CN101096782B - Method for preparing polyurethane snapback fibre with solution polymerization - Google Patents
Method for preparing polyurethane snapback fibre with solution polymerization Download PDFInfo
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Abstract
The invention discloses preparing method of polyurethane elastic fiber with solution polymerization in polyurethane elastic fiber preparing method technique domain, which is characterized by the following: comprising polyether diatomic alcohol, diisocyanate, regular butanol, mixed amine, additive and solvent dimethyl acetamine; proceeding pre-polyreaction in solvent dimethyl acetamine; getting monomolecular prepolymer solution; proceeding continuous enlargered reaction; getting high molecular polymer; adding into various aids; getting spin dope; proceeding dry spin through round passage; coiling; getting urethane elastic fiber silk tubular. This invention can improve regularity of pre-poly intermediate and raw liquid, which can simplify production control.
Description
One, technical field
The present invention relates to a kind of chemical fibre, particularly relate to a kind of method of preparing polyurethane snapback fibre with solution polymerization, belong to preparation method's technical field of polyurethane elastomeric fiber.
Two, background technology
Nineteen thirty-seven, Bayer A.G developed polyurethane resin and polyurethane (spandex) elastomer the earliest, nineteen fifty-nine, du pont company took the lead in realizing the suitability for industrialized production of polyurethane (spandex) elastomer, and name into Lycra (Lycra), some countries of Europe and Japan begin to produce spandex in succession subsequently.To nineteen nineties, along with the development and application of the various new technologies of downstream industry, new material, the Application Areas of spandex is expanded rapidly, and demand significantly increases, and has driven the development of whole spandex industry.
China's spandex industry is started late, but the industry size rate of expansion is very fast, Yantai Polyurethane Fibre Co., Ltd introduces first that the dry method spinning technique spins in Japanese Japan and equipment begins from later 1980s, so far size twenties tame spandex manufacturing enterprises have been developed in the whole nation, process route has contained that dry method is spun, wet method is spun, several main spinning techniques are spun in molten spinning and reaction, surplus a year total production scale reaches 20 ten thousand tons.But because the development of technical research lags behind the rate of expansion of market and production capacity relatively, therefore there is the limitation that repeats to wear out in the production technology of numerous domestic spandex enterprise at present, and product variety is single, and quality can't satisfy the needs of high-end market and novel fabric.
In the existing spandex fibre production technology, because polymerization technique adopts the bulk polymerization mode mostly, add solvent again behind the generation prepolymer and dissolve, its prepolymerization reaction temperature drift, side reaction is many, cause in the prepolymer gel particles many, polymerization gained stoste the uniformity and stable aspect exist not enoughly, the filter life cycle is short, has restricted the raising of spinning speed simultaneously, production efficiency is low, and final gained spandex fibre is having certain defective aspect bar evenness and the physicochemical property.
Three, summary of the invention
The objective of the invention is to overcome above-mentioned weak point, a kind of polymerisation in solution of carrying out in low-temperature solvent is provided, make homogeneous, pure prepolymer, thus again through chain extending reaction continuously, add the method that auxiliary agent, spinning moulding are produced the high-quality polyurethane elastomer.
Purpose of the present invention realizes by the following technical solutions:
A kind of method of preparing polyurethane snapback fibre with solution polymerization, be to obtain the pre-polymerization midbody solution by in solvent dimethylacetylamide (DMAC), carrying out the prepolymerization reaction, obtain high molecular polymer through continuous chain extending reaction again, add various auxiliary agents then and become spinning solution, after round path with dry spinning and reel and make polyurethane elastomeric fiber silk tube, comprises polymerization, two operations of spinning.
The raw material of polyurethane elastomeric fiber comprises polyether Glycols, vulcabond, n-butanol, mixed amine, additive and solvent dimethylacetylamide;
Additive be antioxidant, lubricated separate in easypro agent, ultra-violet absorber, the anti-yellowing agent any one and several;
Wherein the mol ratio of polyether Glycols and vulcabond is 1: (1.55-1.9), the weight ratio of polyether Glycols and n-butanol is 100: (0.05-0.15), above component is formed the pre-polymerization intermediate, and pre-polymerization intermediate and solvent dimethylacetylamide (DMAC) are formed the pre-polymerization midbody solution that concentration is 50-70% jointly; The weight ratio of pre-polymerization intermediate and mixed amine is 100: (1.5-2.0), the two and solvent dimethylacetylamide (DMAC) are formed macromolecule polymer solution; Macromolecule polymer solution is separated the ultra-violet absorber of easypro agent, 0.2-1.0% with antioxidant, 0.02-0.1% lubricated that with respect to pre-polymerization intermediate weight ratio is 0.5-1.5%, anti-yellowing agent and the dimethylacetylamide (DMAC) of 0.5-2.0% formed spinning solution.
Wherein polymerization process is:
(1) in first reactor, adds dimethylacetylamide (DMAC), cooling; Add polyether Glycols, n-butanol, cooling; Add vulcabond, obtaining concentration is the pre-polymerization midbody solution of 50-70%, delivers to second reactor;
(2) the pre-polymerization midbody solution cools in second reactor, stirs, and is transferred in the chain extension storage tank;
(3) the pre-polymerization midbody solution feed in high-speed stirring mixer in the chain extension storage tank, simultaneously, mixed amine solution is to the high-speed stirring mixer feed, the begin chain reaction of propagation, obtain high molecular polymer, be transferred in the viscosity adjustment groove, chain propagation reaction is proceeded, obtain the polymerizate of target molecular weight, transfer to hold-up vessel then;
Mixed amine is to be 1 in molar ratio: ratio (0.1-0.3) is mixed the chain extender diamines with terminal terminator monoamine, and adds that the deployed concentration of solvent dimethylacetylamide is the mixed amine solution of 1-3%.
Chain extender comprises ethylenediamine, 2 methyl pentamethylenediamine, propane diamine, hexamethylene diamine, 1, and 3-cyclohexanediamine or its mixture, terminal terminator are dimethylamine, or diethylamine, or two-n-butylamine, or n-butylamine, or n-hexylamine, or cyclohexylamine, or monoethanolamine, or their mixture.
(4) additive and solvent dimethylacetylamide are added in the emulsification dispersion slot in advance, get emulsion, add the DMAC solution of high molecular polymer then, obtain the additive seasoning liquid of stable in properties;
(5) feed in dynamic mixer of the macromolecule polymer solution in the hold-up vessel, while additive seasoning liquid feed in dynamic mixer, after mixing, dynamic mixer obtains the fire-resistant high-resiliency spandex fabric spinning solution, spinning solution filters in the back immigration stoste storage tank and carries out maturation process, and the spinning solution after slaking is finished promptly can be used for spinning production:
Spinning process is:
(1) spinning solution after the slaking carries out deaeration in the stoste storage tank, transfers to each spinning station, after filtering, is assigned in every block of spinnerets;
(2) spinning solution is extruded through spinneret hole and is promptly entered in the spinning shaft, and solvent dimethylacetylamide wherein volatilizees rapidly, forms spandex fibre; The spandex fibre that comes out from spinning shaft carries out becoming one filament after the boundling obvolvent, becomes fire-resistant high-resiliency spandex silk tube volume on the bobbin through being wound up into after oiling, and the spandex silk tube volume after finishing of reeling is delivered to the hierarchical verification operation and tested and pack.
The method of a kind of preparing polyurethane snapback fibre with solution polymerization of the present invention, changed the mode of polymerization technique employing bulk polymerization in the existing polyurethane elastomeric fiber production process, in low-temperature solvent, carry out polymerisation in solution, improved the uniformity of pre-polymerization intermediate and polymerization stoste, make homogeneous, pure prepolymer, again through continuous chain extending reaction, interpolation auxiliary agent, spinning moulding, produce the high-quality polyurethane elastomer, have advantages such as shaping is good, bar evenness excellence, and simplified in the production process and controlled.
Four, the specific embodiment
Describe the present invention in detail with embodiment below, but these embodiment must not be interpreted as the limitation of the present invention that goes up in all senses.
A kind of method of preparing polyurethane snapback fibre with solution polymerization comprises polymerization, two operations of spinning, and wherein polymerization process is:
(1) in first reactor, adds dimethylacetylamide (DMAC), first reactor temperature is reduced to below 20 ℃ by chuck recirculated water; Under the well-beaten condition of mixer, at the uniform velocity to add with respect to dimethylacetylamide (DMAC) weight in first reactor is the polyether Glycols of 80-180%, add n-butanol simultaneously, first reactor temperature is reduced to below 15 ℃ by chuck recirculated water with respect to polyether Glycols weight 0.05-0.15%; Under the well-beaten condition of mixer, at the uniform velocity to add with respect to the polyether Glycols mol ratio in first reactor is 1: vulcabond (1.55-1.9), by chuck recirculated water control reaction temperature is below 60 ℃, and process obtains single polymer molecule after about 90-180 minute concentration is the pre-polymerization midbody solution of 50-70%; After the reaction time arrived, the prepolymerization reaction was finished, and utilizes nitrogen that first reactor is pressurizeed, and wherein pre-polymerization midbody solution all is transferred to second reactor;
(2) the pre-polymerization midbody solution cools by warm chuck recirculated water in second reactor, use the mixer continuous stirring simultaneously, when second reactor temperature is reduced to below 15 ℃, again by nitrogen pressure or utilize shifting pump that the pre-polymerization midbody solution of low temperature is transferred in the chain extension storage tank;
(3) in the chain extension storage tank pre-polymerization midbody solution after the cooling after filtering by the feed measuring pump with certain flow feed in high-speed stirring mixer continuously, meanwhile, be 1 in advance in molar ratio: ratio (0.1-0.3) the chain extender diamines is mixed with terminal terminator monoamine and add the deployed concentration of solvent dimethylacetylamide be 1-3% mixed amine solution simultaneously by the feed measuring pump to the high-speed stirring mixer feed, the feed amount is 1.5-2.0% with respect to pre-polymerization intermediate weight ratio, super mixer is with the operation of the rotating speed of 1600-2400rpm, make by wherein the pre-polymerization intermediate with mixes the even also begin chain reaction of propagation of amine rapid mixing; High-speed stirring mixer utilizes 5 ℃ in the external jacket--and 20 ℃ of circulating water coolings remain on below 80 ℃ the temperature at mixer outlet place; Outlet at high-speed stirring mixer obtains fully mixing being incorporated in the high molecular polymer that carries out chain propagation reaction, its concentration is 30-34%, viscosity is about 300-500Pa.S, uses shifting pump that high molecular polymer is transferred to the viscosity adjustment groove then through one or more snippets static mixer; The viscosity adjustment groove utilizes 60 ℃ in external jacket--90 ℃ recirculated water insulation, make its internal temperature remain on 60 ℃--between 90 ℃, high molecular polymer chain propagation reaction in the viscosity adjustment groove is proceeded, about 4-20 of the time of staying hour, this moment, reaction was finished, obtain the polymerizate of target molecular weight, utilize nitrogen pressure to transfer then to hold-up vessel; Hold-up vessel utilizes 30 ℃ in the external jacket--and 50 ℃ of recirculated water insulations are reduced to below 60 ℃ the high molecular polymer temperature of immigration;
(4) will be that antioxidant, 0.02-0.1% lubricated of 0.5-1.5% separated the ultra-violet absorber of easypro agent, 0.2-1.0%, anti-yellowing agent and the solvent dimethylacetylamide of 0.5-2.0% is added in the emulsification dispersion slot in advance with respect to pre-polymerization intermediate weight ratio, obtaining concentration after Over emulsfication disperses is that 30-34%, particle diameter are less than 2 μ, the uniform emulsion of component, add high molecular polymer doubly then, obtain the additive seasoning liquid of stable in properties with respect to additive solids content 2-4;
(5) high molecular polymer after the cooling uses measuring pump with stable flow rate feed in dynamic mixer continuously in the hold-up vessel, and the additive seasoning liquid uses measuring pump with respect to the flow of the 4-8% of high molecular polymer weight feed in dynamic mixer continuously simultaneously; After mixing, dynamic mixer obtains the spandex fibre spinning solution in the exit; Prepared spinning solution filters in the back use gear shifting pump immigration stoste storage tank through former liquid filter and carries out maturation process, utilize 30 ℃ in the storage tank external jacket--60 ℃ recirculated water insulation, curing time is about 16-50 hour, and the spinning solution after slaking is finished promptly can be used for spinning production;
Spinning process is:
(1) carries out deaeration in the immigration of the spinning solution after the slaking deaerator in the stoste storage tank; Stoste after the deaeration uses the gear metering conveying pump to transfer to each spinning station with pressure stable, stoste the pipeline of process jacket pipe all is set, with 30 ℃--50 ℃ of recirculated waters insulations; The spinning solution that is transplanted on each spinning station is through 10 μ--and after the spinning filter filtration of 40 μ, rationed in every block of spinnerets through spinning pump again;
(2) spinning solution is extruded through spinneret hole and is promptly entered in the spinning shaft; Spinning shaft is round, and the nitrogen that is heated to 300--350 ℃ is blown into by top, path, vertically evenly flows downward; Enter in the path the stoste thread at high temperature wherein solvent dimethylacetylamide volatilize rapidly, form spandex fibre; The spandex fibre that comes out from spinning shaft carries out becoming one filament after the boundling obvolvent through twister according to kind is different, becomes fire-resistant high-resiliency spandex silk tube volume through the back that oils on the bobbin being wound up on the up-coiler; Spandex silk tube after coiling is finished volume is delivered to the hierarchical verification operation and is tested and pack.
The method of a kind of preparing polyurethane snapback fibre with solution polymerization of present embodiment, owing to changed the mode of polymerization technique employing bulk polymerization in the existing polyurethane elastomeric fiber production process, changed the proportioning of polymer raw, the order that raw material adds, the type of chain extender and terminator and composition, the chain extending reaction form, the type of additive and proportioning and dispensing mode, polymerization technique and path forms such as the form of blender, spinning techniques such as heat medium type, reduced the prepolymerization reaction temperature, reduced side reaction odds in the prepolymerization reaction process, effectively reduce the generation of gel particles, improved the uniformity of pre-polymerization intermediate and polymerization stoste, thereby reduced waste, make production process more stable, continuously, spinning speed increases substantially, it is good that the polyurethane elastomeric fiber of being produced has shaping, characteristics such as bar evenness excellence, and simplified in the production process and controlled.This invention has promoted the quality of polyurethane elastomeric fiber, can satisfy the particularly requirement of chemical fibre class lining and tricot of various novel fabrics and high-grade fabric, for the structure of improving China's textile product, promote the textiles class, the status of further consolidating weaving power played positive and important effect.
Claims (4)
1. the method for preparing polyurethane snapback fibre with solution polymerization, it is characterized in that: be to obtain the pre-polymerization midbody solution by in the solvent dimethylacetylamide, carrying out the prepolymerization reaction, obtain high molecular polymer through continuous chain extending reaction again, add various auxiliary agents then and become spinning solution, after round path with dry spinning and reel and make polyurethane elastomeric fiber silk tube, comprises polymerization, two operations of spinning; The raw material of described polyurethane elastomeric fiber comprises polyether Glycols, vulcabond, n-butanol, mixed amine, additive and solvent dimethylacetylamide;
Described polymerization process is:
(1) in first reactor, adds dimethylacetylamide, first reactor temperature is reduced to below 20 ℃ by chuck recirculated water; Under the well-beaten condition of mixer, at the uniform velocity to add with respect to dimethylacetylamide weight in first reactor is the polyether Glycols of 80-180%, add n-butanol simultaneously, first reactor temperature is reduced to below 15 ℃ by chuck recirculated water with respect to polyether Glycols weight 0.05-0.15%; Under the well-beaten condition of mixer, with at the uniform velocity in first reactor mol ratio according to polyether Glycols and vulcabond be 1: 1.55-1.9 adds vulcabond, by chuck recirculated water control reaction temperature is below 60 ℃, and process obtains single polymer molecule after 90-180 minute concentration is the pre-polymerization midbody solution of 50-70%; After the reaction time arrived, the prepolymerization reaction was finished, and utilizes nitrogen that first reactor is pressurizeed, and wherein pre-polymerization midbody solution all is transferred to second reactor;
(2) the pre-polymerization midbody solution cools by warm chuck recirculated water in second reactor, use the mixer continuous stirring simultaneously, when second reactor temperature is reduced to below 15 ℃, again by nitrogen pressure or utilize shifting pump that the pre-polymerization midbody solution of low temperature is transferred in the chain extension storage tank;
(3) in the chain extension storage tank pre-polymerization midbody solution after the cooling after filtering by the feed measuring pump with certain flow feed in high-speed stirring mixer continuously, meanwhile, be 1 in advance in molar ratio: 0.1-1: 0.3 ratio the chain extender diamines is mixed with terminal terminator monoamine and add the deployed concentration of solvent dimethylacetylamide be 1-3% mixed amine solution simultaneously by the feed measuring pump to the high-speed stirring mixer feed, the feed amount is 1.5-2.0% with respect to pre-polymerization intermediate weight ratio, super mixer is with the operation of the rotating speed of 1600-2400rpm, make by wherein the pre-polymerization intermediate with mixes the even also begin chain reaction of propagation of amine rapid mixing; High-speed stirring mixer utilizes 5 ℃ in the external jacket--and 20 ℃ of circulating water coolings remain on below 80 ℃ the temperature at mixer outlet place; Outlet at high-speed stirring mixer obtains fully mixing being incorporated in the high molecular polymer that carries out chain propagation reaction, its concentration is 30-34%, viscosity is 300-500Pa.S, uses shifting pump that high molecular polymer is transferred to the viscosity adjustment groove then through one or more snippets static mixer; The viscosity adjustment groove utilizes 60 ℃ in external jacket--90 ℃ recirculated water insulation, make its internal temperature remain on 60 ℃--between 90 ℃, high molecular polymer chain propagation reaction in the viscosity adjustment groove is proceeded, time of staying 4-20 hour, this moment, reaction was finished, obtain the polymerizate of target molecular weight, utilize nitrogen pressure to transfer then to hold-up vessel; Hold-up vessel utilizes 30 ℃ in the external jacket--and 50 ℃ of recirculated water insulations are reduced to below 60 ℃ the high molecular polymer temperature of immigration;
(4) will be that antioxidant, 0.02-0.1% lubricated of 0.5-1.5% separated the ultra-violet absorber of easypro agent, 0.2-1.0%, anti-yellowing agent and the solvent dimethylacetylamide of 0.5-2.0% is added in the emulsification dispersion slot in advance with respect to pre-polymerization intermediate weight ratio, obtaining concentration after Over emulsfication disperses is that 30-34%, particle diameter are less than 2 μ, the uniform emulsion of component, add high molecular polymer doubly then, obtain the additive seasoning liquid of stable in properties with respect to additive solids content 2-4;
(5) high molecular polymer after the cooling uses measuring pump with stable flow rate feed in dynamic mixer continuously in the hold-up vessel, and the additive seasoning liquid uses measuring pump with respect to the flow of the 4-8% of high molecular polymer weight feed in dynamic mixer continuously simultaneously; After mixing, dynamic mixer obtains the fire-resistant high-resiliency spandex fabric spinning solution in the exit; Prepared spinning solution filters in the back use gear shifting pump immigration stoste storage tank through former liquid filter and carries out maturation process, utilize 30 ℃ in the storage tank external jacket--60 ℃ recirculated water insulation, curing time is 16-50 hour, and the spinning solution after slaking is finished is used for spinning production.
2. the method for preparing polyurethane snapback fibre with solution polymerization as claimed in claim 1, it is characterized in that: chain extender comprises ethylenediamine, 2 methyl pentamethylenediamine, propane diamine, hexamethylene diamine, 1,3-cyclohexanediamine or its mixture, terminal terminator are dimethylamine, or diethylamine, or two-n-butylamine, or n-butylamine, or n-hexylamine, or cyclohexylamine, or monoethanolamine, or their mixture.
3. the method for preparing polyurethane snapback fibre with solution polymerization as claimed in claim 1, it is characterized in that: described spinning process is:
(1) spinning solution after the slaking carries out deaeration in the stoste storage tank, transfers to each spinning station, after filtering, is assigned in every block of spinnerets;
(2) spinning solution is extruded through spinneret hole and is promptly entered in the spinning shaft, and solvent dimethylacetylamide wherein volatilizees rapidly, forms spandex fibre; The spandex fibre that comes out from spinning shaft carries out becoming one filament after the boundling obvolvent, becomes fire-resistant high-resiliency spandex silk tube volume on the bobbin through being wound up into after oiling, and the spandex silk tube volume after finishing of reeling is delivered to the hierarchical verification operation and tested and pack.
4. the method for preparing polyurethane snapback fibre with solution polymerization as claimed in claim 3, it is characterized in that: described spinning process is:
(1) carries out deaeration in the immigration of the spinning solution after the slaking deaerator in the stoste storage tank; Stoste uses the gear metering conveying pump to transfer to each spinning station with pressure stable after the deaeration, stoste the pipeline of process jacket pipe all is set, with 30 ℃--50 ℃ of recirculated waters insulations; The spinning solution that is transplanted on each spinning station is through 10 μ--and after the spinning filter filtration of 40 μ, rationed in every block of spinnerets through spinning pump again;
(2) spinning solution is extruded through spinneret hole and is promptly entered in the spinning shaft; Spinning shaft is round, and the nitrogen that is heated to 300--350 ℃ is blown into by top, path, vertically evenly flows downward; Enter in the path the stoste thread at high temperature wherein solvent dimethylacetylamide volatilize rapidly, form spandex fibre; The spandex fibre that comes out from spinning shaft carries out becoming one filament after the boundling obvolvent through twister according to kind is different, becomes fire-resistant high-resiliency spandex silk tube volume through the back that oils on the bobbin being wound up on the up-coiler; Spandex silk tube after coiling is finished volume is delivered to the hierarchical verification operation and is tested and pack.
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| CN108950776A (en) * | 2018-09-11 | 2018-12-07 | 福建省德奥针织科技有限公司 | A kind of yarn spandex blend fibre and preparation method thereof |
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| JP5704530B2 (en) * | 2009-12-16 | 2015-04-22 | 東レ・オペロンテックス株式会社 | Polyurethane elastic yarn and method for producing the same |
| CN101736432B (en) * | 2009-12-24 | 2012-09-12 | 烟台泰和新材料股份有限公司 | Production method of anti-yellowing polyurethane elastic fiber |
| CN102127826B (en) * | 2010-01-18 | 2012-10-31 | 浙江华峰氨纶股份有限公司 | Nanoparticle-containing anti-chlorine high temperature resistant polyurethane elastic fiber and preparation method thereof |
| CN102408532B (en) * | 2011-10-18 | 2012-12-05 | 江阴中绿化纤工艺技术有限公司 | Reactor for spandex continuous polymerization production |
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| CN112725929B (en) * | 2020-12-29 | 2022-05-17 | 宁夏宁东泰和新材有限公司 | Spinning control method for high-temperature-resistant polyurethane elastic fiber |
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