CN105155017A - Wear-resistant polyurethane elastomeric fiber and preparation method thereof - Google Patents
Wear-resistant polyurethane elastomeric fiber and preparation method thereof Download PDFInfo
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- CN105155017A CN105155017A CN201510449773.2A CN201510449773A CN105155017A CN 105155017 A CN105155017 A CN 105155017A CN 201510449773 A CN201510449773 A CN 201510449773A CN 105155017 A CN105155017 A CN 105155017A
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Abstract
The invention relates to a wear-resistant polyurethane elastomeric fiber and a preparation method thereof, specifically to a polyurethane resin composition containing a wear-resistant aid and the polyurethane fiber with excellent wear resistance prepared from the polyurethane resin composition. The method comprises the following steps: 1) subjecting oligomer dihydric alcohol and excess organic diisocyanate to primary polymerization so as to obtain prepolymer; 2) dissolving the prepolymer in an organic solvent, then reacting the dissolved prepolymer with diamine and monoamine and carrying out secondary polymerization so as to prepare a polyurethane solution; and 3) adding the wear-resistant aid accounting for 0.5 to 10 wt% of the weight of the polyurethane polymer into the polyurethane solution so as to obtain a mixture and carrying out spinning on the mixture so as to obtain the wear-esistant polyurethane elastomeric fiber. The preparation method is simple to implement and can be widely used for polyurethane elastomeric fibers of different kinds; and the prepared polyurethane elastomeric fiber has excellent wear resistance.
Description
Technical field
The present invention relates to a kind of manufacture method of new function spandex fibre, particularly a kind of have well wear-resisting spandex fibre and manufacture method thereof, the invention belongs to field of polymer material preparing technology.
Background technology
Spandex, be a kind of elastomeric textile fabric, have intensity high, light specific gravity under its normal temperature, the advantages such as elastic recovery rate is large, are widely used in fabric.
As everyone knows, people are no matter in work or study, and motion is continual, at some position of clothing, such as knee joint, elbow joint place, the wearing and tearing of clothing and be out of shape often serious than other position.We can find often at these positions due to long stress deformation, and cause clothing surface can produce projection, lose shape, even damaged, have had a strong impact on the aesthetics of clothing, have reduced the serviceability of clothing.This is mainly because fabric is in reciprocal transformation Recovery Process, and the fiber that spandex fibre manufactures together with other also exists reciprocating friction, and friction can make spandex fibre surface loss, reduces the resilience of spandex fibre.Along with national life level improves constantly, higher requirement be it is also proposed to snugness of fit and fashion.In order to effectively address this problem, need to develop a kind of wear-resisting spandex fibre, to improve the anti-wear performance of spandex fabric.
At present, the patented technology in wear-resisting spandex fibre production and document less, therefore, need develop a kind of new technology of producing wear-resisting spandex fibre, with meet spandex fibre manufacturing technology and garment industry development demand.
Summary of the invention
Technical problem: the technical problem that quasi-solution of the present invention is determined is a kind of wear-resisting spandex fibre preparation method of design.The implementation process of this preparation method is easy, and can be widely used in the polyurethane elastomeric fiber of different cultivars, and the polyurethane elastomeric fiber anti-wear performance of preparation is excellent, can reduce fabric face projection, lose shape, even damaged phenomenon.
Technical scheme: for achieving the above object, the technical solution used in the present invention is as follows:
A preparation method for abrasion resistant polyurethane elastomer, is characterized in that, comprises the steps:
1), by oligomer dihydroxylic alcohols and excessive organic diisocyanate 100 ~ 120min is reacted at 75 ~ 90 DEG C,
Once be polymerized, prepare prepolymer; Wherein the mol ratio of vulcabond and oligomer dihydroxylic alcohols is (1.50 ~ 2.00): 1;
2), described prepolymer is dissolved in organic solvent, then carries out after polymerization to prepare polyurethane solutions with the mixed amine solution reaction of diamines and monoamine;
The mass percent concentration of described mixed amine solution is 1.00 ~ 8.00%;
Described polyurethane solutions mass percent concentration is 30 ~ 45%, and wherein the molal quantity of amido and the mole ratio of isocyanate group are (0.90 ~ 1.30): 1,
3), by antiwear assistant and auxiliary material auxiliary agent join in solvent and mix, and grind 20 ~ 40 hours, forming mass percent concentration is the auxiliary agent slurry of 30 ~ 40%;
4), described auxiliary agent slurry is added to obtain mixture in above-mentioned polyurethane solutions by the certain proportion of polyether polyols with reduced unsaturation weight, stirred slaking through 30 ~ 40 hours, described mixture is carried out spinning, obtains abrasion resistant polyurethane elastomer.
Preferably, described organic solvent is DMF DMF or DMA DMAC, described diamines is ethylenediamine and propane diamine wherein a kind of or mixture both it, and monoamine is diethylamine and di-n-propylamine wherein a kind of or mixture both it.Described vulcabond is 4,4 '-MDI or 2,4 '-MDI, or both mixtures.
Preferably, described step 3) in add antiwear assistant component comprise: surface modifier, nano-oxide, catalyst and dispersion solvent.
Preferably, described surface modifier is the surface modifier containing isopropoxy and organic long-chain.
Preferably, described surface modifier is titanate coupling agent.Titanate coupling agent contains an isopropoxy and 3 longer organic long-chains, isopropoxy can with the hydroxyl reaction of particle surface, form chemical bond, make to isolate between particle and particle.
Preferably, described dispersion solvent is acetone, and described catalyst is p-methyl benzenesulfonic acid.Nano-oxide is main body; Acetone is dispersion solvent, and nano-oxide is diluted, first dispersion to a certain extent; P-methyl benzenesulfonic acid is catalyst, makes titanate coupling agent and the more effective reaction of nano-oxide.
Preferably, the preparation method of described antiwear assistant is as follows:
1) by surface modifier with nano-oxide, dispersion solvent and catalyst according to mass percent: the ratio of 0.1 ~ 1:1:7:0.025 mixes, mechanical agitation 2h, makes it fully to mix, and prepares nano-oxide mixed liquor;
The content of each component combines the effect and the consideration of cost aspect that reach, and through the best proportion that test of many times obtains, if nano oxidized substrate concentration is too high, obtain dispersion effect difference in the solution, if too low, treatment effeciency is low, the wasting of resources; As a same reason, if catalyst p-methyl benzenesulfonic acid is too low, efficiency is not high; Too high, the wasting of resources.
2) by above-mentioned nano-oxide mixed liquor, through 40 ~ 45 DEG C of dryings, after desolventizing, and it is fully ground obtained antiwear assistant.
Preferably, it is characterized in that described nano-oxide is that the aluminium oxide of particle diameter 1-100 nanometer and silica are wherein a kind of, or two mixtures.The particle diameter of nano-oxide has direct impact to the film-nuclear structure formed, nano-oxide particle diameter is 30-70 nanometer more preferably, if particle diameter is excessive, in film-nuclear structure, the ratio of film just have dropped relatively, the stability of film-nuclear structure can be affected, indirectly cause its dispersion effect.
Preferably, it is characterized in that described antiwear assistant accounts for 0.5 ~ 10wt% of polyether polyols with reduced unsaturation weight.Equally, the accounting of antiwear assistant is also combine the best proportion effect that reaches and cost aspect considering to obtain through test of many times, when content lower than 0.5% time, abrasion resistant effect is bad, and higher than 10% time, greatly can improve the price of polyurethane elastomeric fiber, be unfavorable for that spandex fibre is competed in the market.
Preferably, it is characterized in that described auxiliary material auxiliary agent comprises: anti ultraviolet agent, antioxidant, lubricant, delustering agent.
Preferably, described oligomer polybinary alcohol be the polypropylene glycol of the PTMG of number-average molecular weight 1500 ~ 3000 or number-average molecular weight 1500 ~ 3000 also or both mixtures.
The present invention is open abrasion resistant polyurethane elastomer obtained by described manufacture method and the application in textile fabric thereof also.
The beneficial effect that the present invention has:
(1) the present invention relates to a kind of abrasion resistant polyurethane elastomer and preparation method thereof, prepared product is except normally can keeping the conventional index of like product, anti-wear performance can also be had, greatly can improve spandex fibre and other fiber abrasion phenomenons in spandex fabric, make spandex fibre keep original resilience;
(2) design and synthesis has the antiwear assistant of " film-core " structure---and " titanate coupling agent-nano-oxide ", its advantage is, one is the antiwear assistant of " film-core " structure, effectively can solve nano material easily to reunite this problem, two is that the titanate coupling agent that outer wrap can improve the interface binding power with polyurethane fiber, can improve spandex fibre in weaving process, occur dry linting phenomenon;
(3) manufacturing technique of the present invention is ripe, does not have particular/special requirement to equipment, and industrializing implementation is easy, and functional material is with low cost, is convenient to promote.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, but protection scope of the present invention is not only confined to embodiment.
1) by material oligomer dihydroxylic alcohols and vulcabond mixing, at 75 ~ 90 DEG C of reaction 100 ~ 120min, prepare prepolymer, wherein the mol ratio of vulcabond and oligomer dihydroxylic alcohols is (1.50 ~ 2.00): 1;
2) prepare mixed amine solution: by one or both in ethylenediamine, propane diamine, be dissolved into solvent, then add one or both in diethylamine, di-n-propylamine, form the mixed amine solution that mass percent concentration is 1.00 ~ 8.00%;
3) described mixed amine solution to be joined in described pre-polymer solution and to stir, wherein the molal quantity of amido and the mole ratio of isocyanate group are (0.90 ~ 1.30): 1, react, forming mass percent concentration is the polymer solution of 30 ~ 45%;
4) prepare antiwear assistant: by titanate coupling agent with nano-oxide, acetone and p-methyl benzenesulfonic acid according to mass percent: the ratio of 0.1 ~ 1:1:7:0.025 mixes, mechanical agitation 2h, make it fully to mix, prepare nano-oxide mixed solution, again through 40 ~ 45 DEG C of temperature dryings after suction filtration, after desolventizing, and it is fully ground.
5) slurry of preparation containing antiwear assistant: by general auxiliary agents such as anti ultraviolet agent, antioxidant, lubricant, delustering agents, N is joined with energy antiwear assistant, grind 20 ~ 40 hours in N-dimethylacetylamide, forming mass percent concentration is the auxiliary agent slurry of 30 ~ 40%;
6) described auxiliary agent slurry is added in described polymer solution, stirred slaking through 30 ~ 40 hours, by dry spinning, form abrasion resistant polyurethane elastomer.
Described oligomer polybinary alcohol be the polypropylene glycol of the PTMG of number-average molecular weight 1500 ~ 3000 or number-average molecular weight 1500 ~ 3000 also or both mixtures.
Described vulcabond is 4,4 '-MDI or 2,4 '-MDI, or both mixtures; The solvent added is DMF DMF or DMA DMAC.
Described mixed amine solution is chain extender and chain terminating agent mixed solution, and chain extender is selected from ethylenediamine, propane diamine or its mixture; Chain terminating agent is diethylamine, di-n-propylamine or its mixture.
Described nano-oxide be for the aluminium oxide of particle diameter 1-100 nanometer and silica wherein a kind of, or two mixtures.
Abrasion loss is tested:
This is an important indicator being used for evaluating abrasive resistance.Polyurethane stock solution after slaking is carried out knifing, then dries 6h, except desolventizing with 60 DEG C of baking ovens; Clip sample diameter is 38mm, and adopt the wear-resisting and pilling tester of Nu-Martindale to test, experiment load mass is 595g, and testing revolution is 5000 turns; Before and after wear test, its quality is weighed.
Abrasion loss ML is defined as
wherein ML represents the abrasion loss of sample, Mo represent the non-experience wear of sample before the quality of sample, Mf represents the quality of sample sample after wear testing.
Embodiment 1:
1) by raw material polytetramethylene ether diol and 4,4 '-methyl diphenylene diisocyanate mixes, and at 90 DEG C of reaction 120min, prepares prepolymer, wherein 4, the mol ratio of 4 '-methyl diphenylene diisocyanate and polytetramethylene ether diol is 1.73:1;
2) prepare mixed amine solution: by ethylenediamine, propane diamine 5:1 in molar ratio, be dissolved into solvent DMA, then add diethylamine with diamines molar content 15%, form the mixed amine solution that mass percent concentration is 5.00%;
3) being joined by described mixed amine solution in described pre-polymer solution and to stir, wherein the molal quantity of amido and the mole ratio of isocyanate group are 1.06:1, react, and forming mass percent concentration is the polymer solution of 35%;
4) method of antiwear assistant is prepared: titanate coupling agent and nano aluminium oxide, acetone and p-methyl benzenesulfonic acid are added according to the ratio that mass percent is 0.1:1:7:0.025, stir 2 hours, after mixing, again through 45 DEG C of temperature dryings after suction filtration, removing surface solvent, and it is fully ground;
5) slurry of preparation containing antiwear assistant: by the solid content meter of polymer, by the 2-of 0.5wt% (2 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl)-benzotriazole), two (the amino 4-phenyl of N, N-dimethyl-hydrazine) methane of 0.5wt%, the dolomol of 0.1wt%, 0.5wt% titanium dioxide, the antiwear assistant of 0.5wt% joins N, grind 30 hours in N-dimethylacetylamide, forming mass percent concentration is the auxiliary agent slurry of 35%;
6) described antiwear assistant slurry is added in described polymer solution, stirred slaking through 35 hours, by dry spinning, form abrasion resistant polyurethane elastomer.
Evaluate its abrasion loss, evaluation result is shown in following table 1.
Embodiment 2:
1) by raw material polytetramethylene ether diol and 4,4 '-methyl diphenylene diisocyanate mixes, and at 90 DEG C of reaction 120min, prepares prepolymer, wherein 4, the mol ratio of 4 '-methyl diphenylene diisocyanate and polytetramethylene ether diol is 1.73:1;
2) prepare mixed amine solution: by ethylenediamine, propane diamine 5:1 in molar ratio, be dissolved into solvent DMA, then add diethylamine with diamines molar content 15%, form the mixed amine solution that mass percent concentration is 5.00%;
3) being joined by described mixed amine solution in described pre-polymer solution and to stir, wherein the molal quantity of amido and the mole ratio of isocyanate group are 1.06:1, react, and forming mass percent concentration is the polymer solution of 35%;
4) method of antiwear assistant is prepared: titanate coupling agent and nano aluminium oxide, acetone and p-methyl benzenesulfonic acid are added according to the ratio that mass percent is 0.5:1:7:0.025, stir 2 hours, after mixing, again through 40 DEG C of temperature dryings after suction filtration, removing surface solvent, and it is fully ground;
5) slurry of preparation containing antiwear assistant: by the solid content meter of polymer, by the 2-of 0.5wt% (2 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl)-benzotriazole), two (the amino 4-phenyl of N, N-dimethyl-hydrazine) methane of 0.5wt%, the dolomol of 0.1wt%, 0.5wt% titanium dioxide, the antiwear assistant of 5wt% joins N, grind 30 hours in N-dimethylacetylamide, forming mass percent concentration is the auxiliary agent slurry of 35%;
6) described antiwear assistant slurry is added in described polymer solution, stirred slaking through 35 hours, by dry spinning, form abrasion resistant polyurethane elastomer.
Evaluate its abrasion loss, evaluation result is shown in following table 1.
Embodiment 3:
1) by raw material polytetramethylene ether diol and 4,4 '-methyl diphenylene diisocyanate mixes, and at 90 DEG C of reaction 120min, prepares prepolymer, wherein 4, the mol ratio of 4 '-methyl diphenylene diisocyanate and polytetramethylene ether diol is 1.73:1;
2) prepare mixed amine solution: by ethylenediamine, propane diamine 5:1 in molar ratio, be dissolved into solvent DMA, then add diethylamine with diamines molar content 15%, form the mixed amine solution that mass percent concentration is 5.00%;
3) being joined by described mixed amine solution in described pre-polymer solution and to stir, wherein the molal quantity of amido and the mole ratio of isocyanate group are 1.06:1, react, and forming mass percent concentration is the polymer solution of 35%;
4) method of antiwear assistant is prepared: titanate coupling agent and nano aluminium oxide, acetone and p-methyl benzenesulfonic acid are added according to the ratio that mass percent is 1:1:7:0.025, stir 2 hours, after mixing, again through 45 DEG C of temperature dryings after suction filtration, removing surface solvent, and it is fully ground;
5) slurry of preparation containing antiwear assistant: by the solid content meter of polymer, by the 2-of 0.5wt% (2 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl)-benzotriazole), two (the amino 4-phenyl of N, N-dimethyl-hydrazine) methane of 0.5wt%, the dolomol of 0.1wt%, 0.5wt% titanium dioxide, the antiwear assistant of 10wt% joins N, grind 30 hours in N-dimethylacetylamide, forming mass percent concentration is the auxiliary agent slurry of 35%;
6) described antiwear assistant slurry is added in described polymer solution, stirred slaking through 35 hours, by dry spinning, form abrasion resistant polyurethane elastomer.
Evaluate its abrasion loss, evaluation result is shown in following table 1.
Comparative example 1:
Except not adding except antiwear assistant inside slurry, press and the same procedure acquisition pattern solution described in embodiment 1.Stir slaking through 35 hours, by dry spinning, form conventional polyurethanes elastomer.
Evaluate its abrasion loss, evaluation result is shown in following table 1.
Table 1 abrasion loss test result
| Sample | Abrasion loss/% |
| Comparative example 1 | 2.26 |
| Embodiment 1 | 1.25 |
| Embodiment 2 | 0.88 |
| Embodiment 3 | 0.72 |
As shown in Table 1, the abrasion resistant polyurethane elastomer that the present invention obtains is compared common polyurethane elastomeric fiber and is had more excellent anti-wear performance.
Last it is noted that above embodiment only in order to illustrate the present invention and and unrestricted technical scheme described in the invention; Therefore, although this description with reference to each above-mentioned embodiment to present invention has been detailed description, those of ordinary skill in the art should be appreciated that and still can modify to the present invention or equivalent to replace; And all do not depart from technical scheme and the improvement thereof of the spirit and scope of the present invention, it all should be encompassed in right of the present invention.
Claims (10)
1. a preparation method for abrasion resistant polyurethane elastomer, is characterized in that, comprises the steps:
1), by oligomer dihydroxylic alcohols and excessive organic diisocyanate 100 ~ 120min is reacted at 75 ~ 90 DEG C,
Once be polymerized, prepare prepolymer; Wherein the mol ratio of vulcabond and oligomer dihydroxylic alcohols is (1.50 ~ 2.00): 1;
2), described prepolymer is dissolved in organic solvent, then carries out after polymerization to prepare polyurethane solutions with the mixed amine solution reaction of diamines and monoamine;
The mass percent concentration of described mixed amine solution is 1.00 ~ 8.00%;
Described polyurethane solutions mass percent concentration is 30 ~ 45%, and wherein the molal quantity of amido and the mole ratio of isocyanate group are (0.90 ~ 1.30): 1,
3), by antiwear assistant and auxiliary material auxiliary agent join in solvent and mix, and grind 20 ~ 40 hours, forming mass percent concentration is the auxiliary agent slurry of 30 ~ 40%;
4), described auxiliary agent slurry is added to obtain mixture in above-mentioned polyurethane solutions by the certain proportion of polyether polyols with reduced unsaturation weight, stirred slaking through 30 ~ 40 hours, described mixture is carried out spinning, obtains abrasion resistant polyurethane elastomer.
2. the preparation method of abrasion resistant polyurethane elastomer according to claim 1, it is characterized in that, described organic solvent is N, dinethylformamide DMF or N, N-dimethylacetylamide DMAC, described diamines is ethylenediamine and propane diamine wherein a kind of or mixture both it, and monoamine is diethylamine and di-n-propylamine wherein a kind of or mixture both it.
3. the preparation method of abrasion resistant polyurethane elastomer according to claim 1, is characterized in that, described step 3) in add antiwear assistant component comprise: surface modifier, nano-oxide, catalyst and dispersion solvent.
4. the preparation method of abrasion resistant polyurethane elastomer according to claim 1, is characterized in that, described surface modifier is the surface modifier containing isopropoxy and organic long-chain.
5. the preparation method of abrasion resistant polyurethane elastomer according to claim 4, is characterized in that, described surface modifier is titanate coupling agent.
6. the preparation method of abrasion resistant polyurethane elastomer according to claim 5, is characterized in that, described dispersion solvent is acetone, and described catalyst is p-methyl benzenesulfonic acid.
7. the preparation method of abrasion resistant polyurethane elastomer according to claim 6, is characterized in that, the preparation method of described antiwear assistant is as follows:
1) by surface modifier with nano-oxide, dispersion solvent and catalyst according to mass percent: the ratio of 0.1 ~ 1:1:7:0.025 mixes, mechanical agitation 2h, makes it fully to mix, and prepares nano-oxide mixed liquor;
2) by above-mentioned nano-oxide mixed liquor, through 40 ~ 45 DEG C of dryings, after desolventizing, and it is fully ground obtained antiwear assistant.
8. the preparation method of antiwear assistant according to claim 3, is characterized in that described nano-oxide is that the aluminium oxide of particle diameter 1-100 nanometer and silica are wherein a kind of, or two mixtures.
9. the preparation method of abrasion resistant polyurethane elastomer according to claim 1, is characterized in that described antiwear assistant accounts for 0.5 ~ 10wt% of polyether polyols with reduced unsaturation weight.
10. the preparation method of abrasion resistant polyurethane elastomer according to claim 1, is characterized in that described auxiliary material auxiliary agent comprises: anti ultraviolet agent, antioxidant, lubricant, delustering agent.
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| CN106349682A (en) * | 2016-08-30 | 2017-01-25 | 郑明耀 | Nano fibrous material used for making shoes |
| CN106637596A (en) * | 2016-12-26 | 2017-05-10 | 康濑轻工业品（昆山）有限公司 | High-elasticity spandex fabric and preparation process thereof |
| CN106757487A (en) * | 2016-12-16 | 2017-05-31 | 浙江华峰氨纶股份有限公司 | Flexible heating polyurethane fiber of one kind and preparation method thereof |
| CN106978664A (en) * | 2017-02-26 | 2017-07-25 | 浙江峰赫纺织有限公司 | A kind of good sofa fabric of wearability |
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| CN105506777A (en) * | 2016-01-26 | 2016-04-20 | 浙江华峰氨纶股份有限公司 | Polyurethane elastic fiber easy to adhere and preparation method thereof |
| CN106349682A (en) * | 2016-08-30 | 2017-01-25 | 郑明耀 | Nano fibrous material used for making shoes |
| CN106757487A (en) * | 2016-12-16 | 2017-05-31 | 浙江华峰氨纶股份有限公司 | Flexible heating polyurethane fiber of one kind and preparation method thereof |
| CN106757487B (en) * | 2016-12-16 | 2019-03-26 | 浙江华峰氨纶股份有限公司 | Flexible fever polyurethane fiber of one kind and preparation method thereof |
| CN106637596A (en) * | 2016-12-26 | 2017-05-10 | 康濑轻工业品（昆山）有限公司 | High-elasticity spandex fabric and preparation process thereof |
| CN106978664A (en) * | 2017-02-26 | 2017-07-25 | 浙江峰赫纺织有限公司 | A kind of good sofa fabric of wearability |
| CN111393829A (en) * | 2020-04-21 | 2020-07-10 | 东莞市雄林新材料科技股份有限公司 | TPU film for express packaging and preparation method thereof |
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Application publication date: 20151216 |