CN104153033B - A kind of preparation method of porous easy dyeing spandex - Google Patents
A kind of preparation method of porous easy dyeing spandex Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of porous easy dyeing spandex, the method is at the first reactor 1stIn Reactor, add polytetramethylene ether diol PTMG, 4 simultaneously, 4-'-diphenylmethane diisocyanate 4,4-MDI, fully carries out prepolymerization reaction, obtains the prepolymer PP with-NCO end-blocking; In high speed dissolving machine Dissolver, adopt DMA DMAC as solvent, to prepolymer, PP fully dissolves, the pre-polymer solution PPs of contained-NCO end-blocking; At the second reactor 2ndIn Reactor, adopt the mixed amine DMAC solution that contains Diamines chain extender, monoamine terminator and hydramine to carry out chain growth, chain termination to PPs simultaneously, prepare end with-OH polyurea based formic acid esters solution; Then, add antioxidant, lubricant, delustering agent, ultraviolet absorber and polyvinylpyrrolidone PVP, dispersed with stirring; Finally, by dry spinning system, the polyurea based formic acid esters solution that contains auxiliary agent is sprayed to silk a stretching, high temperature drying, finish oil, coiling and molding, just obtain easy pore, chromatophilia can spandex.
Description
Technical field
The present invention is a kind of preparation method of porous easy dyeing spandex, belongs to the technology neck that polyurethane elastomeric fiber material is manufacturedTerritory.
Background technology
Polyurethane elastomeric fiber is commonly called as spandex, and its chemical constitution is generally made up of " soft forging " and " firmly forging " two parts. Soft forgingBe generally polyethers, polyester etc., hard forging is generally made up of isocyanates and chain extender (mostly being diamines). Because soft forging and hard forging existBetween thermodynamics incompatibility, form separately independently microcell by scatter-gather, and show vitrifying temperature separatelyDegree, has excellent elastic stretching performance and ultimate strength. Spandex is called textile " industrial monosodium glutamate ", with non-elastic fiberBlending obtains fabric cloth, can greatly improve fabric dress ground comfort property and aesthetics, has become a kind of indispensableOne of textile raw material.
In recent years, along with growth in the living standard, the pursuit of people to clothing is (as color and luster, feel, bar are done, lines homogeneousProperty etc.) improve constantly, the content of some kind spandex is higher, is again to weave with the form of naked silk, and the dyeability of spandex is carriedGone out higher requirement, otherwise under high draw conditions, easily there is " showing money or valuables one carries unintentionally " phenomenon in fabric, thereby affect clothing aesthetics.At present the factor of restriction spandex dyeability mainly contains following two: 1. spandex heat resistance is not good, high temperature (130 DEG C and withOn) while dyeing under condition, spandex performance can occur deteriorated, elasticity, rebound performance will be part of the loss, and therefore cannot dye by high temperatureLook; 2. in spandex chemical constitution, there are a lot of imino groups (NH-), easy and ammonia ester carbonyl group, allophanyl, ester carbonyl group and ehter bondForm comparatively firmly hydrogen bond, thereby hinder dye molecule and the intermolecular generation physics of spandex hydrogen bond association, therefore cannot arriveBest Color.
Up to now, few about the technology report of spandex dyeing, wherein spandex company in Yantai is respectively in patentCN9611599.X discloses the special end-capping reagent of a kind of employingPrepare polyethers easy dyeing spandex. Yantai spandex public affairsDepartment also discloses the special chain extender of a kind of employing in patent CN200710015248.5Prepare polyethersEasy dyeing spandex. Hua Feng spandex company discloses a kind of employing dihydroxylic alcohols, vulcabond in patent CN200910131830.7For raw material, and in pre-collecting process and chain extension process, adopt respectively n-butanol, diethylamine for reaction controlling agent, prepared resistance to heightTemperature, chromophil polyurethane elastic fiber.
Research by us is found: patent CN9611599.X, employingAs terminator method, andPatent CN200910131830.7 and CN200910131830.7 adopt respectively n-butanol, the diethylamine method pair as terminatorThe improvement amplitude of spandex dyeability is little. Patent CN200710015248.5 adoptsAs chain extenderPreparation method can effectively improve the dyeability of spandex under acid dyes, but for comparatively generally adopt at present pointLoose property dyestuff, it is little that its dyeability is improved degree.
Summary of the invention
Technical problem: the object of the invention is to solve above-mentioned the deficiencies in the prior art, provide a kind of porous easily to dye ammoniaThe preparation method of synthetic fibre.
Technical scheme: the preparation method of porous easy dyeing spandex of the present invention comprises following several step:
Step 1. is at the first reactor 1stIn Reactor, add polytetramethylene ether diol PTMG, 4,4-hexichol simultaneouslyMethane diisocyanate 4,4-MDI, fully carries out prepolymerization reaction, obtains the prepolymer PP with-NCO end-blocking;
Step 2., in high speed dissolving machine Dissolver, adopts DMA DMAC as solvent, to pre-polymerizationThing PP fully dissolves, the pre-polymer solution PPs of contained-NCO end-blocking;
Step 3. is at the second reactor 2ndIn Reactor, adopt and contain Diamines chain extender, monoamine terminator and alcoholThe mixed amine DMAC solution of amine carries out chain growth, chain termination to PPs simultaneously, prepares end with-OH polyurea based formic acid estersSolution;
The end that step 4. obtains in step 3 with in-OH polyurea based formic acid esters solution, add antioxidant, lubricant,Delustering agent, ultraviolet absorber and polyvinylpyrrolidone PVP, and carry out abundant dispersed with stirring, slaking, obtain polyurea based formic acid estersSpinning solution;
Step 5., by dry spinning system and technique, is sprayed silk stretching, high temperature to polyurea based formic acid esters spinning solutionDry, finish oils, coiling and molding, just obtain easy pore, chromatophilia can spandex.
Described prepolymerization reaction temperature is 60 DEG C～90 DEG C.
The molecular weight of described polytetramethylene ether diol PTMG is 1500～3000.
In described prepolymer PP-NCO endgroup content is 2.00wt%～2.60wt%.
Diamines in described Diamines chain extender is ethylenediamine, 1,2-propane diamine, 2-methyl isophthalic acid, 5-pentanediamine, tetramethylEthylenediamine, in one or more; Monoamine in monoamine terminator be dimethylamine, diethylamine, di-n-propylamine, one or more;Hydramine is monoethanolamine, diethanol amine, divinyl ethylene glycol amine or isopropanolamine.
Chain extender diamines addition in described mixed amine DMAC solution and chain terminating agent monoamine and the two addition of hydramineMolal quantity ratio be 5～10; In chain terminating agent, the molar ratio of monoamine and hydramine addition is 0.5～10.
Described mixed amine DMAC solution concentration is 3wt%～8wt%; Polyurea based formic acid esters solution concentration be 30wt%～40wt％。
It is 0.5wt%～5wt% that described polyvinylpyrrolidone PVP addition accounts for naked spandex yarn proportion.
The molecular weight of described polyvinylpyrrolidone PVP is 300000～1300000.
In described step 5, on finish, weight of oil accounts for spandex proportion 5wt%～10wt%.
Beneficial effect: the present invention adopts hydramine as part chain terminating agent, and in solution, add auxiliary agent polyethylene pyrrolesAlkane ketone PVP, preparation polyurea based formic acid esters spinning solution, than other preparation method, the method tool has the following advantages: (1) byIn monoethanolamine-in OH end group and prepolymer-NCO end group reactivity is very low, therefore 2ndReactor reactor originallyTemperature low (generally lower than 90 DEG C), and have a large amount of reactivities high-NH2 end group existence condition under ,-OH end group is hardlyReact with-NCO end group; And polymer is in follow-up high temperature path, due to spin speed fast (generally 900m/min and withOn) ,-OH end group and-NCO end group (under hot conditions, monoamine end-blocking can come off obtain-NCO) occurrence probability is little,And then can prepare with part-OH polyurea based formic acid esters solution, therefore can increase the hydrophilicity of polymer, improve and dyeExpect intermolecular hydrogen bond association ability, thereby improve spandex dyeability. (2) PVP, due to its special construction, has good lifeThing compatibility and hydrophily, can improve the tinctorial property of spandex; Because PVP has well water-solublely, in spandex, addThe PVP of certain molecular weight and addition, spandex is in high-temperature dyeing process, and spandex thread surface can form loose structure, Ke YitiHigh spandex specific area, improves spandex Color to reach, and can adopt the PVP of different molecular weight or addition, arrivesTarget dyeability. Due to above advantage, therefore can realize the object of preparation porous easy dyeing spandex.
Brief description of the drawings
Spandex surface topography before Fig. 1 dyes.
Spandex surface topography after Fig. 2 dyes.
Detailed description of the invention
Describe the present invention in detail with example below, but these examples must not be interpreted as and go up in all senses limit of the present inventionSystem.
Embodiment 1
Step 1. is by 395.16kg polytetramethylene ether diol (molecular weight 1800), 89.97kg4, and 4-diphenyl-methane two is differentCyanate is delivered in the first reactor simultaneously, reaction time 2hr, and 80 DEG C of reaction temperatures, obtain prepolymer (PP);
Step 2. is by 469.97kg prepolymer and 573.91kgN, and N-dimethylacetylamide (DMAC) solvent is delivered to simultaneouslyIn high speed dissolving machine, and under the effect of high speed shear power, PP is fully dissolved, obtain pre-polymer solution (PPs);
Step 3. by 1043.88kg pre-polymer solution and 286.57kg mixed amine DMAC solution (comprise 1.02kg propane diamine,7.72kg ethylenediamine, 0.99kg diethylamine, 0.42kg isopropanolamine), under the condition of rapid stirring, occur simultaneously chain growth andChain termination, preparation polyurea based formic acid esters polymer solution;
Step 4. adds 27.48kg to contain antioxidant, lubricant, delustring in the polyurea based formic acid esters solution of step 3Agent and ultraviolet absorber and polyvinylpyrrolidone PVP (PVP accounts for spandex proportion 3.0wt%), and carry out abundant dispersed with stirring, ripeChange, obtain polyurea based formic acid esters spinning solution;
Step 5., by dry spinning system, is sprayed silk stretching, high temperature drying, oil to polyurea based formic acid esters spinning solutionAgent oil (finish accounts for spandex proportion 7%), coiling and molding, just obtain easy pore, chromatophilia can spandex.
Embodiment 2
Step 1. is by 402.50kg polytetramethylene ether diol (molecular weight 1800), 90.17kg4, and 4-diphenyl-methane two is differentCyanate is delivered in the first reactor simultaneously, reaction time 2hr, and 80 DEG C of reaction temperatures, obtain prepolymer (PP);
Step 2. is by 487.12kg prepolymer and 574.42kgN, and N-dimethylacetylamide (DMAC) solvent is delivered to simultaneouslyIn high speed dissolving machine, and under the effect of high speed shear power, PP is fully dissolved, obtain pre-polymer solution (PPs);
Step 3. by 1051.45kg pre-polymer solution and 287.23kg mixed amine DMAC solution (comprise 1.03kg propane diamine,7.69kg ethylenediamine, 0.97kg diethylamine, 0.45kg isopropanolamine), under the condition of rapid stirring, occur simultaneously chain growth andChain termination, preparation polyurea based formic acid esters polymer solution;
Step 4. adds 16.91kg to contain antioxidant, lubricant, delustring in the polyurea based formic acid esters solution of step 3Agent and ultraviolet absorber and polyvinylpyrrolidone PVP (PVP accounts for spandex proportion 1.5wt%), and carry out abundant dispersed with stirring, ripeChange, obtain polyurea based formic acid esters spinning solution;
Step 5., by dry spinning system, is sprayed silk stretching, high temperature drying, oil to polyurea based formic acid esters spinning solutionAgent oil (finish accounts for spandex proportion 6.5%), coiling and molding, just obtain easy pore, chromatophilia can spandex.
Embodiment 3
Step 1. is by 375.87kg polytetramethylene ether diol (molecular weight 1800), 83.52kg4, and 4-diphenyl-methane two is differentCyanate is delivered in the first reactor simultaneously, reaction time 2hr, and 80 DEG C of reaction temperatures, obtain prepolymer (PP);
Step 2. is by 452.43kg prepolymer and 554.82kgN, and N-dimethylacetylamide (DMAC) solvent is delivered to simultaneouslyIn high speed dissolving machine, and under the effect of high speed shear power, PP is fully dissolved, obtain pre-polymer solution (PPs);
Step 3. by 1043.88kg pre-polymer solution and 273.27kg mixed amine DMAC solution (comprise 0.97kg propane diamine,7.12kg ethylenediamine, 0.94kg diethylamine, 0.52kg isopropanolamine), under the condition of rapid stirring, occur simultaneously chain growth andChain termination, preparation polyurea based formic acid esters polymer solution;
Step 4. adds 14.44kg to contain antioxidant, lubricant, delustring in the polyurea based formic acid esters solution of step 3Agent and ultraviolet absorber and polyvinylpyrrolidone PVP (PVP accounts for spandex proportion 1.0wt%), and carry out abundant dispersed with stirring, ripeChange, obtain polyurea based formic acid esters spinning solution;
Step 5., by dry spinning system, is sprayed silk stretching, high temperature drying, oil to polyurea based formic acid esters spinning solutionAgent oil (finish accounts for spandex proportion 6.5%), coiling and molding, just obtain easy pore, chromatophilia can spandex.
Embodiment 4
Step 1. is by 375.81kg polytetramethylene ether diol (molecular weight 1800), 83.49kg4, and 4-diphenyl-methane two is differentCyanate is delivered in the first reactor simultaneously, reaction time 2hr, and 80 DEG C of reaction temperatures, obtain prepolymer (PP);
Step 2. is by 452.12kg prepolymer and 555.29kgN, and N-dimethylacetylamide (DMAC) solvent is delivered to simultaneouslyIn high speed dissolving machine, and under the effect of high speed shear power, PP is fully dissolved, obtain pre-polymer solution (PPs);
Step 3. by 1045.51kg pre-polymer solution and 274.12kg mixed amine DMAC solution (comprise 0.99kg propane diamine,7.31kg ethylenediamine, 0.92kg diethylamine, 0.68kg isopropanolamine), under the condition of rapid stirring, occur simultaneously chain growth andChain termination, preparation polyurea based formic acid esters polymer solution;
Step 4. adds 12.00kg to contain antioxidant, lubricant, delustring in the polyurea based formic acid esters solution of step 3Agent and ultraviolet absorber and polyvinylpyrrolidone PVP (PVP accounts for spandex proportion 0.5wt%), and carry out abundant dispersed with stirring, ripeChange, obtain polyurea based formic acid esters spinning solution;
Step 5., by dry spinning system, is sprayed silk stretching, high temperature drying, oil to polyurea based formic acid esters spinning solutionAgent oil (finish accounts for spandex proportion 5%), coiling and molding, just obtain easy pore, chromatophilia can spandex.
Claims (4)
1. a preparation method for porous easy dyeing spandex, is characterized in that the method comprises following several step:
Step 1. is at the first reactor 1stIn Reactor, add polytetramethylene ether diol PTMG, 4,4-diphenyl-methane simultaneouslyVulcabond 4,4-MDI, fully carries out prepolymerization reaction, obtains the prepolymer PP with-NCO end-blocking;
Step 2., in high speed dissolving machine Dissolver, adopts DMA DMAC as solvent, to prepolymer PPFully dissolve the pre-polymer solution PPs of contained-NCO end-blocking;
Step 3. is at the second reactor 2ndIn Reactor, adopt and contain Diamines chain extender, monoamine terminator and hydramineMixed amine DMAC solution carries out chain growth, chain termination to PPs simultaneously, prepares end with-OH polyurea based formic acid esters solution;
The end that step 4. obtains in step 3 adds antioxidant, lubricant, delustring with in-OH polyurea based formic acid esters solutionAgent, ultraviolet absorber and polyvinylpyrrolidone PVP, and carry out abundant dispersed with stirring, slaking, obtain the spinning of polyurea based formic acid estersSolution;
Step 5. is by dry spinning system and technique, to polyurea based formic acid esters spinning solution spray a silk stretching, high temperature drying,Finish oils, coiling and molding, just obtains the spandex of easy pore, chromatophilia energy;
Wherein,
The molecular weight of described polytetramethylene ether diol PTMG is 1500～3000;
In described prepolymer PP-NCO endgroup content is 2.00wt%～2.60wt%;
Diamines in described Diamines chain extender is ethylenediamine, 1,2-propane diamine, 2-methyl isophthalic acid, 5-pentanediamine, tetramethyl second twoOne or more in amine; Monoamine in monoamine terminator is one or more in dimethylamine, diethylamine, di-n-propylamine; AlcoholAmine is monoethanolamine, diethanol amine, divinyl ethylene glycol amine or isopropanolamine;
Rubbing of chain extender diamines addition in described mixed amine DMAC solution and chain terminating agent monoamine and the two addition of hydramineYour number ratio is 5～10; In chain terminating agent, the molar ratio of monoamine and hydramine addition is 0.5～10;
Described mixed amine DMAC solution concentration is 3wt%～8wt%; Polyurea based formic acid esters solution concentration be 30wt%～40wt％；
It is 0.5wt%～5wt% that described polyvinylpyrrolidone PVP addition accounts for naked spandex yarn proportion.
2. the preparation method of a kind of porous easy dyeing spandex according to claim 1, is characterized in that described prepolymerization reactionTemperature is 60 DEG C～90 DEG C.
3. the preparation method of a kind of porous easy dyeing spandex according to claim 1, is characterized in that described polyethylene pyrrolesThe molecular weight of alkane ketone PVP is 300000～1300000.
4. the preparation method of a kind of porous easy dyeing spandex according to claim 1, is characterized in that finish in described step 5Upper weight of oil accounts for spandex proportion 5wt%～10wt%.
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| CN105177755B (en) * | 2015-07-30 | 2017-05-17 | 浙江华峰氨纶股份有限公司 | High-concentration polyurethane-urea spinning solution and preparation method therefor |
| CN105442083B (en) * | 2015-12-29 | 2017-09-12 | 浙江华峰氨纶股份有限公司 | A kind of preparation method of reactive dye easy dyeing spandex |
| CN106702526B (en) * | 2016-12-15 | 2019-08-20 | 浙江华峰氨纶股份有限公司 | A kind of disperse dyeable and the excellent spandex and preparation method thereof of high temperature resistance |
| CN109537092B (en) * | 2018-11-26 | 2021-01-05 | 华峰重庆氨纶有限公司 | Preparation method of multifunctional polyurethane elastic fiber |
| CN110923844B (en) * | 2019-12-16 | 2022-06-03 | 华峰化学股份有限公司 | Preparation method of spandex easy to unwind |
| CN111424332B (en) * | 2020-04-28 | 2022-07-22 | 华峰化学股份有限公司 | Special spandex for mask belt and preparation method thereof |
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| KR20090073749A (en) * | 2007-12-31 | 2009-07-03 | 주식회사 효성 | Easily dyeable polyurethaneurea spandex yarn and preparing method the same |
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Address after: No. 1788, Dongshan Economic Development Zone, Ruian, Wenzhou, Zhejiang Patentee after: Huafeng Chemical Co.,Ltd. Address before: No. 1788, Dongshan Economic Development Zone, Ruian, Wenzhou, Zhejiang Patentee before: ZHEJIANG HUAFENG SPANDEX Co.,Ltd. |