CN101922063B - Method for regenerating dry-spinning waste polyurethane filament into polyurethane spinning stock solution with chlorine resistance - Google Patents
Method for regenerating dry-spinning waste polyurethane filament into polyurethane spinning stock solution with chlorine resistance Download PDFInfo
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- CN101922063B CN101922063B CN2010102490115A CN201010249011A CN101922063B CN 101922063 B CN101922063 B CN 101922063B CN 2010102490115 A CN2010102490115 A CN 2010102490115A CN 201010249011 A CN201010249011 A CN 201010249011A CN 101922063 B CN101922063 B CN 101922063B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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Abstract
The invention relates to a method for regenerating dry-spinning waste polyurethane filament into polyurethane spinning stock solution with chlorine resistance, comprising the following technical process: at the temperature of 30 DEG C below zero to 40 DEG C below zero, smashing waste polyurethane filament into short fibre; washing by water and detergent and drying; adding organic solvent accounting for 50-200 wt% of waste polyurethane filament; then adding waste polyurethane filament; finally, adding organic solvent accounting for 46.4-284 wt% of waste polyurethane filament; under the protection of N2, stirring and reacting for 2-4 hours at the reaction temperature of 50-100 DEG C; spraying reaction control agent blended by organic solvent; adding reaction auxiliary agent blended by the organic solvent; stirring for 20-120 minutes; and after curing, obtaining spinning stock solution with proper viscosity. The polyurethane spinning stock solution produced by the method of the invention has good stability, evenness and spinnability and has obvious effect of good chlorine resistance of the product.
Description
(1) technical field
The present invention relates to a kind of is the method that contains the spandex fiber stoste of anti-chlorine characteristic with regenerating dry-spinning waste polyurethane filament.Belong to the spandex fiber technical field.
(2) background technology
Patent No. ZL200710015256.X, title " a kind of method that the dry method spandex waste silk is regenerated as normal spandex silk " disclose the method that a kind of dry method spandex waste silk utilizes again, to solve environmental pollution, the raising spandex input and output rate that spandex waste silk causes.This method is with spandex waste silk elder generation low-temperature grinding, and through water and detergent washing, drying drops into reactor together with organic solvent, auxiliary agent then, reacts down at 45 ℃～100 ℃ to obtain spinning solution in 6～12 hours.This patented method can become regenerating dry-spinning waste polyurethane filament the spandex silk, and the whole operation program is simple.But, because the viscosity of spandex waste silk differs bigger, and additive dosage is very little, cause the auxiliary agent and the spandex waste silk of interpolation to be difficult to mix, then directly influence stability, the homogeneity of the spinning solution that spandex waste silk obtains, remote-effects the spinnability of stoste, and then influence the quality of regenerated silk; In addition, by the stoste shortage chlorine resistance of its gained, the swimsuit finished product of especially making is subject to the erosion of active chlorine can lose its intensity and elasticity, so limited its scope of application relatively.
(3) summary of the invention
The objective of the invention is to overcome above-mentioned deficiency, provide a kind of can be with the method for the spandex fiber stoste of regenerating dry-spinning waste polyurethane filament stability, homogeneity and good spinnability.
Another object of the present invention provides the additive of the chlorine resistance that replenishes spandex fiber stoste, can make it make the useful spandex fiber stoste of chlorine resistance.
The object of the present invention is achieved like this: with regenerating dry-spinning waste polyurethane filament is the method that contains the spandex fiber stoste of anti-chlorine characteristic, and described method comprises following technical process:
Step 1, at-30 ℃～-40 ℃, utilize the weak elasticity and the brittle behavior of spandex silk performance, spandex waste silk is ground into staple fibre;
Step 2, clean spandex waste silk 10～90min, wash finish and other impurity on spandex waste silk surface off, then oven dry with 40 ℃～100 ℃ water and washing agent;
Step 3, earlier add that to account for the spandex waste silk mass percent be 50～200% organic solvent, add spandex waste silk then, add again that to account for the spandex waste silk mass percent be 46.4～284.0% organic solvent at last, at N
2Under the protection, stirring reaction 2～4 hours, reaction temperature is 50 ℃～100 ℃;
Reaction controlling agent after step 4, spray are allocated with the described organic solvent of step 3, spray speed is 0.01～1Kg/min, stirs 20～100min;
Reaction promoter after step 5, interpolation are allocated with the described organic solvent of step 3 stirs 20～120min, can obtain the spinning solution of appropriate viscosity after the slaking;
Described organic solvent is dimethylacetylamide (DMAC) or dimethyl formamide (DMF);
Described reaction controlling agent is the mixture of monoamine and diamine, and the mol ratio of the two is a monoamine: diamine=8: (1～4); The mass percent that the reaction controlling agent accounts for the organic solvent of its allotment is 5～6%, and the addition of reaction controlling agent is: the mass percent that accounts for spandex waste silk is 0.01%～0.4%;
Described reaction promoter is made up of the antiager that accounts for spandex waste silk 0.01%～0.5% mass percent, the anti-yellow agent that accounts for spandex waste silk 0.01%～0.5% mass percent, the lubricant that accounts for the anti-chlorine additive of spandex waste silk 0.1%～3.0% mass percent and account for spandex waste silk 0.01%～0.5% mass percent;
Described reaction promoter grinds the back allotment;
Described antiager is the mixture that has the mixture of synergistic Ciba 1790 and Ciba 622 or have synergistic Ciba 245 and Ciba 622, wherein the mass ratio of the two is Ciba 1790: Ciba 622=1: 3, or Ciba 245: Ciba 622=1: 3;
Described anti-yellow agent is SAS or Ciba HN-150;
Described anti-chlorine additive is a kind of in zinc oxide (ZnO), hydrotalcite or the mixture (ZnO/DESn) with synergistic zinc oxide and dibutyl tin laurate, and described ZnO/DESn mixture quality is than being ZnO: DESn=4: 1;
Described lubricant is a dolomol;
The mass percent that described antiager, anti-yellow agent and anti-chlorine additive account for the organic solvent of its allotment is 30～35%, and the mass percent that lubricant accounts for the organic solvent of its allotment is 8～9%.
The invention has the beneficial effects as follows:
The present invention can make interpolation auxiliary agent and spandex waste silk mix, and obtains the regeneration spinning solution of better stability and homogeneity, further improves the spinnability of regeneration stoste.And, improve the chlorine-resistant property of regeneration stoste, and then improved the regenerated silk product quality, widened its scope of application.
(4) specific embodiment
Describe the present invention in detail below in conjunction with embodiment, but these embodiment must not be interpreted as the limitation of the present invention that goes up in all senses.
Embodiment 1:
One, batching
1, allotment reaction controlling agent: be monoamine and diamine to join container at 8: 1 according to mol ratio at first, add the organic solvent dimethylacetylamide then, be deployed into mass percent and be 5.1% solution;
2, allotment reaction promoter: after at first reaction promoter being ground, react the program of controlling agent again according to allotment, 3 mass ratioes), anti-yellow agent SAS and the ZnO of anti-the chlorine additive all be deployed into 32% solution (Ciba245: Ciba 622=1:, it is 8.5% solution that magnesium stearate lubricant is deployed into mass percent the mixture of antiager Ciba 245 and Ciba 622 to use dimethylacetylamide respectively.
Two, make
Step 1, at-30 ℃～-40 ℃, utilize the weak elasticity and the brittle behavior of spandex silk performance, spandex waste silk is ground into staple fibre;
Step 2, clean 10～90min, wash finish and other impurity on spandex waste silk surface off, then oven dry with 40 ℃～100 ℃ water and washing agent;
Step 3, elder generation add 12.5Kg DMAC dipping reactor, will drop in the reactor through the spandex waste silk 25.0Kg after step 2 oil removing, the oven dry then, add 11.6Kg DMAC at last again, at N
2Under the protection, stirring reaction 2～4 hours, reaction temperature is 50 ℃～100 ℃;
Reaction controlling agent after step 4, spray are allocated with DMAC, spray speed is 0.01～1Kg/min, addition is 0.05Kg, stirs 20～100min;
Step 5, the interpolation deployed reaction promoter of DMAC, its addition is respectively: the mixture 0.12Kg of antiager Ciba 245 and Ciba 622, anti-yellow agent SAS 0.08Kg, the ZnO of anti-chlorine additive 0.9Kg, magnesium stearate lubricant 0.08Kg, stir 20～120min, can obtain the spinning solution that appropriate viscosity contains anti-chlorine characteristic after the slaking.
Embodiment 2:
The difference of the present invention and embodiment 1 is:
Add 25.0Kg DMAC dipping reactor earlier, behind the spandex waste silk input reactor after oil removing, the oven dry, add 22.10Kg DMAC again; In the reaction controlling agent, the mol ratio of monoamine and diamine is 6: 1, and addition is 1.0Kg; Antiager is that (Ciba 1790: Ciba 622=1: 3 mass ratioes), addition is 0.16Kg for the mixture of Ciba 1790 and Ciba 622; Anti-yellow agent SAS addition is 0.01Kg; (ZnO: DESn=4: 1) addition is 1.5Kg to the ZnO/DESn of anti-the chlorine additive; The magnesium stearate lubricant addition is 0.9Kg.
Embodiment 3:
The difference of the present invention and embodiment 1 is:
Used organic solvent is DMF, adds 50.0Kg DMF dipping reactor earlier, behind the spandex waste silk input reactor after oil removing, the oven dry, adds 20.5Kg DMF again; In the reaction controlling agent, the mol ratio of monoamine and diamine is 5: 1, and addition is 1.5Kg; Antiager is the mixture of Ciba 245 and Ciba622, and addition is 0.01Kg; Anti-yellow agent Ciba HN-150, addition is 0.32Kg; The ZnO of anti-chlorine additive addition is 2.0Kg; The magnesium stearate lubricant addition is 1.47Kg.
Embodiment 4:
The difference of the present invention and embodiment 1 is:
Used organic solvent is DMF, adds the DMF of 50.0Kg earlier, with behind the spandex waste silk input reactor after oil removing, the oven dry, adds 46.2Kg DMF more then; In the reaction controlling agent, the mol ratio of monoamine and diamine is 4: 1, and addition is 1.96Kg; Antiager is the mixture of Ciba 1790 and Ciba622, and addition is 0.39Kg; Anti-yellow agent SAS addition is 0.39Kg; The hydrotalcite of anti-chlorine additive addition is 2.0Kg; The magnesium stearate lubricant addition is 0.03Kg.
Embodiment 5:
The difference of the present invention and embodiment 1 is:
Add 50.0Kg DMAC dipping reactor earlier, with behind the spandex waste silk input reactor after oil removing, the oven dry, add 70.9Kg DMAC more then; In the reaction controlling agent, the mol ratio of monoamine and diamine is 2: 1, and addition is 1.96Kg; The mixture of antiager Ciba 245 and Ciba 622, addition are 0.25Kg; Anti-yellow agent Ciba HN-150 addition is 0.39Kg, and the hydrotalcite of anti-chlorine additive addition is 2.34Kg; The magnesium stearate lubricant addition is 0.3Kg.
Claims (1)
1. one kind is the method that contains the spandex fiber stoste of anti-chlorine characteristic with regenerating dry-spinning waste polyurethane filament, and it is characterized in that: described method comprises following technical process:
Step 1, at-30 ℃～-40 ℃, spandex waste silk is ground into staple fibre;
Step 2, clean spandex waste silk 10～90min with 40 ℃～100 ℃ water and washing agent, oven dry then;
Step 3, earlier add that to account for the spandex waste silk mass percent be 50～200% organic solvent, add spandex waste silk then, add again that to account for the spandex waste silk mass percent be 46.4～284.0% organic solvent at last, at N
2Under the protection, stirring reaction 2～4 hours, reaction temperature is 50 ℃～100 ℃;
Reaction controlling agent after step 4, spray are allocated with the described organic solvent of step 3, spray speed is 0.01～1Kg/min, stirs 20～100min;
Reaction promoter after step 5, interpolation are allocated with the described organic solvent of step 3 stirs 20～120min, can obtain the spinning solution of appropriate viscosity after the slaking;
Described organic solvent is dimethylacetylamide or dimethyl formamide;
Described reaction controlling agent is the mixture of monoamine and diamine, and the mol ratio of the two is a monoamine: diamine=8: 1～4; The mass percent that the reaction controlling agent accounts for the organic solvent of its allotment is 5～6%, and the addition of reaction controlling agent is: the mass percent that accounts for spandex waste silk is 0.01%～0.4%;
Described reaction promoter is made up of the antiager that accounts for spandex waste silk 0.01%～0.5% mass percent, the anti-yellow agent that accounts for spandex waste silk 0.01%～0.5% mass percent, the lubricant that accounts for the anti-chlorine additive of spandex waste silk 0.1%～3.0% mass percent and account for spandex waste silk 0.01%～0.5% mass percent;
Described reaction promoter grinds the back allotment;
Described antiager is the mixture of Ciba 1790 and Ciba 622 or the mixture of Ciba 245 and Ciba622, and wherein the mass ratio of the two is Ciba 1790: Ciba 622=1: 3, or Ciba245: Ciba 622=1: 3;
Described anti-yellow agent is SAS or Ciba HN-150;
A kind of in the mixture that described anti-chlorine additive is hydrotalcite, zinc oxide, magnesia or zinc oxide and dibutyl tin laurate, described zinc oxide and dibutyl tin laurate mixture quality are than being zinc oxide: dibutyl tin laurate=4: 1;
Described lubricant is a dolomol;
The mass percent that described antiager, anti-yellow agent and anti-chlorine additive account for the organic solvent of its allotment is 30～35%, and the mass percent that lubricant accounts for the organic solvent of its allotment is 8～9%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102490115A CN101922063B (en) | 2010-08-05 | 2010-08-05 | Method for regenerating dry-spinning waste polyurethane filament into polyurethane spinning stock solution with chlorine resistance |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102490115A CN101922063B (en) | 2010-08-05 | 2010-08-05 | Method for regenerating dry-spinning waste polyurethane filament into polyurethane spinning stock solution with chlorine resistance |
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| CN101922063A CN101922063A (en) | 2010-12-22 |
| CN101922063B true CN101922063B (en) | 2011-10-19 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102251316B (en) * | 2011-06-14 | 2012-11-28 | 吴中虎 | Method for producing spandex filament by using recycled spandex filament wastes |
| CN102277649B (en) * | 2011-07-19 | 2013-02-27 | 奥斯汀新材料（张家港）有限公司 | Method for preparing melt-spinning chlorine-resistant high-resilience spandex fiber |
| CN104073904B (en) * | 2014-07-17 | 2016-01-20 | 江苏侨新纤维有限公司 | A kind of spandex waste silk that utilizes prepares the method for hygienic material with thick dawn spandex fibre |
| CN105133093B (en) * | 2015-09-04 | 2017-07-04 | 浙江宝莲纤维科技有限公司 | A kind of method of dry-spinning waste polyurethane filament highly efficient regeneration spandex thread |
| CN107447289A (en) * | 2017-09-19 | 2017-12-08 | 常州朋悦纺织品有限公司 | A kind of preparation method of modified spandex |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1122850A (en) * | 1995-09-13 | 1996-05-22 | 连云港钟山氨纶有限公司 | Chlorine-resistance spandex fibre prodn. method |
| KR100268113B1 (en) * | 1998-08-18 | 2000-10-16 | 이귀영 | Method of recycling polyureathane wasted yarns |
| KR100448722B1 (en) * | 2001-08-24 | 2004-09-13 | 대진합성화학 주식회사 | Regenerating method of waste spandex and manufacturing method of synthetic and artificial leather |
| CN100494525C (en) * | 2007-07-06 | 2009-06-03 | 烟台氨纶股份有限公司 | Method for regenerating normal spandex fibre from dry spinning spandex waste silk |
| CN101096783A (en) * | 2007-07-06 | 2008-01-02 | 烟台氨纶股份有限公司 | Process for manufacturing chlorine-resistant spandex fibre |
| CN101760799B (en) * | 2010-01-15 | 2011-12-14 | 连云港宏润再生资源有限公司 | Regeneration method of dry spinning spandex waste silk |
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