CN111101230A - Spandex with good heat-resistant stability and preparation method thereof - Google Patents
Spandex with good heat-resistant stability and preparation method thereof Download PDFInfo
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- CN111101230A CN111101230A CN201911374828.2A CN201911374828A CN111101230A CN 111101230 A CN111101230 A CN 111101230A CN 201911374828 A CN201911374828 A CN 201911374828A CN 111101230 A CN111101230 A CN 111101230A
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- spandex
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- good heat
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6685—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses spandex with good heat-resistant stability and a preparation method thereof, belonging to the field of spandex materials, wherein the spandex with good heat-resistant stability comprises the following raw materials in parts by weight: 50-75 parts of polytetramethylene ether glycol, 12-18 parts of isophorone diisocyanate, 1.5-3 parts of a chain extender, 0.3-1 part of a stabilizer, 0.2-1 part of a terminator, 0.1-0.3 part of quaternary ammonium salt and 2-6 parts of a modified additive. The spandex with good heat resistance and stability has high heat resistance and good stability.
Description
Technical Field
The invention relates to the field of spandex, in particular to spandex with good heat-resistant stability and a preparation method thereof.
Background
Spandex is a short for polyurethane fiber and is an elastic fiber. Spandex generally consists of a plurality of filaments, generally 10D/filament, 15D/filament, even 20D/filament, the smaller the theoretical number of filament, the better the evenness of yarn evenness, because the chance rate of overlapping shape is smaller, the production solution DMAC produced by dry spinning is harmful to the liver of human body, generally 0.5mg/kg is contained in 10D/filament, and if 15D/filament, 0.7mg/kg is contained, which exceeds the standard. When producing spandex fiber, special attention is paid to breaking strength, breaking elongation, forming degree, oil adhesion, elastic recovery rate and the like, and the problems directly affect weaving, and especially, the production of single-faced cloth by knitting is more attentive. The spandex fiber disclosed by the prior art mainly has the functions of light guide, flame retardance, ultraviolet resistance and the like, but has poor heat resistance.
Disclosure of Invention
The invention aims to provide spandex with good heat-resistant stability and a preparation method thereof, wherein the heat resistance of the spandex is obviously improved compared with that of the conventional spandex.
In order to achieve the purpose, the invention provides the following technical scheme:
spandex with good heat-resistant stability comprises the following raw materials in parts by weight: 50-75 parts of polytetramethylene ether glycol, 12-18 parts of isophorone diisocyanate, 1.5-3 parts of a chain extender, 0.3-1 part of a stabilizer, 0.2-1 part of a terminator, 0.5-2 parts of antimony potassium tartrate, 0.1-0.3 part of quaternary ammonium salt and 2-6 parts of a modified additive;
the modified additive comprises the following raw materials in parts by weight: 1-3 parts of flatting agent, 0.5-1 part of lubricant, 0.1-0.8 part of antioxidant and 1-3 parts of anti-ultraviolet agent.
Preferably, the chain extender comprises ethylenediamine and butanediamine, and the molar ratio of the ethylenediamine to the butanediamine is 3: 1-8:1.
Preferably, the stabilizer is vinyl pyrrolidone.
Preferably, the terminating agent is diethylamine.
Preferably, the quaternary ammonium salt is dodecyl dimethyl benzyl ammonium chloride.
A preparation method of spandex with good heat-resistant stability comprises the following steps:
(1) prepolymerization reaction: mixing polytetramethylene ether glycol and isophorone diisocyanate, reacting at 68-72 ℃ for 120min, then using N, N-dimethylacetamide as a solvent, fully dissolving a prepolymer, and cooling to obtain a prepolymer solution;
(2) polymerization reaction: transferring the prepolymer solution into a polymerization reactor, uniformly stirring, and performing chain extension and chain termination by controlling addition of a chain extender and a terminator at low temperature to obtain a polymer solution;
(3) adding auxiliary materials: continuously transferring polymer solution continuously generated by potassium antimony tartrate and quaternary ammonium salt in a polymerization reactor into a stirring tank, and simultaneously adding quaternary ammonium salt and a modified additive into the stirring tank to obtain a spandex spinning stock solution;
(4) spinning: and (4) preparing the spandex spinning stock solution prepared in the step (3) into spandex fibers by adopting a dry spinning method.
Preferably, in the step (2), a cooling pipe is coiled outside the polymerization reactor for controlling the temperature inside the polymerization reactor.
Preferably, in the step (1), polytetramethylene ether glycol and isophorone diisocyanate are mixed and reacted at a temperature of 70 ℃ for 120min, and then the prepolymer is sufficiently dissolved by using N, N-dimethylacetamide as a solvent, and a prepolymer solution is obtained after cooling.
Compared with the prior art, the invention has the beneficial effects that:
compared with the traditional spandex material, the raw material of the invention is also added with a modified additive which contains an antioxidant and an anti-ultraviolet agent, on one hand, the antioxidant can delay or inhibit the oxidation process of the polymer and prevent the aging of the polymer, on the other hand, the antioxidant can prevent the thermal oxidation degradation in the reprocessing process of other raw material polymers, and the prepared spandex material is not volatilized and is not decomposed at higher temperature, thereby greatly improving the heat-resistant stability of the traditional spandex material; meanwhile, the ultraviolet resistant agent can inhibit and delay ultraviolet rays from causing photo-aging on the polymer, and the stability of the spandex material is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Spandex with good heat-resistant stability comprises the following raw materials in parts by weight: 50 parts of polytetramethylene ether glycol, 12 parts of isophorone diisocyanate, 1.5 parts of a chain extender, 0.3 part of a stabilizer, 0.2 part of a terminator, 0.5 part of antimony potassium tartrate, 0.1 part of quaternary ammonium salt and 2 parts of a modified additive; the modified additive comprises the following raw materials in parts by weight: 1 part of flatting agent, 0.5 part of lubricating agent, 0.1 part of antioxidant and 1 part of anti-ultraviolet agent; the chain extender comprises ethylenediamine and butanediamine, and the molar ratio of the ethylenediamine to the butanediamine is 3: 1; the stabilizer is vinyl pyrrolidone; the terminator is diethylamine; the quaternary ammonium salt is dodecyl dimethyl benzyl ammonium chloride.
A preparation method of spandex with good heat-resistant stability comprises the following steps:
(1) prepolymerization reaction: mixing polytetramethylene ether glycol (molecular weight is 1800) and isophorone diisocyanate, reacting at 68 ℃ for 120min, then using N, N-dimethylacetamide as a solvent, fully dissolving a prepolymer, and cooling to obtain a prepolymer solution;
(2) polymerization reaction: transferring the prepolymer solution into a polymerization reactor, uniformly stirring, arranging a cooling pipe outside the polymerization reactor in a coiling manner, controlling the temperature in the polymerization reactor, and controlling the addition of a chain extender and a terminator at low temperature to perform chain extension and chain termination to obtain a polymer solution;
(3) adding auxiliary materials: continuously transferring polymer solution continuously generated by potassium antimony tartrate and quaternary ammonium salt in a polymerization reactor into a stirring tank, and simultaneously adding quaternary ammonium salt and a modified additive into the stirring tank to obtain a spandex spinning stock solution;
(4) spinning: and (4) preparing the spandex spinning stock solution prepared in the step (3) into spandex fibers by adopting a dry spinning method.
Example 2
Spandex with good heat-resistant stability comprises the following raw materials in parts by weight: 65 parts of polytetramethylene ether glycol, 15 parts of isophorone diisocyanate, 1.2 parts of a chain extender, 0.7 part of a stabilizer, 2.1 parts of a terminator, 1.2 parts of antimony potassium tartrate, 0.2 part of a quaternary ammonium salt and 4 parts of a modified additive; the modified additive comprises the following raw materials in parts by weight: 2 parts of flatting agent, 0.6 part of lubricating agent, 0.5 part of antioxidant and 2 parts of anti-ultraviolet agent; the chain extender comprises ethylenediamine and butanediamine, and the molar ratio of the ethylenediamine to the butanediamine is 5: 1; the stabilizer is vinyl pyrrolidone; the terminator is diethylamine; the quaternary ammonium salt is dodecyl dimethyl benzyl ammonium chloride.
A preparation method of spandex with good heat-resistant stability comprises the following steps:
(1) prepolymerization reaction: mixing polytetramethylene ether glycol (molecular weight is 1800) and isophorone diisocyanate, reacting at 70 ℃ for 120min, then using N, N-dimethylacetamide as a solvent, fully dissolving a prepolymer, and cooling to obtain a prepolymer solution;
(2) polymerization reaction: transferring the prepolymer solution into a polymerization reactor, uniformly stirring, arranging a cooling pipe outside the polymerization reactor in a coiling manner, controlling the temperature in the polymerization reactor, and controlling the addition of a chain extender and a terminator at low temperature to perform chain extension and chain termination to obtain a polymer solution;
(3) adding auxiliary materials: continuously transferring polymer solution continuously generated by potassium antimony tartrate and quaternary ammonium salt in a polymerization reactor into a stirring tank, and simultaneously adding quaternary ammonium salt and a modified additive into the stirring tank to obtain a spandex spinning stock solution;
(4) spinning: and (4) preparing the spandex spinning stock solution prepared in the step (3) into spandex fibers by adopting a dry spinning method.
Example 3
Spandex with good heat-resistant stability comprises the following raw materials in parts by weight: 75 parts of polytetramethylene ether glycol, 18 parts of isophorone diisocyanate, 2 parts of chain extender, 1 part of stabilizer, 3 parts of terminator, 2 parts of antimony potassium tartrate, 0.3 part of quaternary ammonium salt and 6 parts of modified additive; the modified additive comprises the following raw materials in parts by weight: 3 parts of flatting agent, 1 part of lubricating agent, 0.8 part of antioxidant and 3 parts of anti-ultraviolet agent; the chain extender comprises ethylenediamine and butanediamine, and the molar ratio of the ethylenediamine to the butanediamine is 8: 1; the stabilizer is vinyl pyrrolidone; the terminator is diethylamine; the quaternary ammonium salt is dodecyl dimethyl benzyl ammonium chloride.
A preparation method of spandex with good heat-resistant stability comprises the following steps:
(1) prepolymerization reaction: mixing polytetramethylene ether glycol (molecular weight is 1800) and isophorone diisocyanate, reacting at 72 ℃ for 120min, then using N, N-dimethylacetamide as a solvent, fully dissolving a prepolymer, and cooling to obtain a prepolymer solution;
(2) polymerization reaction: transferring the prepolymer solution into a polymerization reactor, uniformly stirring, arranging a cooling pipe outside the polymerization reactor in a coiling manner, controlling the temperature in the polymerization reactor, and controlling the addition of a chain extender and a terminator at low temperature to perform chain extension and chain termination to obtain a polymer solution;
(3) adding auxiliary materials: continuously transferring polymer solution continuously generated by potassium antimony tartrate and quaternary ammonium salt in a polymerization reactor into a stirring tank, and simultaneously adding quaternary ammonium salt and a modified additive into the stirring tank to obtain a spandex spinning stock solution;
(4) spinning: and (4) preparing the spandex spinning stock solution prepared in the step (3) into spandex fibers by adopting a dry spinning method.
Two spandex fiber materials on the market are selected as a comparative example 1 and a comparative example 2, and the spandex fibers prepared in the examples 1-3 and the comparative examples 1-2 are subjected to HDT test, and the test results are shown in the following table:
TABLE 1 spandex fiber thermal performance data for examples 1-3 and comparative examples 1-2
| Sample information | Heat distortion temperature starting value (. degree. C.) | Maximum Heat distortion temperature (. degree. C.) | |
| Example 1 | 170℃/10min | 193 | 209 |
| Example 2 | 170℃/10min | 200 | 215 |
| Example 3 | 170℃/10min | 196 | 211 |
| Comparative example 1 | 170℃/10min | 190 | 204 |
| Comparative example 2 | 170℃/10min | 185 | 198 |
As can be seen from the above table, the spandex fiber prepared according to the present invention has high heat resistance and good stability, compared to conventional spandex fibers.
The foregoing is merely exemplary and illustrative of the present invention and various modifications, additions and substitutions may be made by those skilled in the art to the specific embodiments described without departing from the scope of the present invention as defined in the accompanying claims.
Claims (8)
1. The spandex with good heat resistance and stability is characterized by comprising the following raw materials in parts by weight: 50-75 parts of polytetramethylene ether glycol, 12-18 parts of isophorone diisocyanate, 1.5-3 parts of a chain extender, 0.3-1 part of a stabilizer, 0.2-1 part of a terminator, 0.5-2 parts of antimony potassium tartrate, 0.1-0.3 part of quaternary ammonium salt and 2-6 parts of a modified additive;
the modified additive comprises the following raw materials in parts by weight: 1-3 parts of flatting agent, 0.5-1 part of lubricant, 0.1-0.8 part of antioxidant and 1-3 parts of anti-ultraviolet agent.
2. The spandex with good heat resistance and stability according to claim 1, wherein: the chain extender comprises ethylenediamine and butanediamine, and the molar ratio of the ethylenediamine to the butanediamine is 3: 1-8:1.
3. The spandex with good heat resistance and stability according to claim 3, wherein: the stabilizer is vinyl pyrrolidone.
4. The spandex with good heat resistance and stability according to claim 1, wherein: the terminator is diethylamine.
5. The spandex with good heat resistance and stability according to claim 1, wherein: the quaternary ammonium salt is dodecyl dimethyl benzyl ammonium chloride.
6. The method for preparing spandex with good heat stability according to any one of claims 1 to 5, comprising the steps of:
(1) prepolymerization reaction: mixing polytetramethylene ether glycol and isophorone diisocyanate, reacting at 68-72 ℃ for 120min, then using N, N-dimethylacetamide as a solvent, fully dissolving a prepolymer, and cooling to obtain a prepolymer solution;
(2) polymerization reaction: transferring the prepolymer solution into a polymerization reactor, uniformly stirring, and performing chain extension and chain termination by controlling addition of a chain extender and a terminator at low temperature to obtain a polymer solution;
(3) adding auxiliary materials: continuously transferring polymer solution continuously generated by potassium antimony tartrate and quaternary ammonium salt in a polymerization reactor into a stirring tank, and simultaneously adding quaternary ammonium salt and a modified additive into the stirring tank to obtain a spandex spinning stock solution;
(4) spinning: and (4) preparing the spandex spinning stock solution prepared in the step (3) into spandex fibers by adopting a dry spinning method.
7. The method for preparing spandex with good heat resistance and stability according to claim 6, wherein the method comprises the following steps: in the step (2), a cooling pipe is coiled outside the polymerization reactor and used for controlling the temperature in the polymerization reactor.
8. The method for preparing spandex with good heat resistance and stability according to claim 6, wherein the method comprises the following steps: in the step (1), polytetramethylene ether glycol and isophorone diisocyanate are mixed and reacted at 70 ℃ for 120min, then N, N-dimethylacetamide is used as a solvent, the prepolymer is fully dissolved, and a prepolymer solution is obtained after cooling.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911374828.2A CN111101230A (en) | 2019-12-27 | 2019-12-27 | Spandex with good heat-resistant stability and preparation method thereof |
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| CN201911374828.2A CN111101230A (en) | 2019-12-27 | 2019-12-27 | Spandex with good heat-resistant stability and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112725929A (en) * | 2020-12-29 | 2021-04-30 | 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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| KR20140098325A (en) * | 2013-01-30 | 2014-08-08 | 주식회사 효성 | Method for preparing polyurethaneurea elastic fiber |
| CN105420843A (en) * | 2014-09-23 | 2016-03-23 | 浙江华峰氨纶股份有限公司 | Preparation method of easy-dyeing polyurethane elastic fibers |
| CN105908281A (en) * | 2016-04-28 | 2016-08-31 | 浙江开普特氨纶有限公司 | Dyeable spandex fiber preparation method |
| CN106757485A (en) * | 2016-11-23 | 2017-05-31 | 华峰重庆氨纶有限公司 | A kind of preparation method of high drawing spandex fibre |
| CN110042519A (en) * | 2019-04-24 | 2019-07-23 | 海宁源茂针织有限公司 | Spandex blend fibre |
-
2019
- 2019-12-27 CN CN201911374828.2A patent/CN111101230A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20140098325A (en) * | 2013-01-30 | 2014-08-08 | 주식회사 효성 | Method for preparing polyurethaneurea elastic fiber |
| CN105420843A (en) * | 2014-09-23 | 2016-03-23 | 浙江华峰氨纶股份有限公司 | Preparation method of easy-dyeing polyurethane elastic fibers |
| CN105908281A (en) * | 2016-04-28 | 2016-08-31 | 浙江开普特氨纶有限公司 | Dyeable spandex fiber preparation method |
| CN106757485A (en) * | 2016-11-23 | 2017-05-31 | 华峰重庆氨纶有限公司 | A kind of preparation method of high drawing spandex fibre |
| CN110042519A (en) * | 2019-04-24 | 2019-07-23 | 海宁源茂针织有限公司 | Spandex blend fibre |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112725929A (en) * | 2020-12-29 | 2021-04-30 | 宁夏宁东泰和新材有限公司 | Spinning control method for high-temperature-resistant polyurethane elastic fiber |
| 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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Application publication date: 20200505 |