CN103993379A - Method for preparing polyurethane elastic fiber with high production efficiency - Google Patents
Method for preparing polyurethane elastic fiber with high production efficiency Download PDFInfo
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Abstract
The invention relates to a method for preparing a polyurethane elastic fiber with high production efficiency. The method comprises the following steps: (1) mixing a component a and oligomeric polyalcohol, and uniformly stirring, thereby forming a stable mixture, wherein the component a consists of a nonionic surfactant and an organic solvent; (2) adding diisocyanate into the mixture, and fully reacting, thereby obtaining an isocyanate blocked prepolymer solution; (3) performing a chain extension reaction on the prepolymer by a mixed amine solution, thereby generating a polyurethane stock solution; (4) adding a component b into the polyurethane stock solution, and stirring and curing to obtain a spinning solution, wherein the component b consists of a nonionic surfactant, an anionic surfactant and an organic solvent; and (5) performing dry spinning on the spinning solution to prepare the polyurethane elastic fiber. The prepared polyurethane elastic fiber has high breaking strength and elongation at break. Therefore, the method can meet the requirement of a high-speed spinning process, and the production efficiency can be obviously improved.
Description
Technical field
The present invention relates to a kind of technology of preparing of the polyurethane elastomeric fiber with high efficiency, also relate to a kind of method that improves polyurethane elastomeric fiber elastic performance, belong to polyurethane elastomeric fiber technical field.More specifically, the present invention relates to have by adding surfactant to make the polyurethane elastomeric fiber of excellent resilience performance, can meet the requirement of high-speed spinning technique.
Background technology
Polyurethane elastomeric fiber has excellent intensity, high extension at break and the elastic recovery rate of drawing high, and is widely used in the elastic fabric such as knitting and woven.Along with social development and the aggravation of market competition, people are also pursuing higher production efficiency and production capacity, and can reduce costs.In order to meet above-mentioned requirements, can suitably shorten polymerization time on the one hand; Can improve on the other hand spinning speed, and the raising of spinning speed certainly will cause the decline of polyurethane elastomeric fiber elastic performance.Therefore develop the technology that can improve polyurethane elastomeric fiber fracture strength and extension at break high speed spinning is just seemed to particularly necessary.
Segmented polyurethane phenyl ring, urea groups and carbamate polarity is strong, cohesive energy is high, easily form intermolecular or intramolecular physical crosslinking, the viscosity of polyurethane stock solution system is raise, and can generating portion gel, be unfavorable for the processing and forming in later stage.High production efficiency generally needs high concentration, therefore its requirement to production technology is higher, under higher concentration, the stability of stoste also can variation, and cohesive energy has exceeded limiting value, when having improved spinning speed, stoste shortened again through the time of spinnerets, and the cohesive energy of stoste system has little time effective release, thereby made strand generation cohesive force cut off in spinnerets exit, form fracture of wire, reduced spinnability.Meanwhile, the raising of spinning speed can make the crystallinity of polyurethane strand, the degree of orientation increase, and causes the spring function of fiber impaired, affects product quality.
Surfactant is the material that a class has amphiphile, amphiphilic molecule structure, can improve interface state and the physicochemical property of solution system, due to homogenizing and the hydrotropy effect of surfactant, the uniformity of polyurethane stock solution microstructure be improved, the unstability of eliminating stoste, suitably reduces cohesive energy.Meanwhile, the use of surfactant in polyurethane stock solution can make the adhesion cross flow of stoste at spinnerets wall, and all makes moderate progress in the extrusion swelling phenomenon in spinnerets exit, improved the spinning property of stoste.But in the time of single use certain or certain class surfactant, its large usage quantity, can cause surfactant and stoste compatibility variation, infringement spinnability and fibrous mechanical property.Even consumption is less, under general process conditions, the use of single surfactant to fibrous elasticity performance to improve effect also also not obvious.
Summary of the invention
Technical problem: in order to solve the problem existing in background technology, the object of this invention is to provide a kind of preparation method of the polyurethane elastomeric fiber with high efficiency, first add surfactant by original position, the compound system that then adds again surfactant in stoste provides a kind of preparation method of the polyurethane elastomeric fiber with high efficiency.The polyurethane elastomeric fiber that process according to the present invention makes has high fracture strength and elongation at break, is applicable to the requirement of high-speed spinning technique, and can shorten the time of polymerisation, obviously enhances productivity.
Technical scheme: the invention provides a kind of preparation method of the polyurethane elastomeric fiber with high efficiency, it comprises the following steps:
1) component a is joined in oligomer polyol, fully mix by powerful mechanical agitation, form stable mixture system;
2) in above-mentioned system, add vulcabond, under the condition of 25～55 DEG C, react 60～120min, obtain having the pre-polymer solution of isocyano end-blocking;
3) pre-polymer solution obtaining is cooled to after 3～25 DEG C, adds mixed amine solution to carry out chain extending reaction, generate polyurethane stock solution;
4) be fully uniformly mixed to adding components b, antioxidant, ultra-violet absorber, anti-yellow agent, lubricant, dyeing assistant in above-mentioned polyurethane stock solution, after slaking, obtain spinning solution;
5) above-mentioned spinning solution is carried out to dry spinning, obtain polyurethane elastomeric fiber;
Wherein: component a is made up of non-ionic surface active agent and the organic solvent with general formula I structure, and R in formula
1, R
2, R
3for carbon number be 1～16 straight chain, side chain or cyclic alkyl;
Components b by thering is the non-ionic surface active agent of general formula II～V structure, anion surfactant and the organic solvent with general formula VI～IX structure forms; R in general formula II～IX
4for carbon number be 8～18 straight chain, side chain or cyclic alkyl, R
5for straight chain, side chain or cyclic alkyl that carbon number is 2～20, M is alkali metal, alkaline-earth metal, ammonium or organic amine, x, y, z=1～30, n=1～10;
In described component a, the mass percent of non-ionic surface active agent in polyurethane elastomeric fiber is 0.005%～0.02%; In components b, the mass ratio of non-ionic surface active agent and anion surfactant is 1: 1～4: 1, and the mass percent of the two total amount in polyurethane elastomeric fiber is 0.03%～1.5%.
Described oligomer polyol is that molecular weight is 1000～3000 polytetramethylene ether diol or polypropylene glycol, also or both mixtures.
Described vulcabond is 4,4 '-methyl diphenylene diisocyanate or 2, and 4 '-methyl diphenylene diisocyanate, also or both mixtures, and the mol ratio of vulcabond and oligomer polyol is 1: 1.6～1: 2.2.
Described mixed amine solution is made up of chain extender, chain terminating agent and organic solvent, wherein the mol ratio of chain extender and chain terminating agent is 2: 1～25: 1, chain extender is unbranched chain extender ethylenediamine, 1,3-propane diamine or 1, one or more in 4-butanediamine, chain terminating agent is one or more that are selected from diethylamine, monoethanolamine or diisopropylamine or dibutyl amine.
Described chain extender is unbranched chain extender and the mixture with side chain chain extender, wherein unbranched chain extender accounts for 80%～99% of chain extender integral molar quantity, account for 1%～20% of chain extender integral molar quantity with side chain chain extender, band side chain chain extender is one or more in 1,2-propane diamine or 2 methyl pentamethylenediamine or NEED.
The solid content of the spinning solution of described polyurethane elastomeric fiber is 30wt%～45wt%.
Described organic solvent is DMF or DMA.
Beneficial effect: the present invention is under specific process conditions, the method that adopts two steps to add surfactant is prepared polyurethane elastomeric fiber, first in pre-polymerization process, add non-ionic surface active agent, utilize the infiltration of non-ionic surface active agent and emulsification make mixed system more evenly, polymerization process is more stable, can effectively shorten polymerization time simultaneously; Then in the maturing process of polyurethane stock solution, add the compound system of non-ionic surface active agent and anion surfactant, by both cooperative effects, can effectively reduce the use amount of surfactant, intermolecular or intramolecular unordered unsettled hydrogen bond in polyurethane stock solution system is adjusted simultaneously, to obtain hard section of uniform and stable region, and promotion microphase-separated, thereby the spinnability of stoste and the elastic performance of fiber are improved, can meet the requirement of high-speed spinning process, reach the object of High-efficient Production.
Detailed description of the invention
The preparation method of a kind of polyurethane elastomeric fiber with high efficiency of the present invention comprises the following steps:
1) component a is joined in oligomer polyol, fully mix by powerful mechanical agitation, form stable mixture system;
2) in above-mentioned system, add vulcabond, under the condition of 25～55 DEG C, react 60～120min, obtain having the pre-polymer solution of isocyano end-blocking;
3) pre-polymer solution obtaining is cooled to after 3～25 DEG C, adds mixed amine solution to carry out chain extending reaction, generate polyurethane stock solution;
4) be fully uniformly mixed to adding components b, antioxidant, ultra-violet absorber, anti-yellow agent, lubricant, dyeing assistant in above-mentioned polyurethane stock solution, after slaking, obtain spinning solution;
5) above-mentioned spinning solution is carried out to dry spinning, obtain polyurethane elastomeric fiber.
The preparation method of a kind of polyurethane elastomeric fiber with high efficiency of the present invention, wherein said component a is made up of non-ionic surface active agent and the organic solvent with general formula I structure, and R in formula
1, R
2, R
3for carbon number be 1～16 straight chain, side chain or cyclic alkyl.
In described component a, the mass percent of non-ionic surface active agent in polyurethane elastomeric fiber is 0.005%～0.02%.
Described components b by thering is the non-ionic surface active agent of general formula II～V structure, anion surfactant and the organic solvent with general formula VI～IX structure forms; R in general formula II～IX
4for carbon number be 8～18 straight chain, side chain or cyclic alkyl, R
5for straight chain, side chain or cyclic alkyl that carbon number is 2～20, M is alkali metal, alkaline-earth metal, ammonium or organic amine, x, y, z=1～30, n=1～10.
In described components b, the mass ratio of non-ionic surface active agent and anion surfactant is 1: 1～4: 1, and the mass percent of the two total amount in polyurethane elastomeric fiber is 0.03%～1.5%.
The preparation method of a kind of polyurethane elastomeric fiber with high efficiency of the present invention, wherein said step 1) in oligomer polyol be that molecular weight is 1000～3000 polytetramethylene ether diol or polypropylene glycol, also or both mixtures.
The preparation method of a kind of polyurethane elastomeric fiber with high efficiency of the present invention, wherein said step 2) in vulcabond be 4,4 '-methyl diphenylene diisocyanate or 2,4 '-methyl diphenylene diisocyanate, also or both mixtures, and the mol ratio of vulcabond and oligomer polyol is 1: 1.6～1: 2.2.
The preparation method of a kind of polyurethane elastomeric fiber with high efficiency of the present invention, wherein said step 3) in mixed amine solution formed by chain extender, chain terminating agent and organic solvent, wherein the mol ratio of chain extender and chain terminating agent is 2: 1～25: 1, chain extender is unbranched chain extender ethylenediamine, 1,3-propane diamine or 1, one or more in 4-butanediamine, chain terminating agent is one or more that are selected from diethylamine, monoethanolamine or diisopropylamine or dibutyl amine.
The preparation method of a kind of polyurethane elastomeric fiber with high efficiency of the present invention, wherein said chain extender is unbranched chain extender and the mixture with side chain chain extender, wherein unbranched chain extender accounts for 80%～99% of chain extender integral molar quantity, account for 1%～20% of chain extender integral molar quantity with side chain chain extender, band side chain chain extender is one or more in 1,2-propane diamine or 2 methyl pentamethylenediamine or NEED.
The preparation method of a kind of polyurethane elastomeric fiber with high efficiency of the present invention, wherein said step 4) in antioxidant can be 245, ultra-violet absorber can be UV-320, anti-yellow agent can be UDT, lubricant can be dolomol, dyeing assistant can be SAS.
The preparation method of a kind of polyurethane elastomeric fiber with high efficiency of the present invention, the solid content of the spinning solution of wherein said polyurethane elastomeric fiber is 30wt%～45wt%.
The preparation method of a kind of polyurethane elastomeric fiber with high efficiency of the present invention, wherein said organic solvent is DMF or DMA.
The preparation method of a kind of polyurethane elastomeric fiber with high efficiency of the present invention, wherein said step 5) in dry spinning be that spinning solution is extruded by spinnerets after filtering, by high temperature path, through false twisting, oil and reel and make polyurethane elastomeric fiber.
For further illustrating the present invention, describe specific operation process of the present invention in detail by specific embodiment below, but these embodiment must not be interpreted as the limitation of the present invention going up in all senses.In addition should be understood that and reading after content of the present invention, the various changes that those skilled in the art can do the present invention, these equivalent form of values belong to the application's claims limited range equally.
Embodiment 1:
The DMA solution of the surfactant of 250g (concentration is 1%) is joined in the DMA and 10.0kg polytetramethylene ether diol solution of 5.0kg, stir.Then add 4 of 2.5kg, 4 '-methyl diphenylene diisocyanate reacts 80min under 40 DEG C of conditions, then adds the DMA of 11.38kg to stir, and obtains the pre-polymer solution of isocyano end-blocking.
Pre-polymer solution is cooled to after 5 DEG C, in 80min, progressively add 1 of ethylenediamine that 6.35kg contains 223.9g, 30.7g, the N of the diethylamine of 2-propane diamine, 45.1g, N-dimethylacetamide solution carries out chain extending reaction and generates polyurethane stock solution, then the compound system solution (concentration is 10%) that adds the Polyethylene Octylphenol Ether of 25.7g and the DBSA triethanolamine of 12.8g, finally adds antioxidant, ultra-violet absorber, anti-yellow agent, lubricant, dyeing assistant to obtain spinning solution.
Above-mentioned spinning solution, after slaking, filtration, deaeration, is carried out to dry spinning with the speed of 900m/min, produce the polyurethane elastomeric fiber of 22dtex/2f.
Embodiment 2:
Prepare polyurethane elastomeric fiber according to the same method described in embodiment 1, difference is, spinning speed is 1200m/min.
Embodiment 3:
Prepare polyurethane elastomeric fiber according to the same method described in embodiment 1, difference is, has added the compound system solution (concentration is 10%) of the Polyethylene Octylphenol Ether of 12.8g and the DBSA triethanolamine of 25.7g in polyurethane stock solution.
Embodiment 4:
Prepare polyurethane elastomeric fiber according to the same method described in embodiment 1, difference is, has added the compound system solution (concentration is 10%) of the Polyethylene Octylphenol Ether of 25.7g and the DBSA triethanolamine of 25.7g in polyurethane stock solution.
Embodiment 5:
Prepare polyurethane elastomeric fiber according to the same method described in embodiment 1, difference is, has added the compound system solution (concentration is 10%) of the Polyethylene Octylphenol Ether of 2.6g and the DBSA triethanolamine of 1.3g in polyurethane stock solution.
Embodiment 6:
Prepare polyurethane elastomeric fiber according to the same method described in embodiment 1, difference is, has added the compound system solution (concentration is 10%) of the Polyethylene Octylphenol Ether of 8.3g and the DBSA triethanolamine of 4.5g in polyurethane stock solution.
Embodiment 7:
Prepare polyurethane elastomeric fiber according to the same method described in embodiment 1, difference is, has added the compound system solution (concentration is 10%) of the Polyethylene Octylphenol Ether of 83.2g and the DBSA triethanolamine of 44.9g in polyurethane stock solution.
Embodiment 8:
Prepare polyurethane elastomeric fiber according to the same method described in embodiment 1, difference is, has added the compound system solution (concentration is 10%) of the Polyethylene Octylphenol Ether of 128.3g and the DBSA triethanolamine of 64.1g in polyurethane stock solution.
Embodiment 9:
Prepare polyurethane elastomeric fiber according to the same method described in embodiment 1, difference is, has added the compound system solution (concentration is 10%) of the Nino that of 25.7g and the neopelex of 12.8g in polyurethane stock solution.
Comparative example 1:
Prepare polyurethane elastomeric fiber according to the same method described in embodiment 1, difference is, in pre-collecting process, no longer add non-ionic surface active agent, in polyurethane stock solution, also no longer add the compound system solution of non-ionic surface active agent and anion surfactant simultaneously.
Comparative example 2:
Prepare polyurethane elastomeric fiber according to the same method described in embodiment 1, difference is, only in pre-collecting process, no longer adds non-ionic surface active agent.
Comparative example 3:
Prepare polyurethane elastomeric fiber according to the same method described in embodiment 1, difference is, only in polyurethane stock solution, no longer adds the compound system solution of non-ionic surface active agent and anion surfactant.
The mechanical property of the above-mentioned polyurethane elastomeric fiber making the results are shown in following table
The result of table 1 embodiment of the present invention and comparative example.
As can be seen from Table 1, under the identical condition of other techniques, compared with the existing polyurethane elastomeric fiber that does not add surfactant, product prepared by the present invention has higher fracture strength and elongation at break.In experimentation, find simultaneously, in the time that the addition of surfactant is less, still can improve the elastic performance of product, but very few surfactant can make the system viscosity of spinning solution reduce; In the time of relatively large interpolation surfactant, the fracture strength of product and elongation at break increase rate are not obvious, and to increase substantially appear in system viscosity, and the spinning property of stoste declines.Can find with comparative example 1 by embodiment 2, in the time that spinning speed has improved 30%, the fracture strength of fiber and elongation at break still can reach target.Therefore based on above-mentioned phenomenon, the present invention chooses preferably technical recipe, can significantly improve fracture strength and the elongation at break of polyurethane elastomeric fiber, and meets the requirement of high-speed spinning process.
The present invention has described by detailed technical scheme and concrete case study on implementation describes.For those skilled in the art, the change in various forms or the details of making on the basis of technical solution of the present invention, all should fall in the definite protection domain of the claims in the present invention book.
Claims (8)
1. there is a preparation method for the polyurethane elastomeric fiber of high efficiency, it is characterized in that the method comprises the following steps:
1) component a is joined in oligomer polyol, fully mix by powerful mechanical agitation, form stable mixture system;
2) in above-mentioned system, add vulcabond, under the condition of 25～55 DEG C, react 60～120min, obtain having the pre-polymer solution of isocyano end-blocking;
3) pre-polymer solution obtaining is cooled to after 3～25 DEG C, adds mixed amine solution to carry out chain extending reaction, generate polyurethane stock solution;
4) be fully uniformly mixed to adding components b, antioxidant, ultra-violet absorber, anti-yellow agent, lubricant, dyeing assistant in above-mentioned polyurethane stock solution, after slaking, obtain spinning solution;
5) above-mentioned spinning solution is carried out to dry spinning, obtain polyurethane elastomeric fiber;
Wherein: component a is made up of non-ionic surface active agent and the organic solvent with general formula I structure, and R in formula
1, R
2, R
3for carbon number be 1～16 straight chain, side chain or cyclic alkyl;
Components b by thering is the non-ionic surface active agent of general formula II～V structure, anion surfactant and the organic solvent with general formula VI～IX structure forms; R in general formula II～IX
4for carbon number be 8～18 straight chain, side chain or cyclic alkyl, R
5for straight chain, side chain or cyclic alkyl that carbon number is 2～20, M is alkali metal, alkaline-earth metal, ammonium or organic amine, x, y, z=1～30, n=1～10;
2. the preparation method of the polyurethane elastomeric fiber with high efficiency according to claim 1, is characterized in that in described component a, the mass percent of non-ionic surface active agent in polyurethane elastomeric fiber is 0.005%～0.02%; In components b, the mass ratio of non-ionic surface active agent and anion surfactant is 1: 1～4: 1, and the mass percent of the two total amount in polyurethane elastomeric fiber is 0.03%～1.5%.
3. the preparation method of the polyurethane elastomeric fiber with high efficiency according to claim 1, it is characterized in that: described oligomer polyol is that molecular weight is 1000～3000 polytetramethylene ether diol or polypropylene glycol, also or both mixtures.
4. the preparation method of the polyurethane elastomeric fiber with high efficiency according to claim 1, it is characterized in that: described vulcabond is 4,4 '-methyl diphenylene diisocyanate or 2,4 '-methyl diphenylene diisocyanate, also or both mixtures, and the mol ratio of vulcabond and oligomer polyol is 1: 1.6～1: 2.2.
5. the preparation method of the polyurethane elastomeric fiber with high efficiency according to claim 1, it is characterized in that: described mixed amine solution is made up of chain extender, chain terminating agent and organic solvent, wherein the mol ratio of chain extender and chain terminating agent is 2: 1～25: 1, chain extender is unbranched chain extender ethylenediamine, 1,3-propane diamine or 1, one or more in 4-butanediamine, chain terminating agent is one or more that are selected from diethylamine, monoethanolamine or diisopropylamine or dibutyl amine.
6. the preparation method of the polyurethane elastomeric fiber with high efficiency according to claim 1, it is characterized in that: described chain extender is unbranched chain extender and the mixture with side chain chain extender, wherein unbranched chain extender accounts for 80%～99% of chain extender integral molar quantity, account for 1%～20% of chain extender integral molar quantity with side chain chain extender, band side chain chain extender is one or more in 1,2-propane diamine or 2 methyl pentamethylenediamine or NEED.
7. the preparation method of the polyurethane elastomeric fiber with high efficiency according to claim 1, is characterized in that: the solid content of the spinning solution of described polyurethane elastomeric fiber is 30wt%～45wt%.
8. the preparation method of the polyurethane elastomeric fiber with high efficiency according to claim 1, is characterized in that: described organic solvent is DMF or DMA.
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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. |
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