temperature sensitive intelligent anti-dip facing material, this temperature sensitive intelligent anti-dip facing material adopts temperature sensitive intelligent anti-dip facing material preparation method of the present invention to make.
Compared with prior art, preparation method of the present invention is simple, does not need main equipment or special equipment, and easy operating is suitable for suitability for industrialized production.Preparation method's resulting product of the present invention is that anti-dip facing material has formed the dry state hydrogel layer because of the surface, can cover fabric face behind this gel layer water absorption and swelling, has reduced the space in the fabric, therefore has the anti-block-water performance that soaks; Because the N tert butyl acrylamide and the acrylamide copolymer that are synthesized have " temperature sensitive intelligent ", so fabric also makes anti-dip facing material of the present invention have " temperature sensitive intelligent " after being the coating liquid coating of major function composition with it.
Description of drawings
Fig. 1 varies with temperature (being temperature sensitivity) curve map for the light transmittance of a kind of embodiment gained of preparation method of the present invention coating liquid;
Fig. 2 varies with temperature (being temperature sensitivity) curve map for the anti-dip facing material swelling ratio of a kind of embodiment gained of preparation method of the present invention;
Fig. 3 is the environmental scanning electronic microscope figure of anti-dip facing material its cross section shapes when dry state of a kind of embodiment gained of preparation method of the present invention;
Fig. 4 is the environmental scanning electronic microscope figure of anti-dip facing material its cross section shapes when complete swelling of a kind of embodiment gained of preparation method of the present invention.
The specific embodiment
Further narrate the present invention below in conjunction with embodiment and accompanying drawing thereof.Specific embodiment does not limit claim of the present invention.
At the problem that present Type B anti-dip facing material exists, mentality of designing of the present invention is that intelligent aqueous gel capable is applied among the anti-dip facing material, wishes to obtain a kind of novel " temperature sensitive intelligent " anti-dip facing material.It is being taken under the environment normally, and moisture absorption is ventilative, comfortable nature; The wearer is in case in danger falling into water, and anti-ly soaks (clothes) lining and can make active response to the variation of environment, leads wet passage and seals rapidly ventilative in the fabric, stops water infiltration inner, with effective protection user.
The preparation method (abbreviation preparation method) of the temperature sensitive intelligent anti-dip facing material (abbreviation anti-dip facing material) of the present invention's design may further comprise the steps:
1. synthetic temperature sensitive property N tert butyl acrylamide and acrylamide copolymer; Adopting raw materials components mole ratio is that the N tert butyl acrylamide of 60～40: 40～60 (preferred 50: 50) and acrylamide are initator generation radical polymerization with ammonium persulfate or azodiisobutyronitrile (initiator system of ammonium persulfate) in methyl alcohol; Reacted mixed liquor goes out copolymer with acetone precipitation under vigorous stirring, through 3-5 dissolution precipitation, obtain N tert butyl acrylamide and acrylamide copolymer pure, white solid.The aqueous solution of gained copolymer has temperature sensitivity, can be dissolved in the water under a certain temperature, is higher than this temperature and does not then dissolve, and can make solution the white opacity thing occur, and this temperature is called lower critical solution temperature (LCST).
2. prepare coating liquid: coating liquid is the aqueous solution that is mixed by following mass percentage concentration formulated: copolymer 8-15%, the crosslinking agent 1 of the 1st step gained, 2,3,4-BTCA (BTCA) 2.0-5.0% and catalyst sodium hypophosphite (SHP) 0.5-2.5%.This coating liquid can be called temperature sensitive intelligent coating liquid.
3. fabric coating: to the fabric coating through pre-treatment, the fabric after the coating cures 1-5min at 180-200 ℃ then at 100-130 ℃ of oven dry 4-8min down, obtains coated fabric with the described coating liquid of the 2nd step preparation; Described fabric is COTTON FABRIC, viscose fabric, sticking/cotton blended fabric and other cellulose base fiber fabric.The pre-treatment of described fabric comprises technologies such as destarch, kiering and bleaching.These technologies are prior art.
4. post processing was soaked the gained coated fabric 2-5 days in water, during changed water one time every 5-10 hour, to remove unreacted reactant; Take out at last after oven dry under 60-90 ℃, can obtain described anti-dip facing material.
Preparation method's of the present invention further feature is, described fabric coating is 2-5 time, and repeatedly coating can have better coating result; After each coating is intact, fabric is dried 4-8min down at 100-130 ℃, fabric after the last oven dry cures 1-5min at 180-200 ℃, so that better reaction takes place in BTCA and copolymer and fabric (cellulose) fiber, form three-dimensional cross-linked polymer, and and fabric (cellulose) fiber between set up covalently cross-linked.This three-dimensional cross-linked polymer is water insoluble, can be swelled into the three-dimensional cross-linked aquogel with honeycomb hole (referring to Fig. 4) in water at low temperature, is called the dry state aquogel during drying regime.
Direct resulting product of preparation method of the present invention or product promptly are described anti-dip facing materials.The surface of this anti-dip facing material has one deck cross-linked polymer---the dry state aquogel.When dry state, the aquogel molecule is in contraction state (referring to Fig. 3), and space in the anti-dip facing material is open, fabric ventilative, water vapour permeability is good; And in a single day fabric immerses in the water at low temperature, and the face coat water absorption and swelling on the anti-dip facing material becomes the aquogel with honeycomb hole, covers fabric face (referring to Fig. 4), can stop water to permeate to fabric, plays the anti-effect of soaking of waterproof; When anti-dip facing material is separated from water environment, after its water evaporates, aquogel shrinks, and the space in the fabric exposes again, recovers its ventilative, poisture-penetrability automatically, has " intelligent ".In addition, the coating aquogel has temperature sensitivity, below 32 ℃ the time, and swelling behavior, the infiltration of block water; In 32-55 ℃ of temperature range, aquogel shrinks, and fabric void is exposed gradually, and the infiltration capacity of water increases gradually, so anti-dip facing material of the present invention can adjust its permeable vapor transfer rate automatically according to water temperature, has " temperature sensitive intelligent ".
The present invention does not address part and is applicable to prior art.
Provide preparation method's specific embodiment of the present invention below.
Embodiment 1
1. synthetic temperature sensitive property N tert butyl acrylamide and acrylamide copolymer; Adopting raw materials components mole ratio is that 50: 50 N tert butyl acrylamide and acrylamide are initator generation Raolical polymerizable with the ammonium persulfate in methyl alcohol; Reacted mixed liquor goes out copolymer with acetone precipitation under vigorous stirring, through 5 dissolution precipitations, obtain N tert butyl acrylamide and acrylamide copolymer pure, white solid.It is 28.2 ℃ (referring to Fig. 1) that the gained copolymer adopts AAS to record its LCST.
2. prepare coating liquid: 8% (quality, down with) copolymer of the 1st step gained, 2.3% crosslinking agent B TCA and 2.2% catalyst S HP be mixed with the aqueous solution, put into refrigerator after the stirring, deaeration at least 24 hours, and make it further dissolve mixing, can often stir during this time,, be prepared into temperature sensitive intelligent coating liquid with accelerate dissolution and mixing.
3. fabric coating: to through the pure cotton fabric coating of pre-treatment 5 times, the fabric after each coating cures 2min at 120 ℃ of oven dry 5min down after the last coating under 200 ℃, obtain coated fabric with the coating liquid of the 2nd step preparation.
4. post processing: the gained coated fabric after running water flushing, was used distilled water immersion 3 days again, during changed water one time every 8 hours, to remove unreacted reactant; At last coated fabric is taken out after 80 ℃ of oven dry, promptly obtain anti-dip facing material of the present invention.
1. synthetic temperature sensitive property N tert butyl acrylamide and acrylamide copolymer; Adopting raw materials components mole ratio is that 40: 60 N tert butyl acrylamide and acrylamide are initator generation Raolical polymerizable with the azodiisobutyronitrile in methyl alcohol; Reacted mixed liquor goes out copolymer with acetone precipitation under vigorous stirring, through 4 dissolution precipitations, obtain N tert butyl acrylamide and acrylamide copolymer pure, white solid.It is 39.0 ℃ that the gained copolymer adopts AAS to record its LCST.
2. prepare coating liquid: 15% (quality, down together) copolymer of the 1st step gained, 5.0% crosslinking agent B TCA and 2.5% catalyst S HP are mixed with the aqueous solution that is mixed, surplus with embodiment 1.
3. fabric coating: to through the pure cotton fabric coating of pre-treatment 2 times, the fabric after each coating cures 3min at 100 ℃ of oven dry 8min down after the last coating under 190 ℃, obtain coated fabric with the coating liquid of the 2nd step preparation.
4. post processing: implementation method is with embodiment 1.Promptly obtain anti-dip facing material of the present invention.
Embodiment 3
1. synthetic temperature sensitive property N tert butyl acrylamide and acrylamide copolymer; Adopting raw materials components mole ratio is that 60: 40 N tert butyl acrylamide and acrylamide are initator generation Raolical polymerizable with the ammonium persulfate in methyl alcohol; Reacted mixed liquor goes out copolymer with acetone precipitation under vigorous stirring, through 5 dissolution precipitations, obtain N tert butyl acrylamide and acrylamide copolymer pure, white solid.It is 18.0 ℃ that the gained copolymer adopts AAS to record its LCST.
2. prepare coating liquid: 10% (quality, down together) copolymer of the 1st step gained, 3.0% crosslinking agent B TCA and 2.0% catalyst S HP are mixed with the aqueous solution, surplus with embodiment 1.
3. fabric coating: to through the pure cotton fabric coating of pre-treatment 3 times, the fabric after each coating cures 1min at 120 ℃ of oven dry 4min down after the last coating under 200 ℃, obtain coated fabric with the coating liquid of the 2nd step preparation.
4. post processing: implementation method is with embodiment 1.Promptly obtain anti-dip facing material of the present invention.
Claims (4)
1. the preparation method of a temperature sensitive intelligent anti-dip facing material, this preparation method may further comprise the steps:
(1). synthetic temperature sensitive property N tert butyl acrylamide and acrylamide copolymer; Adopting raw materials components mole ratio is that 60～40: 40～60 N tert butyl acrylamide and acrylamide are initator generation radical polymerization with ammonium persulfate or azodiisobutyronitrile in methyl alcohol; Reacted mixed liquor goes out copolymer with acetone precipitation under vigorous stirring, through 3-5 dissolution precipitation, obtain N tert butyl acrylamide and acrylamide copolymer pure, white solid;
(2). preparation coating liquid: be the crosslinking agent 1,2,3 of the described copolymer of coating liquid: 8-15%, 2.0-5.0%, the catalyst sodium hypophosphite of 4-BTCA and 0.5-2.5% by the following mass percentage concentration formulated aqueous solution that becomes to be mixed;
(3). fabric coating: to the fabric coating through pre-treatment, the fabric after the coating is dried 4-8min down at 100-130 ℃, cures 1-5min at 180-200 ℃ then, obtains coated fabric with described coating liquid; Described fabric is COTTON FABRIC, viscose fabric, sticking/cotton blended fabric and other cellulose base fiber fabric;
(4). post processing, the gained coated fabric was soaked in water 2-5 days, during changed water one time every 5-10 hour, take out at last at 60-90 ℃ down after the oven dry, can obtain described anti-dip facing material.
2. the preparation method of temperature sensitive intelligent anti-dip facing material according to claim 1, the raw materials components mole ratio that it is characterized in that described N tert butyl acrylamide and acrylamide is 50: 50, described initator is an ammonium persulfate.
3. the preparation method of temperature sensitive intelligent anti-dip facing material according to claim 1 is characterized in that described fabric coating is 2-5 time; After each coating was intact, fabric was dried 4-8min down at 100-130 ℃, and the fabric after the last oven dry cures 1-5min at 180-200 ℃.
4. a temperature sensitive intelligent anti-dip facing material is characterized in that this anti-dip facing material adopts claim 1,2 or 3 described temperature sensitive intelligent anti-dip facing material preparation methods to make.
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| CN101302718B true CN101302718B (en) | 2010-06-09 |
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| CN102587152A (en) * | 2012-02-22 | 2012-07-18 | 苏州金尚豪纺织有限公司 | Immersion-resistant aromatic fabric |
| CN103741326B (en) * | 2013-12-17 | 2015-03-25 | 葛小飞 | Method for preparing wear-proof cotton and linen fabric |
| CN105803762B (en) * | 2016-04-27 | 2018-07-06 | 浙江理工大学 | A kind of method for realizing textile intelligent cleaning function by being crosslinked temperature sensitive copolymer |
| CN106498720B (en) * | 2016-11-18 | 2019-03-05 | 辽东学院 | A kind of temperature sensitive waterproof moisture permeable fabric and preparation method thereof |
| CN109252370A (en) * | 2018-08-03 | 2019-01-22 | 浙江理工大学 | The method for reducing preparation cost by improving cross-linking efficiency and improving cleaning efficiency |
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| CN1883438A (en) * | 2005-06-21 | 2006-12-27 | 香港理工大学 | Temperature responsive intelligent facial mask and method for preparing same |
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