CN102250379A - Method for separation of terylene-cotton blended fabrics and repolymerization of terylene - Google Patents
Method for separation of terylene-cotton blended fabrics and repolymerization of terylene Download PDFInfo
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- CN102250379A CN102250379A CN2011101456959A CN201110145695A CN102250379A CN 102250379 A CN102250379 A CN 102250379A CN 2011101456959 A CN2011101456959 A CN 2011101456959A CN 201110145695 A CN201110145695 A CN 201110145695A CN 102250379 A CN102250379 A CN 102250379A
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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Abstract
The invention discloses a separation method of (waste) terylene-cotton blended fabrics. The terylene-cotton blended fabrics are composed of polyethylene terephthalate and cotton fibers. The method comprises the following steps: carrying out an alcoholysis reaction on the terylene-cotton blended fabrics, ethylene glycol and an alcoholysis catalyst to obtain a reaction mixture, wherein the alcoholysis catalyst is zinc acetate; carrying out solid-liquid separation on the reaction mixture to obtain a solid matter and a liquid matter, wherein the solid matter is the cotton fibers; and carrying out a pre-polycondensation reaction and a final polycondensation reaction on the liquid matter in the presence of a polycondensation catalyst to obtain polyethylene terephthalate. By using the separation method disclosed by the invention, the (waste) terylene-cotton blended fabrics with various blending ratios are successfully separated to obtain the terylene and cotton fibers.
Description
Technical field
The present invention relates to the separation and the terylene repolymerization method of a kind of (waste and old) polyester cotton.
Background technology
China is a weaving big country, and the raw-material demand of annual textiles reaches more than 3,500 ten thousand tons, because shortage of resources need a large amount of textiless of import and starting material thereof every year, but the utilization ratio of China's reclaimed materials is but extremely low.It is estimated that more than 2,000 ten thousand tons of the quantity of annual waste textile, the overwhelming majority are failed effective recycling, cause the waste textile enormous amount nearly, not only contaminate environment, occupy a large amount of storage spaces, and cause the great wasting of resources.
Waste textile is divided according to fibre fractionation, can be divided into single-component fabric and BLENDED FABRIC.At present, the recoverying and utilizing method of single-component textiles has: the one, and the utilization again of textile textiles is promptly by physical methods such as opener technologies, the textile textiles shredding of will giving up becomes staple fibre, the utilization of spinning again, but because fiber is shorter, can only be used for low value-added product; The 2nd, pure terylene textiles is recycled, and 2 kinds of approach are arranged: a kind of is physical method, by granule, respin and make polyester staple fiber, but brute force is lower, can not be used for conventional textiles.A kind of is chemical process, by various chemical processes such as hydrolysis method, alcoholysis method, supercutical fluid methods, polyester is degraded into monomer or half ester, is used as chemical raw material or coating, tackiness agent etc.
But, account for the polyester cotton blending textiles of waste textile ratio maximum, because recovery difficult is very big, domestic for a long time never enterprise carries out this type of work, at present unique application can only be as weighting material etc.
It is reported that u s company once adopted naphthalene to make solvent, the terylene in the polyester cotton is dissolved, again the terylene chemical degradation is realized utilizing after the separation.This method flow is long, and complex process can produce atmospheric pollution after the solvent evaporates.United States Patent (USP) CN98804291.6 has invented a kind of " reclaiming the method for polyester from the polyester waste that pollutes ", by fused dimethyl terephthalate (DMT) (DMT) equal solvent and useless polyester are mixed and heated to 256 ℃, realize the dissolving of useless polyester, solid impurity material (as cotton fibre, metal oxide, binding agent etc.) with wherein goes out polyester components by crystallisation by cooling then.This method is applicable to the polyester waste that amount of polyester is very high, because solid impurity such as cotton fibre can not utilize again, impurity can't filter totally simultaneously, long flow path, and the cost height is unfavorable for higher value application.Chinese patent CN88100610.6 has invented a kind of " the recovery processing method of waste polyester sort materials ", adopts the mixture of a condensed ethandiol and ethylene glycol to make depolymerizing agent, and degraded polyester, cotton fibre separate the back as papermaking, and the polyester after the degraded is used as coating etc.This method has been used a condensed ethandiol, and the polyester after the depolymerization can't become the linear polyester section that can be used for spinning of certain molecular weight in polycondensation, and the cotton fibre degradation is mainly used in papermaking, and the added value of product after the recovery is lower.
Summary of the invention
The purpose of this invention is to provide the separation of a kind of (waste and old) polyester cotton and the method for terylene repolymerization.
The separation method of (waste and old) provided by the invention polyester cotton, described polyester cotton is made up of polyethylene terephthalate and cotton fibre; Comprise the steps: that described polyester cotton, ethylene glycol and alcoholysis catalysts carry out alcoholysis reaction and obtain reaction mixture, described alcoholysis catalysts is a zinc acetate; Described reaction mixture obtains solid matter and liquid substance through solid-liquid separation, and described solid matter is described cotton fibre; Described liquid substance promptly gets described polyethylene terephthalate through prepolymerization reaction and the poly-reaction of final minification under the condition that polycondensation catalyst exists.
In the above-mentioned separation method, described polyester cotton can be chopped into surface-area is 4cm
2-25cm
2Sheet after carry out described alcoholysis reaction again, be easy to the carrying out of described alcoholysis reaction.
In the above-mentioned separation method, the ratio of quality and the number of copies of the mixture of described polyester cotton and described ethylene glycol and alcoholysis catalysts can be 1: (4-7), specifically can be 1: 4 or 1: 6; The ratio of quality and the number of copies of described ethylene glycol and alcoholysis catalysts can be 1: 0.001.
In the above-mentioned separation method, the temperature of described alcoholysis reaction can be 195 ℃-200 ℃, specifically can be 196 ℃ or 200 ℃; The time of described alcoholysis reaction can be 1.2 hours-2.0 hours, specifically can be 1.5 hours.
In the above-mentioned separation method, the temperature of described solid-liquid separation can be 150 ℃-196 ℃, specifically can be 150 ℃ or 196 ℃, can take filtering mode to separate.
In the above-mentioned separation method, described method also comprises the step that described solid matter spent glycol successively and water are washed, and when spent glycol washed, the temperature of may command washing was 150 ℃.
In the above-mentioned separation method, described polycondensation catalyst can be antimony glycol.
In the above-mentioned separation method, the ratio of quality and the number of copies of described polycondensation catalyst and described liquid substance can be 0.001: 1.
In the above-mentioned separation method, the temperature of described prepolymerization reaction can be 265 ℃-275 ℃; The time of described prepolymerization reaction can be 0.5 hour; The vacuum tightness of described prepolymerization reaction is 0.9kPa; The stirring velocity of described prepolymerization reaction is 6r/min.
In the above-mentioned separation method, the temperature of the poly-reaction of described final minification can be 285 ℃; The time of the poly-reaction of described final minification is 0.5 hour-3 hours, specifically can be 0.5 hour or 3 hours; The vacuum tightness of the poly-reaction of described final minification is 10Pa-40Pa, specifically can be 10Pa or 40Pa.
The present invention is a purpose with waste and old polyester cotton higher value application, adopt the depolymerizing agent the do not influence polycondensation of polyester terylene of degrading, by the airtight filtration of high temperature, with cotton fibre secondary filtration and washing, the cotton fibre that formation can be used for weaving, the polyester after the degraded form the regenerated terylene section that limiting viscosity reaches 0.65dL/g-0.70dL/g by precondensation and polycondensation, can be used for spinning, two kinds of components have all realized higher value application.
Embodiment
Employed experimental technique is ordinary method if no special instructions among the following embodiment.
Used material, reagent etc. if no special instructions, all can obtain from commercial channels among the following embodiment.
Among the following embodiment, the measuring method of breaking tenacity and elongation at break is GB/T 13783-1992.
The separation of embodiment 1, polyester cotton
To clean exsiccant polyester cotton blending ratio and be 4: the 1 waste and old polyester cotton of (being polyethylene terephthalate (PET) and the ratio of quality and the number of copies of cotton fibre) is chopped into area and is approximately 4cm
2Fragment, get 200Kg.Is to be made into ethylene glycol mixture at 1: 0.001 with ethylene glycol and catalyst acetic acid zinc according to ratio of quality and the number of copies, is to join at 1: 6 to carry out alcoholysis reaction in the high-temperature reactor that has whipping appts and obtain reaction mixture with waste and old polyester cotton and ethylene glycol mixture according to ratio of quality and the number of copies, the alcoholysis reaction temperature is 196 ℃, and the time is 1.5h; This reaction mixture is filtered 150 ℃ the time, obtain solid matter and liquid substance, solid matter through 150 ℃ of ethylene glycol washings, after the water washing drying, obtains purified cotton fibre earlier again; Is that 1: 0.001 ratio joins and carries out polycondensation in the batch condensation polymerization reactor with liquid substance and catalyst glycol antimony according to ratio of quality and the number of copies: the precondensation pumpdown time is 0.5h, and stirring velocity is 6r/min, and temperature is 265 ℃, and vacuum tightness is 0.9kPa; The poly-pumpdown time of final minification is 0.5h, and stirring velocity is 4.5r/min, and temperature remains 285 ℃, and vacuum tightness should remain on 10Pa; Obtain reproducing polyethylene terephthalate (PET) through precondensation and final minification are poly-.
In the above-mentioned experiment, recording the terylene percent alcoholysis is 98.8%.The limiting viscosity of the PET that polycondensation obtains satisfies the imitative silk of chemical fibre needs between 0.60-0.62dL/g.Carry out ultimate fibre tension test test to separating the back cotton fibre, obtain the breaking tenacity 2.19cN/dtex (primary cotton fibre is 1.8-3.1cN/dtex) of cotton fibre, the requirement that elongation at break 7.91% (primary cotton fibre is 7.0-12.0%) all meets primary cotton fibre.
The separation of embodiment 2, polyester cotton
The waste and old polyester cotton that will clean exsiccant polyester cotton blending ratio and be 1: 1 (being the ratio of quality and the number of copies of PET and cotton fibre) is chopped into area and is approximately 25cm
2Fragment, get 200Kg.Is to be made into ethylene glycol mixture at 1: 0.001 with ethylene glycol and catalyst acetic acid zinc according to ratio of quality and the number of copies, is to join at 1: 4 to carry out alcoholysis reaction in the high-temperature reactor that has whipping appts and obtain reaction mixture with waste and old polyester cotton and ethylene glycol mixture according to ratio of quality and the number of copies, the alcoholysis reaction temperature is 200 ℃, and the time is 1.5h; This reaction mixture is filtered 196 ℃ the time, obtain solid matter and liquid substance; Solid matter through 150 ℃ of ethylene glycol washings, after the water washing drying, obtains purified cotton fibre earlier again; Is that 1: 0.001 ratio joins and carries out polycondensation in the batch condensation polymerization reactor with liquid substance and catalyst glycol antimony according to ratio of quality and the number of copies: the precondensation pumpdown time is 0.5h, and stirring velocity is 6r/min, and temperature is 275 ℃, and vacuum tightness is 0.9kPa; The poly-pumpdown time of final minification is 3h, and stirring velocity is 4.5r/min, and temperature remains 285 ℃, and vacuum tightness should remain on 40Pa; Obtain reproducing polyethylene terephthalate (PET) through precondensation and final minification are poly-.
In the above-mentioned experiment, recording the terylene percent alcoholysis is 94.6%, and the limiting viscosity of the PET that polycondensation obtains satisfies spinning requirement between 0.65-0.69dL/g.Carry out ultimate fibre tension test test to separating the back cotton fibre, obtain the breaking tenacity 2.0cN/dtex (primary cotton fibre is 1.8-3.1cN/dtex) of cotton fibre, the requirement that elongation at break 7% (primary cotton fibre is 7.0-12.0%) all meets primary cotton fibre.As seen, the cotton fibre after the separation and reproduce after PET all meet and utilize requirement again.
Claims (9)
1. the separation method of a polyester cotton, described polyester cotton is made up of polyethylene terephthalate and cotton fibre; Comprise the steps: that described polyester cotton, ethylene glycol and alcoholysis catalysts carry out alcoholysis reaction and obtain reaction mixture, described alcoholysis catalysts is a zinc acetate; Described reaction mixture obtains solid matter and fluent meterial through solid-liquid separation, and described solid matter is described cotton fibre; Described fluent meterial promptly gets described polyethylene terephthalate through prepolymerization reaction and the poly-reaction of final minification under the condition that polycondensation catalyst exists.
2. method according to claim 1 is characterized in that: the ratio of quality and the number of copies of the mixture of described polyester cotton and described ethylene glycol and alcoholysis catalysts is 1: (5-7); The ratio of quality and the number of copies of described ethylene glycol and alcoholysis catalysts is 1: 0.001.
3. method according to claim 1 and 2 is characterized in that: the temperature of described alcoholysis reaction is 195 ℃-200 ℃; The time of described alcoholysis reaction is 1.2 hours-2.0 hours.
4. according to arbitrary described method among the claim 1-3, it is characterized in that: the temperature of described solid-liquid separation is 150 ℃-196 ℃.
5. according to arbitrary described method among the claim 1-4, it is characterized in that: described method also comprises the step that described solid matter spent glycol successively and water are washed.
6. according to arbitrary described method among the claim 1-5, it is characterized in that: described polycondensation catalyst is an antimony glycol.
7. according to arbitrary described method among the claim 1-6, it is characterized in that: the ratio of quality and the number of copies of described polycondensation catalyst and described liquid substance is 0.001: 1.
8. according to arbitrary described method among the claim 1-7, it is characterized in that: the temperature of described prepolymerization reaction is 265 ℃-275 ℃; The time of described prepolymerization reaction is 0.5 hour; The vacuum tightness of described prepolymerization reaction is 0.9kPa.
9. according to arbitrary described method among the claim 1-8, it is characterized in that: the temperature of the poly-reaction of described final minification is 285 ℃; The time of the poly-reaction of described final minification is 0.5 hour-3 hours; The vacuum tightness of the poly-reaction of described final minification is 10Pa-40Pa.
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| CN2011101456959A CN102250379B (en) | 2011-06-01 | 2011-06-01 | Method for separation of terylene-cotton blended fabrics and repolymerization of terylene |
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| CN2011101456959A CN102250379B (en) | 2011-06-01 | 2011-06-01 | Method for separation of terylene-cotton blended fabrics and repolymerization of terylene |
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Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936765A (en) * | 2012-11-09 | 2013-02-20 | 绍兴文理学院元培学院 | Method for separating blend fibers from worn out clothes |
| CN103665426A (en) * | 2013-11-27 | 2014-03-26 | 青岛福创环境科技有限公司 | Method for recycling cotton fibers from waste clothes |
| CN104060473A (en) * | 2014-07-04 | 2014-09-24 | 临沂市清宇环境资源综合利用研究院 | Enzyme solution and technology for processing waste polyester/cotton fabric |
| CN104327255A (en) * | 2014-11-06 | 2015-02-04 | 上海聚友化工有限公司 | Device and process for continuously separating and recycling waste polyester cotton textiles |
| CN105334280A (en) * | 2015-10-16 | 2016-02-17 | 上海纺织集团检测标准有限公司 | Method used for qualitative and quantitative identification of PET, PTT, and PBT fiber, and compounds of PET, PTT, and PBT |
| CN106459471A (en) * | 2014-05-16 | 2017-02-22 | 卡比欧斯公司 | Process of recycling mixed PET plastic articles |
| CN106519293A (en) * | 2016-12-26 | 2017-03-22 | 深圳市恒锋环境资源控股有限公司 | Waste polyester-cotton textile degrading and recycling process and system |
| CN107245161A (en) * | 2017-06-05 | 2017-10-13 | 东华大学 | A kind of method of the mechanically decoupled waste and old polyester cotton of sulfuric acid |
| WO2019047177A1 (en) * | 2017-09-08 | 2019-03-14 | 香港纺织及成衣研发中心 | Method for recycling waste polyester blended fabric containing natural fiber |
| CN109912835A (en) * | 2019-03-06 | 2019-06-21 | 中国科学院过程工程研究所 | A kind of method of polyester cotton preparation cellulose aerogels |
| US10508269B2 (en) | 2015-03-13 | 2019-12-17 | Carbios | Polypeptide having a polyester degrading activity and uses thereof |
| US10717996B2 (en) | 2015-12-21 | 2020-07-21 | Carbios | Recombinant yeast cells producing polylactic acid and uses thereof |
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| JP2021511445A (en) * | 2018-01-15 | 2021-05-06 | レンツィング アクツィエンゲゼルシャフト | How to Reuse Blended Textiles Containing Cellulose and Synthetic Plastics |
| JP2021511447A (en) * | 2018-01-15 | 2021-05-06 | レンツィング アクツィエンゲゼルシャフト | Reuse of insoluble particles from starting materials containing cellulose |
| JP2021511448A (en) * | 2018-01-15 | 2021-05-06 | レンツィング アクツィエンゲゼルシャフト | Mold containing elastane incorporated in cellulose and manufacturing method |
| CN113119349A (en) * | 2019-12-31 | 2021-07-16 | 中国科学院化学研究所 | Method for separating cotton and micro-plastic in waste textile and laundry wastewater and application |
| CN114479175A (en) * | 2017-02-20 | 2022-05-13 | 宜家供应股份公司 | Polyester textile waste recycling |
| WO2022118148A1 (en) | 2020-12-02 | 2022-06-09 | International Business Machines Corporation | Recycling process for recovery of cotton from polyester-cotton fabrics and/or fibers |
| CN114736427A (en) * | 2022-03-22 | 2022-07-12 | 广东省科学院资源利用与稀土开发研究所 | Method for controllable alcoholysis of polyester blended fiber solid waste and full utilization of product thereof |
| WO2023155367A1 (en) * | 2022-02-18 | 2023-08-24 | 青岛阿脒诺材料技术有限公司 | Method for recycling blended fabric containing polyester |
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| CN102936765B (en) * | 2012-11-09 | 2015-10-21 | 绍兴文理学院元培学院 | Blend fibre separation method in a kind of waste and old clothes |
| CN102936765A (en) * | 2012-11-09 | 2013-02-20 | 绍兴文理学院元培学院 | Method for separating blend fibers from worn out clothes |
| CN103665426A (en) * | 2013-11-27 | 2014-03-26 | 青岛福创环境科技有限公司 | Method for recycling cotton fibers from waste clothes |
| CN106459471A (en) * | 2014-05-16 | 2017-02-22 | 卡比欧斯公司 | Process of recycling mixed PET plastic articles |
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| CN107245161A (en) * | 2017-06-05 | 2017-10-13 | 东华大学 | A kind of method of the mechanically decoupled waste and old polyester cotton of sulfuric acid |
| WO2019047177A1 (en) * | 2017-09-08 | 2019-03-14 | 香港纺织及成衣研发中心 | Method for recycling waste polyester blended fabric containing natural fiber |
| JP2021511447A (en) * | 2018-01-15 | 2021-05-06 | レンツィング アクツィエンゲゼルシャフト | Reuse of insoluble particles from starting materials containing cellulose |
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| CN109912835A (en) * | 2019-03-06 | 2019-06-21 | 中国科学院过程工程研究所 | A kind of method of polyester cotton preparation cellulose aerogels |
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| WO2022118148A1 (en) | 2020-12-02 | 2022-06-09 | International Business Machines Corporation | Recycling process for recovery of cotton from polyester-cotton fabrics and/or fibers |
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| CN114736427A (en) * | 2022-03-22 | 2022-07-12 | 广东省科学院资源利用与稀土开发研究所 | Method for controllable alcoholysis of polyester blended fiber solid waste and full utilization of product thereof |
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