CN109868524B - Melt-spun spandex slice and preparation method thereof - Google Patents
Melt-spun spandex slice and preparation method thereof Download PDFInfo
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- CN109868524B CN109868524B CN201811599140.XA CN201811599140A CN109868524B CN 109868524 B CN109868524 B CN 109868524B CN 201811599140 A CN201811599140 A CN 201811599140A CN 109868524 B CN109868524 B CN 109868524B
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- 229920002334 Spandex Polymers 0.000 title claims abstract description 53
- 239000004759 spandex Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title description 7
- 229920005862 polyol Polymers 0.000 claims abstract description 32
- 150000003077 polyols Chemical class 0.000 claims abstract description 32
- 238000001035 drying Methods 0.000 claims abstract description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 24
- 229920001610 polycaprolactone Polymers 0.000 claims description 13
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 13
- 238000004806 packaging method and process Methods 0.000 claims description 11
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 9
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000007725 thermal activation Methods 0.000 claims description 9
- PMMYEEVYMWASQN-IMJSIDKUSA-N cis-4-Hydroxy-L-proline Chemical compound O[C@@H]1CN[C@H](C(O)=O)C1 PMMYEEVYMWASQN-IMJSIDKUSA-N 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 239000005038 ethylene vinyl acetate Substances 0.000 abstract description 15
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 abstract description 15
- 239000004970 Chain extender Substances 0.000 abstract description 8
- 239000004721 Polyphenylene oxide Substances 0.000 abstract description 8
- 239000012948 isocyanate Substances 0.000 abstract description 8
- 150000002513 isocyanates Chemical class 0.000 abstract description 8
- 229920005906 polyester polyol Polymers 0.000 abstract description 8
- 229920000570 polyether Polymers 0.000 abstract description 8
- 206010053615 Thermal burn Diseases 0.000 abstract description 4
- 238000004043 dyeing Methods 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 17
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 12
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 6
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000004814 polyurethane Substances 0.000 description 3
- 229920002635 polyurethane Polymers 0.000 description 3
- ZUFUSIMENKJSMG-UHFFFAOYSA-N 1-methyl-3,5-bis(methylsulfanyl)benzene Chemical compound CSC1=CC(C)=CC(SC)=C1 ZUFUSIMENKJSMG-UHFFFAOYSA-N 0.000 description 2
- PISLZQACAJMAIO-UHFFFAOYSA-N 2,4-diethyl-6-methylbenzene-1,3-diamine Chemical compound CCC1=CC(C)=C(N)C(CC)=C1N PISLZQACAJMAIO-UHFFFAOYSA-N 0.000 description 2
- KCIZUAMTTBFYNX-UHFFFAOYSA-N 4-hydroperoxyphenol Chemical compound OOC1=CC=C(O)C=C1 KCIZUAMTTBFYNX-UHFFFAOYSA-N 0.000 description 2
- 239000005058 Isophorone diisocyanate Substances 0.000 description 2
- MRUXVMBOICABIU-UHFFFAOYSA-N [3,5-bis(methylsulfanyl)phenyl]methanediamine Chemical compound CSC1=CC(SC)=CC(C(N)N)=C1 MRUXVMBOICABIU-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 125000005442 diisocyanate group Chemical group 0.000 description 2
- -1 dimethylene phenyl glycol Chemical compound 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 238000010409 ironing Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920003225 polyurethane elastomer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Landscapes
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a melt-spun spandex slice, which is obtained by adding polyether polyol, polyester polyol, ethylene-vinyl acetate copolymer, isocyanate and a chain extender into a reactive double-screw extruder, extruding and granulating and drying. The melt-spun spandex slice has lower Vicat softening temperature, and spandex yarns produced by the spandex also have lower Vicat softening temperature, are convenient to scald and finish, and have high rebound rate and good dyeing property.
Description
Technical Field
The invention relates to the field of polyurethane, in particular to a melt-spun spandex slice and a preparation method thereof.
Background
Melt-spun spandex slices are the upstream raw material for manufacturing melt-spun spandex filaments, and at present, the spandex at home and abroad mainly has two types according to different manufacturing methods: namely dry spandex and melt-spun spandex, the melt-spun spandex has the obvious advantage over the dry spandex of ー that the production process does not use solvents, so the dry spandex is called as 'green spandex'. Is an important chemical fiber raw material for manufacturing spandex high-grade clothes and underwear, and is generally favored by textile and chemical fiber markets at home and abroad. Melt-spun spandex, however, has limited its application to a large extent because of its lower heat resistance and elasticity than dry spandex. The heat resistance and resilience of the melt-spun spandex filament depend on the heat resistance and mechanical properties of the melt-spun spandex slice to a great extent. Improving the heat resistance and mechanical properties of melt-spun spandex slices becomes ー hot spots and difficulties which are commonly concerned by the industry of melt-spun spandex and polyurethane elastomers. Melt-spun spandex slices produced by the prior art have higher Vicat softening temperature, so that spandex filaments produced by the spandex slices have higher Vicat softening temperature, cause certain troubles for ironing, are not suitable for ー application fields needing lower Vicat softening temperature, and have low rebound resilience rate and poor dyeability.
Because the melt-spun spandex has high processing temperature, compared with dry-spun spandex, the rebound resilience and the heat resistance are poorer, and in order to improve the performance of the melt-spun spandex, an upstream product, namely a polyurethane slice needs to be modified so as to improve the performance of a final product, Chinese patent application CN01115739 is added with nano powder in the spandex slice and is blended for spinning, so that the thermal performance and the mechanical performance of the melt-spun spandex can be improved; the Chinese patent application CN200410065487 adopts a method of mixing assistants such as cross-linking agent, heat stabilizer and the like into polyester slices to improve the performance of melt-spun spandex; but the blending uniformity of the polyurethane slices, the additives and the like is difficult to control, and the quality control of melt-spun spandex is difficult.
Based on the situation, the invention provides a melt-spun spandex slice and a preparation method thereof, which can effectively solve the problems.
Disclosure of Invention
The invention aims to provide a melt-spun spandex slice and a preparation method thereof. The melt-spun spandex slice has lower Vicat softening temperature, and spandex yarns produced by the spandex also have lower Vicat softening temperature, are convenient to scald and finish, and have high rebound rate and good dyeing property.
The invention is realized by the following technical scheme:
a melt-spun spandex slice is prepared by adding polyether polyol, polyester polyol, ethylene-vinyl acetate copolymer, isocyanate and a chain extender into a reactive double-screw extruder, extruding, granulating and drying.
The melt-spun spandex slice has lower Vicat softening temperature, and spandex yarns produced by the spandex also have lower Vicat softening temperature, are convenient to scald and finish, and have high rebound rate and good dyeing property.
Preferably, the polyester polyol is poly epsilon-caprolactone diol; the polyether polyol is polytetrahydrofuran polyol.
Preferably, the number average molecular weight of the polyester polyol and the polyether polyol is 500-5000.
Preferably, the content of vinyl acetate in the ethylene-vinyl acetate copolymer is 10-88%.
Preferably, the content of vinyl acetate in the ethylene-vinyl acetate copolymer is 44-80%.
Preferably, the chain extender is any one or more of ethylene glycol, propylene glycol, 1, 4-butanediol, diethylene glycol, 1, 4-cyclohexanediol, dimethylene phenyl glycol, hydroquinone hydroxy ether, diethyl toluene diamine and 3, 5-dimethyl thio toluene diamine.
Preferably, the isocyanate is any one or more of 4, 4 '-diphenylmethane diisocyanate, toluene diisocyanate, hexamethylene diisocyanate, isophorone diisocyanate, and (4, 4' -dicyclohexylmethane) diisocyanate.
The invention also provides a preparation method of the melt-spun spandex slice, which is characterized by comprising the following steps:
A. uniformly blending poly-epsilon-caprolactone glycol, polytetramethylene ether glycol and ethylene-vinyl acetate copolymer to obtain mixed polyol;
B. and (3) pumping the mixed polyol, the isocyanate and the chain extender into a reaction double screw by using a metering pump, carrying out underwater granulation at the reaction temperature of 160-200 ℃, drying and packaging to obtain the melt-spun spandex slice.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the melt-spun spandex slice has lower Vicat softening temperature, and spandex yarns produced by the spandex also have lower Vicat softening temperature, are convenient to scald and finish, and have high rebound rate and good dyeing property.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
The test methods or test methods described in the following examples are conventional methods unless otherwise specified; the reagents and materials, unless otherwise indicated, are conventionally obtained commercially or prepared by conventional methods.
The molecular weight in the invention is number average molecular weight.
Example 1:
a melt-spun spandex slice is prepared by adding polyether polyol, polyester polyol, ethylene-vinyl acetate copolymer, isocyanate and a chain extender into a reactive double-screw extruder, extruding, granulating and drying.
Example 2:
a melt-spun spandex slice is prepared by adding polyether polyol, polyester polyol, ethylene-vinyl acetate copolymer, isocyanate and a chain extender into a reactive double-screw extruder, extruding, granulating and drying.
Preferably, the polyester polyol is poly epsilon-caprolactone diol; the polyether polyol is polytetrahydrofuran polyol.
Preferably, the number average molecular weight of the polyester polyol and the polyether polyol is 500-5000.
Preferably, the content of vinyl acetate in the ethylene-vinyl acetate copolymer is 10-88%.
Preferably, the content of vinyl acetate in the ethylene-vinyl acetate copolymer is 44-80%.
Preferably, the chain extender is any one or more of ethylene glycol, propylene glycol, 1, 4-butanediol, diethylene glycol, 1, 4-cyclohexanediol, dimethylene phenyl glycol, hydroquinone hydroxy ether, diethyl toluene diamine and 3, 5-dimethyl thio toluene diamine.
Preferably, the isocyanate is any one or more of 4, 4 '-diphenylmethane diisocyanate, toluene diisocyanate, hexamethylene diisocyanate, isophorone diisocyanate, and (4, 4' -dicyclohexylmethane) diisocyanate.
The invention also provides a preparation method of the melt-spun spandex slice, which is characterized by comprising the following steps:
A. uniformly blending poly-epsilon-caprolactone glycol, polytetramethylene ether glycol and ethylene-vinyl acetate copolymer to obtain mixed polyol;
B. and (3) pumping the mixed polyol, the isocyanate and the chain extender into a reaction double screw by using a metering pump, carrying out underwater granulation at the reaction temperature of 160-200 ℃, drying and packaging to obtain the melt-spun spandex slice.
Example 3
70 parts of poly-epsilon-caprolactone glycol (with the molecular weight of 2500), 20 parts of polytetramethylene ether glycol (with the molecular weight of 2000) and 10 parts of ethylene-vinyl acetate copolymer EVA (with the vinyl acetate VA content of 60%) are uniformly blended to obtain mixed polyol; and (3) using a metering pump to obtain a mixed solution with a mol ratio of 1.03: 0.97: 2, putting the mixed polyol, 1, 4-butanediol and hexamethylene diisocyanate into a reaction double screw, reacting at the temperature of 170 ℃, granulating underwater, drying and packaging to obtain the product. The thermal activation temperature (the setting temperature of spandex and nylon blending) of the product is 110 ℃, the hardness is 80A, the resilience rate is 78 percent, and the breaking tensile strength is 15 Mpa.
Comparative example 1
70 parts of poly-epsilon-caprolactone glycol (with the molecular weight of 2500) and 20 parts of polytetramethylene ether glycol (with the molecular weight of 2000) are uniformly blended to obtain mixed polyol; and (3) using a metering pump to obtain a mixed solution with a mol ratio of 1.03: 0.97: 2, putting the mixed polyol, 1, 4-butanediol and hexamethylene diisocyanate into a reaction double screw, reacting at the temperature of 170 ℃, granulating underwater, drying and packaging to obtain the product. The thermal activation temperature of the product is 120 ℃, the hardness is 82A, the rebound rate is 69%, and the breaking tensile strength is 16 Mpa.
Example 4
80 parts of poly-epsilon-caprolactone glycol (with the molecular weight of 1000), 10 parts of polytetramethylene ether glycol (with the molecular weight of 1500) and 10 parts of EVA (with the VA content of 60%) are uniformly blended to obtain mixed polyol; and (3) using a metering pump to obtain a mixed solution with a mol ratio of 1.03: 0.97: 2, adding mixed polyol, 3, 5-dimethylthiotoluenediamine and 4, 4' -diphenylmethane diisocyanate into a reaction double screw, reacting at the temperature of 190 ℃, granulating underwater, drying and packaging to obtain the product. The thermal activation temperature of the product is 110 ℃, the hardness is 85A, the rebound resilience is 85 percent, and the breaking tensile strength is 35 Mpa.
Comparative example 2
80 parts of poly-epsilon-caprolactone glycol (with the molecular weight of 1000) and 10 parts of polytetramethylene ether glycol (with the molecular weight of 1500) are uniformly blended to obtain mixed polyol; and (3) using a metering pump to obtain a mixed solution with a mol ratio of 1.03: 0.97: 2, adding mixed polyol, 3, 5-dimethylthiotoluenediamine and 4, 4' -diphenylmethane diisocyanate into a reaction double screw, reacting at the temperature of 190 ℃, granulating underwater, drying and packaging to obtain the product. The thermal activation temperature of the product is 130 ℃, the hardness is 86A, the rebound rate is 80 percent, and the breaking tensile strength is 37 Mpa.
Example 5
60 parts of poly-epsilon-caprolactone glycol (with the molecular weight of 1500), 20 parts of polytetramethylene ether glycol (with the molecular weight of 1000) and 20 parts of EVA (with the VA content of 60%) are uniformly blended to obtain mixed polyol; and (3) using a metering pump to obtain a mixed solution with a mol ratio of 1.03: 0.97: 2, putting the mixed polyol, 1, 4-butanediol and 4, 4' -diphenylmethane diisocyanate into a reaction double screw, reacting at the temperature of 190 ℃, granulating underwater, drying and packaging to obtain the product. The thermal activation temperature of the product is 115 ℃, the hardness is 86A, the rebound resilience is 86 percent, and the breaking tensile strength is 27 Mpa.
Comparative example 3
60 parts of poly-epsilon-caprolactone glycol (with the molecular weight of 1500) and 20 parts of polytetramethylene ether glycol (with the molecular weight of 1000) are uniformly blended to obtain mixed polyol; and (3) using a metering pump to obtain a mixed solution with a mol ratio of 1.03: 0.97: 2, putting the mixed polyol, 1, 4-butanediol and 4, 4' -diphenylmethane diisocyanate into a reaction double screw, reacting at the temperature of 190 ℃, granulating underwater, drying and packaging to obtain the product. The thermal activation temperature of the product is 125 ℃, the hardness is 88A, the rebound resilience is 84%, and the breaking tensile strength is 29 Mpa.
Example 6
85 parts of poly-epsilon-caprolactone diol (with the molecular weight of 4500), 5 parts of polytetramethylene ether glycol (with the molecular weight of 500) and 15 parts of EVA (with the VA content of 60%) are uniformly blended to obtain mixed polyol; and (3) using a metering pump to obtain a mixed solution with a mol ratio of 1.03: 0.97: 2, adding the mixed polyol, the 1, 4-cyclohexanediol and the 4, 4' -diphenylmethane diisocyanate into a reaction double screw, reacting at the temperature of 190 ℃, granulating underwater, drying and packaging to obtain the product. The thermal activation temperature of the product is 125 ℃, the hardness is 85A, the rebound rate is 88 percent, and the breaking tensile strength is 40 Mpa.
Comparative example 4
85 parts of poly-epsilon-caprolactone diol (with the molecular weight of 4500) and 5 parts of polytetramethylene ether glycol (with the molecular weight of 500) are uniformly blended to obtain mixed polyol; and (3) using a metering pump to obtain a mixed solution with a mol ratio of 1.03: 0.97: 2, adding the mixed polyol, the 1, 4-cyclohexanediol and the 4, 4' -diphenylmethane diisocyanate into a reaction double screw, reacting at the temperature of 190 ℃, granulating underwater, drying and packaging to obtain the product. The thermal activation temperature of the product is 135 ℃, the hardness is 86A, the rebound rate is 81 percent, and the breaking tensile strength is 45 Mpa.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and all simple modifications and equivalent variations of the above embodiments according to the technical spirit of the present invention are included in the scope of the present invention.
Claims (1)
1. A melt-spun spandex chip, characterized in that: 85 parts of poly-epsilon-caprolactone glycol with the molecular weight of 4500, 5 parts of polytetramethylene ether glycol with the molecular weight of 500 and 15 parts of EVA with the VA content of 60 percent are uniformly blended to obtain mixed polyol; and (3) using a metering pump to obtain a mixed solution with a mol ratio of 1.03: 0.97: 2, putting the mixed polyol, the 1, 4-cyclohexanediol and the 4, 4' -diphenylmethane diisocyanate into a reaction double screw, and granulating, drying and packaging under water at the reaction temperature of 190 ℃; the thermal activation temperature of the product is 125 ℃, the hardness is 85A, the rebound rate is 88 percent, and the breaking tensile strength is 40 Mpa.
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| CN112501767B (en) * | 2020-11-25 | 2022-07-26 | 武汉猫人云商科技有限公司 | Integrated trousers and production process thereof |
| CN113861917A (en) * | 2021-09-27 | 2021-12-31 | 深圳市联星服装辅料有限公司 | Primer, glue, super-soft waterproof zipper and production method thereof |
| CN114230753A (en) * | 2021-12-09 | 2022-03-25 | 烟台泰和新材料股份有限公司 | Preparation method of polyether ester type melt-spun spandex slice |
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Effective date of registration: 20221230 Address after: No. 2999, Renmin North Road, Songjiang District, Shanghai, 201699 Patentee after: Wu Jianru Address before: 314000 68 Yanhu Road, Baibu Town, Haiyan County, Jiaxing City, Zhejiang Province Patentee before: ZHEJIANG JILUN HIGH POLYMER MATERIAL Co.,Ltd. |