CN103993379B - The preparation method with the polyurethane elastomeric fiber of high efficiency - Google Patents
The preparation method with the polyurethane elastomeric fiber of high efficiency Download PDFInfo
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Abstract
The preparation method that the present invention relates to a kind of polyurethane elastomeric fiber with high efficiency.1) component a is mixed with oligomeric polyols, stir, form stable mixture；Described component a is made up of nonionic surfactant and organic solvent；2) in said mixture, add diisocyanate, fully react, obtain the pre-polymer solution of isocyano end-blocking；3) adopt mixed amine solution that prepolymer carries out chain extending reaction, generate polyurethane stock solution；4) to addO-on therapy b in polyurethane stock solution, after stirring ripening, spinning solution is obtained；Described component b is made up of nonionic surfactant, anion surfactant and organic solvent；5) spinning solution is carried out dry spinning and prepares described polyurethane elastomeric fiber.Polyurethane elastomeric fiber prepared by the present invention has high fracture strength and elongation at break, and therefore the method for the present invention can meet the requirement of spinning technique at high speed, and can significantly improve production efficiency.
Description
Technical field
The present invention relates to the technology of preparing of a kind of polyurethane elastomeric fiber with high efficiency, further relate to a kind of method improving polyurethane elastomeric fiber elastic performance, belong to polyurethane elastomeric fiber technical field.More particularly it relates to prepare the polyurethane elastomeric fiber with excellent resilience performance by adding surfactant, the requirement of spinning technique at high speed can be met.
Background technology
What polyurethane elastomeric fiber had an excellence draws high intensity, high extension at break and elastic recovery rate, is widely used in the elastic fabric such as knitting and woven.Along with the aggravation of social development and the market competition, people are also pursuing higher production efficiency and production capacity, and can reduce cost.In order to meet above-mentioned requirements, can suitably shorten polymerization time on the one hand；Spinning speed can be improved on the other hand, and the raising of spinning speed certainly will cause the decline of polyurethane elastomeric fiber elastic performance.High speed spinning is just seemed particularly necessary by the technology being therefore developed to improve polyurethane elastomeric fiber fracture strength and extension at break.
Segmented polyurethane phenyl ring, urea groups and carbamate polarity is strong, cohesive energy is high, be easily formed intermolecular or intramolecular physical crosslinking, make the viscosity of polyurethane stock solution system raise, and can generating section gel, be unfavorable for the processing and forming in later stage.High production efficiency is it is generally required to high concentration, therefore it is higher to the requirement of production technology, in higher concentrations, the stability of stock solution also can be deteriorated, and cohesive energy has exceeded ultimate value, when improve spinning speed, stock solution shortened again through the time of spinneret, and the cohesive energy of stock solution system has little time effective release, thus making strand generation cohesiveness cut off at die orifice exit, form fracture of wire, reduce spinnability.Meanwhile, the raising of spinning speed can make the crystallinity of polyurethane strand, the degree of orientation increase, and causes that the spring function of fiber is impaired, affects product quality.
Surfactant is the material that a class has amphiphile, amphiphilic molecule structure, interface state and the physicochemical property of solution system can be improved, due to homogenizing and the hydrotropy effect of surfactant, make the uniformity of polyurethane stock solution microstructure improve, eliminate the unstability of stock solution, suitably reduce cohesive energy.Meanwhile, surfactant use in polyurethane stock solution can make stock solution in the adhesion cross flow of spray webbing wooden partition, and all makes moderate progress in the extrusion swelling phenomenon of die orifice exit, improves the spinning property of stock solution.But, when single use certain or certain class surfactant, its large usage quantity, surfactant and stock solution compatibility poor, infringement spinnability and fibrous mechanical property can be caused.Even consumption is less, under general process conditions, using to the improvement effect of fibrous elasticity performance also and inconspicuous of single surfactant.
Summary of the invention
Technical problem: in order to solve Problems existing in background technology, the preparation method that it is an object of the invention to provide a kind of polyurethane elastomeric fiber with high efficiency, first pass through original position and add surfactant, in stock solution, then add the compound system of the surfactant preparation method to provide a kind of polyurethane elastomeric fiber with high efficiency again.The polyurethane elastomeric fiber that process according to the invention method prepares has high fracture strength and elongation at break, is suitable for the requirement of spinning technique at high speed, and can shorten the time of polyreaction, hence it is evident that improve production efficiency.
Technical scheme: the preparation method that the invention provides a kind of polyurethane elastomeric fiber with high efficiency, it comprises the following steps:
1) component a is joined in oligomer polyol, be sufficiently mixed by powerful mechanical agitation, form stable mixture system；
2) in above-mentioned system, add diisocyanate, react 60～120min when 25～55 DEG C, obtain the pre-polymer solution with isocyano end-blocking；
3), after the pre-polymer solution obtained being cooled to 3～25 DEG C, add mixed amine solution and carry out chain extending reaction, generate polyurethane stock solution；
4) it is sufficiently stirred for mixing to addO-on therapy b, antioxidant, UV absorbent, anti-yellow agent, lubricant, dyeing assistant in above-mentioned polyurethane stock solution, after ripening, obtains spinning solution；
5) above-mentioned spinning solution is carried out dry spinning, namely obtain polyurethane elastomeric fiber；
Wherein: component a is made up of the nonionic surfactant and organic solvent with formula I structure, and R in formula1、R2、R3For straight chain, side chain or cyclic alkyl that carbon number is 1～16；
Component b is formed by having the nonionic surfactant of formula II～V structure, the anion surfactant with formula VI～Ⅸ structure and organic solvent；R in formula II～Ⅸ4For straight chain, side chain or cyclic alkyl, R that carbon number is 8～185For 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, nonionic surfactant mass percent in polyurethane elastomeric fiber is 0.005%～0.02%；In component b, nonionic surfactant is 1: 1～4: 1 with the mass ratio of anion surfactant, and the two total amount mass percent in polyurethane elastomeric fiber is 0.03%～1.5%.
Described oligomer polyol is molecular weight be 1000～3000 polytetramethylene ether diol or polypropylene glycol, also or both mixture.
Described diisocyanate is 4,4 '-methyl diphenylene diisocyanate or 2,4 '-methyl diphenylene diisocyanate, and also or both mixture, and the mol ratio of diisocyanate 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 chain extender is 2: 1～25: 1 with the mol ratio of chain terminating agent, chain extender be unbranched chain extender ethylenediamine, 1,3-propane diamine or 1, one or more in 4-butanediamine, chain terminating agent is one or more in diethylamine, ethanolamine 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 the 80%～99% of chain extender integral molar quantity, the 1%～20% of chain extender integral molar quantity is accounted for 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 N,N-dimethylformamide or DMAC N,N' dimethyl acetamide.
Beneficial effect: the present invention is under specific process conditions, the method that two steps add surfactant is adopted to prepare polyurethane elastomeric fiber, first in pre-polymerization process, add nonionic surfactant, utilize the infiltration of nonionic surfactant and emulsification make mixed system more uniformly, polymerization process more stable, can effectively shorten polymerization time simultaneously；Then in the maturing process of polyurethane stock solution, add the compound system of nonionic surfactant and anion surfactant, by both cooperative effects, that can effectively reduce surfactant makes consumption, simultaneously between polyurethane stock solution system Middle molecule or the hydrogen bond of intramolecular unordered instability be adjusted, to obtain uniform and stable hard section region, and promotion microphase-separated, thus improve the spinnability of stock solution and the elastic performance of fiber, the requirement of high-speed spinning process can be met, reach the purpose of efficiently 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, be sufficiently mixed by powerful mechanical agitation, form stable mixture system；
2) in above-mentioned system, add diisocyanate, react 60～120min when 25～55 DEG C, obtain the pre-polymer solution with isocyano end-blocking；
3), after the pre-polymer solution obtained being cooled to 3～25 DEG C, add mixed amine solution and carry out chain extending reaction, generate polyurethane stock solution；
4) it is sufficiently stirred for mixing to addO-on therapy b, antioxidant, UV absorbent, anti-yellow agent, lubricant, dyeing assistant in above-mentioned polyurethane stock solution, after ripening, obtains spinning solution；
5) above-mentioned spinning solution is carried out dry spinning, namely 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 the nonionic surfactant and organic solvent with formula I structure, and R in formula1、R2、R3For straight chain, side chain or cyclic alkyl that carbon number is 1～16.
In described component a, nonionic surfactant mass percent in polyurethane elastomeric fiber is 0.005%～0.02%.
Described component b is formed by having the nonionic surfactant of formula II～V structure, the anion surfactant with formula VI～Ⅸ structure and organic solvent；R in formula II～Ⅸ4For straight chain, side chain or cyclic alkyl, R that carbon number is 8～185For 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 b, nonionic surfactant is 1: 1～4: 1 with the mass ratio of anion surfactant, and the two total amount mass percent 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 to be molecular weight be 1000～3000 polytetramethylene ether diol or polypropylene glycol, also or both mixture.
A kind of preparation method of the polyurethane elastomeric fiber with high efficiency of the present invention, wherein said step 2) in diisocyanate be 4,4 '-methyl diphenylene diisocyanate or 2,4 '-methyl diphenylene diisocyanate, also or both mixture, and the mol ratio of diisocyanate and oligomer polyol be 1: 1.6～1: 2.2.
A kind of preparation method of the polyurethane elastomeric fiber with high efficiency of the present invention, wherein said step 3) in mixed amine solution be made up of chain extender, chain terminating agent and organic solvent, wherein chain extender is 2: 1～25: 1 with the mol ratio of chain terminating agent, chain extender be unbranched chain extender ethylenediamine, 1,3-propane diamine or 1, one or more in 4-butanediamine, chain terminating agent is one or more in diethylamine, ethanolamine or diisopropylamine or dibutyl amine.
A kind of preparation method of the 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 the 80%～99% of chain extender integral molar quantity, the 1%～20% of chain extender integral molar quantity is accounted for 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, UV absorbent can be UV-320, anti-yellow agent can be UDT, lubricant can be magnesium stearate, 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 N,N-dimethylacetamide.
A kind of preparation method of the polyurethane elastomeric fiber with high efficiency of the present invention, wherein said step 5) in dry spinning be namely that spinning solution is extruded by spinneret after filtering, by high temperature path, through false twisting, oil and wind and make polyurethane elastomeric fiber.
For further illustrating the present invention, the specific operation process of the present invention it is described in detail below by specific embodiment, but these embodiments must not be interpreted as the limitation of the present invention that goes up in all senses.In addition, it is to be understood that after reading present disclosure, the various changes that the present invention can be made by those skilled in the art, these equivalent form of values also belong to the application claims limited range.
Embodiment 1:
The N,N-dimethylacetamide solution (concentration is 1%) of the surfactant of 250g is joined in N,N-dimethylacetamide and the 10.0kg polytetramethylene ether diol solution of 5.0kg, stir.It is subsequently adding the 4 of 2.5kg, 4 '-methyl diphenylene diisocyanate, under 40 DEG C of conditions, react 80min, the N,N-dimethylacetamide adding 11.38kg stirs, and namely obtains the pre-polymer solution of isocyano end-blocking.
After pre-polymer solution is cooled to 5 DEG C, be gradually added in 80min ethylenediamine that 6.35kg contains 223.9g, 30.7g 1,2-propane diamine, 45.1g the N of diethylamine, N-dimethylacetamide solution carries out chain extending reaction and generates polyurethane stock solution, it is subsequently adding the compound system solution (concentration is 10%) of the Polyethylene Octylphenol Ether of 25.7g and the DBSA triethanolamine of 12.8g, is eventually adding antioxidant, UV absorbent, anti-yellow agent, lubricant, dyeing assistant obtain spinning solution.
By above-mentioned spinning solution after ripening, filtration, deaeration, carry out dry spinning with the speed of 900m/min, produce the polyurethane elastomeric fiber of 22dtex/2f.
Embodiment 2:
Same method according to embodiment 1 prepares polyurethane elastomeric fiber, is different in that, spinning speed is 1200m/min.
Embodiment 3:
Same method according to embodiment 1 prepares polyurethane elastomeric fiber, it is different in that, polyurethane stock solution with the addition of the compound system solution of the DBSA triethanolamine of the Polyethylene Octylphenol Ether of 12.8g and 25.7g (concentration is 10%).
Embodiment 4:
Same method according to embodiment 1 prepares polyurethane elastomeric fiber, it is different in that, polyurethane stock solution with the addition of the compound system solution of the DBSA triethanolamine of the Polyethylene Octylphenol Ether of 25.7g and 25.7g (concentration is 10%).
Embodiment 5:
Same method according to embodiment 1 prepares polyurethane elastomeric fiber, it is different in that, polyurethane stock solution with the addition of the compound system solution of the DBSA triethanolamine of the Polyethylene Octylphenol Ether of 2.6g and 1.3g (concentration is 10%).
Embodiment 6:
Same method according to embodiment 1 prepares polyurethane elastomeric fiber, it is different in that, polyurethane stock solution with the addition of the compound system solution of the DBSA triethanolamine of the Polyethylene Octylphenol Ether of 8.3g and 4.5g (concentration is 10%).
Embodiment 7:
Same method according to embodiment 1 prepares polyurethane elastomeric fiber, it is different in that, polyurethane stock solution with the addition of the compound system solution of the DBSA triethanolamine of the Polyethylene Octylphenol Ether of 83.2g and 44.9g (concentration is 10%).
Embodiment 8:
Same method according to embodiment 1 prepares polyurethane elastomeric fiber, it is different in that, polyurethane stock solution with the addition of the compound system solution of the DBSA triethanolamine of the Polyethylene Octylphenol Ether of 128.3g and 64.1g (concentration is 10%).
Embodiment 9:
Same method according to embodiment 1 prepares polyurethane elastomeric fiber, is different in that, with the addition of the compound system solution (concentration is 10%) of the dodecylbenzene sodium sulfonate of the Nino of 25.7g that and 12.8g in polyurethane stock solution.
Comparative example 1:
Same method according to embodiment 1 prepares polyurethane elastomeric fiber, it is different in that, pre-collecting process does not add nonionic surfactant, in polyurethane stock solution, does not add the compound system solution of nonionic surfactant and anion surfactant simultaneously yet.
Comparative example 2:
Same method according to embodiment 1 prepares polyurethane elastomeric fiber, is different in that, does not only add nonionic surfactant in pre-collecting process.
Comparative example 3:
Same method according to embodiment 1 prepares polyurethane elastomeric fiber, is different in that, does not only add the compound system solution of nonionic surfactant and anion surfactant in polyurethane stock solution.
The mechanical property result of above-mentioned prepared polyurethane elastomeric fiber is shown in following table
The result of table 1 embodiment of the present invention and comparative example.
As can be seen from Table 1, when other techniques are identical, compared with the existing polyurethane elastomeric fiber not adding surfactant, product prepared by the present invention has higher fracture strength and elongation at break.Experimentation finds simultaneously, when the addition of surfactant is less, still can improve the elastic performance of product, but the system viscosity that very few surfactant can make spinning solution reduces；When larger amount of interpolation surfactant, fracture strength and the elongation at break increase rate of product are inconspicuous, and increasing substantially occurs in system viscosity, and the spinning property of stock solution declines.By embodiment 2 with comparative example 1 it is found that when spinning speed improves 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, fracture strength and the elongation at break of polyurethane elastomeric fiber can be greatly improved, and meet the requirement of high-speed spinning process.
The present invention describes already by detailed technical scheme and concrete case study on implementation illustrates.For those skilled in the art, the change on the various forms made on the basis of technical solution of the present invention or details, all should fall in the protection domain that claims of the present invention is determined.
Claims (8)
1. the preparation method of a polyurethane elastomeric fiber with high efficiency, it is characterised in that the method comprises the following steps:
1) component a is joined in oligomer polyol, be sufficiently mixed by powerful mechanical agitation, form stable mixture system；
2) in above-mentioned system, add diisocyanate, react 60～120min when 25～55 DEG C, obtain the pre-polymer solution with isocyano end-blocking；
3), after the pre-polymer solution obtained being cooled to 3～25 DEG C, add mixed amine solution and carry out chain extending reaction, generate polyurethane stock solution；
4) it is sufficiently stirred for mixing to addO-on therapy b, antioxidant, UV absorbent, anti-yellow agent, lubricant, dyeing assistant in above-mentioned polyurethane stock solution, after ripening, obtains spinning solution；
5) above-mentioned spinning solution is carried out dry spinning, namely obtain polyurethane elastomeric fiber；
Wherein: component a is made up of the nonionic surfactant and organic solvent with formula I structure, and R in formula1、R2、R3For straight chain, side chain or cyclic alkyl that carbon number is 1～16；
Component b is formed by having the nonionic surfactant of formula II～V structure, the anion surfactant with formula VI～Ⅸ structure and organic solvent；R in formula II～Ⅸ4For straight chain, side chain or cyclic alkyl, R that carbon number is 8～185For 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, it is characterised in that in described component a, nonionic surfactant mass percent in polyurethane elastomeric fiber is 0.005%～0.02%；In component b, nonionic surfactant is 1: 1～4: 1 with the mass ratio of anion surfactant, and the two total amount mass percent 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 characterised in that: described oligomer polyol is molecular weight be 1000～3000 polytetramethylene ether diol or polypropylene glycol, also or both mixture.
4. the preparation method of the polyurethane elastomeric fiber with high efficiency according to claim 1, it is characterized in that: described diisocyanate is 4,4 '-methyl diphenylene diisocyanate or 2,4 '-methyl diphenylene diisocyanate, also or both mixture, and the mol ratio of diisocyanate and oligomer polyol be 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 chain extender is 2: 1～25: 1 with the mol ratio of chain terminating agent, chain extender be unbranched chain extender ethylenediamine, 1,3-propane diamine or 1, one or more in 4-butanediamine, chain terminating agent is one or more in diethylamine, ethanolamine 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: in described chain extending reaction, chain extender is unbranched chain extender and the mixture with side chain chain extender, wherein unbranched chain extender accounts for the 80%～99% of chain extender integral molar quantity, the 1%～20% of chain extender integral molar quantity is accounted for 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, it is characterised 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, it is characterised in that: described organic solvent is DMF or N,N-dimethylacetamide.
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