CN109467741B - Method for separating and recycling waste polyester-cotton textiles through hydrothermal reaction catalyzed by organic acid - Google Patents
Method for separating and recycling waste polyester-cotton textiles through hydrothermal reaction catalyzed by organic acid Download PDFInfo
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- CN109467741B CN109467741B CN201710806970.4A CN201710806970A CN109467741B CN 109467741 B CN109467741 B CN 109467741B CN 201710806970 A CN201710806970 A CN 201710806970A CN 109467741 B CN109467741 B CN 109467741B
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/14—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with steam or water
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention provides a method for separating and recovering waste polyester-cotton textiles by a hydrothermal reaction catalyzed by organic acid, which comprises the following steps: cutting waste polyester-cotton textiles into fragments, and dispersing the fragments in an aqueous solution system of an organic acid catalyst to obtain a mixed system; heating the mixed system to 110-180 ℃ in a high-pressure reactor to enable the cotton fibers in the waste polyester-cotton textiles to undergo degradation reaction for 0.5-3h to obtain a mixture; and filtering the mixture by using a screen, cleaning to obtain a polyester fiber aggregate, performing vacuum filtration on the rest part by using a filtering membrane, and cleaning to obtain cotton fiber fragments. The method has advanced and simple process, the catalyst used in the process is from the nature and can be biodegraded, the catalyst cannot be decomposed in the process, the environment cannot be polluted, and the separation, recovery and reutilization of the waste polyester-cotton textiles can be efficiently realized.
Description
Technical Field
The invention relates to the field of textile resource regeneration, in particular to a method for separating and recovering waste polyester-cotton textiles through hydrothermal reaction catalyzed by organic acid.
Background
With the increasing world population and the rapid change of fashion trend, more and more textile waste products are generated, and polyester fiber is one of the most commonly used fibers, especially for manufacturing polyester-cotton blended fabrics and the like. However, polyester fiber is a material which is difficult to naturally degrade, and is likely to have adverse effects on the environment after being discarded. From the viewpoint of environmental protection and resource saving, recycling is one of the most ideal methods for disposing of such waste.
In order to achieve a perfect recycling effect, two different types of fibers in waste polyester-cotton textiles are firstly separated properly, and in this respect, a chemical method is more complete than a physical method and can thoroughly realize separation and recovery. The chemical method is mainly to convert one of the fibers into a soluble substance through chemical degradation or modification reaction, or directly use a corresponding solvent for selective dissolution, so as to achieve the complete separation of the fibers. Admittedly, however, the current technology has drawbacks, in either way, including the use of more harmful chemicals, such as: hydrochloric acid (US patent No.4345039) and tetramethylene sulfone (US patent No.5342854), or the like, or require the use of large amounts of expensive solvents such as: NMMO, ionic liquids (WO patent No.2014081291 a1), DMT (CN patent No.2014081291 a1), and the like, which inevitably burden cost control and environmental protection.
Disclosure of Invention
The invention aims to solve the defects of the existing polyester-cotton textile recycling technology, and separates and recycles the waste polyester-cotton textiles by taking biodegradable organic acid from the nature as a catalyst and matching with a hydrothermal reaction method, and does not cause secondary pollution to the environment.
In order to achieve the aim, the invention provides a method for separating and recovering waste polyester-cotton textiles by a hydrothermal reaction catalyzed by organic acid, which comprises the following steps:
cutting waste polyester-cotton textiles into fragments, and dispersing the fragments in an aqueous solution system of an organic acid catalyst to obtain a mixed system;
heating the mixed system to 110-180 ℃ in a high-pressure reactor to enable the cotton fibers in the waste polyester-cotton textiles to undergo degradation reaction for 0.5-3h to obtain a mixture; and
and filtering the mixture by using a screen, cleaning to obtain a polyester fiber aggregate, performing vacuum filtration on the rest part by using a filtering membrane, and cleaning to obtain cotton fiber fragments.
In one embodiment of the process of the present invention, the organic acid is methanesulfonic acid, oxalic acid, tartaric acid, citric acid, malic acid, formic acid or acetic acid, preferably methanesulfonic acid, oxalic acid, citric acid.
In another embodiment of the method of the present invention, the polyester content in the polyester-cotton textile is 1% to 99% by weight percentage.
In another embodiment of the process of the present invention, the aqueous system comprises from 0.1% to 30%, preferably from 0.5% to 10% by weight of the organic acid catalyst.
In another embodiment of the method of the present invention, the solid-to-liquid ratio of the mixed system is 1: 30-200, preferably 1: 50-150.
In another embodiment of the method of the present invention, the temperature of the mixed system is increased under stirring at a rate of 4 to 6 ℃/min.
In another embodiment of the process of the present invention, the mixed system is warmed to form an autogenous pressure, which is 0.10 to 1 MPa.
In another embodiment of the method of the present invention, the method further comprises drying the polyester fiber assembly and the cotton fiber pieces in a forced air oven to a constant weight, respectively.
In another embodiment of the method of the present invention, the method further comprises subjecting the polyester fiber assembly to a mechanical action to become a re-spinnable fiber raw material.
In another embodiment of the method of the present invention, further comprising reusing the cotton fiber pieces as a cellulosic production feedstock.
Compared with the prior art, the method for separating and recycling the waste polyester-cotton textiles through the hydrothermal reaction catalyzed by the organic acid has the advantages that the process is advanced and simple, the catalyst used in the process is from the nature and can be biodegraded, the catalyst cannot be decomposed in the process, secondary pollution to the environment cannot be caused, and the separation, recycling and reutilization of the waste polyester-cotton textiles can be efficiently realized.
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FIG. 1 is a scanning electron microscope image of waste polyester-cotton textiles before treatment;
FIG. 2 is a scanning electron microscope image of a polyester fiber assembly obtained after treatment by the method of the present invention;
FIG. 3 is a scanning electron microscope image of cotton fibers treated by the method of the present invention;
FIG. 4 is a Fourier transform Infrared Spectroscopy (FTIR) analysis comparison graph of polyester fibers before and after treatment;
FIG. 5 is a Differential Scanning Calorimetry (DSC) analysis comparison of polyester fibers before and after treatment.
Detailed Description
The technical solution of the present invention is further explained below according to specific embodiments. The scope of protection of the invention is not limited to the following examples, which are set forth for illustrative purposes only and are not intended to limit the invention in any way.
The method for separating and recovering the waste polyester-cotton textiles is realized by using hydrothermal reaction catalyzed by organic acid, and mainly comprises the following steps:
cutting waste polyester-cotton textiles into fragments, and dispersing the fragments in an aqueous solution system of an organic acid catalyst to obtain a mixed system;
heating the mixed system to 110-180 ℃ in a high-pressure reactor to enable the cotton fibers in the waste polyester-cotton textiles to undergo degradation reaction for 0.5-3h to obtain a mixture; and
filtering the mixture by a screen, cleaning to obtain a polyester fiber aggregate, performing vacuum filtration on the rest part by a filter membrane, and cleaning to obtain cotton fiber fragments.
Fig. 1 is a scanning electron microscope image of waste polyester-cotton textiles before treatment, as shown in fig. 1, in the method for separating and recovering waste polyester-cotton textiles of the present invention, the polyester-cotton textiles are fabrics woven by yarns blended from polyester and cotton fibers, the waste polyester-cotton textiles may be waste polyester-cotton textiles containing polyester content in any proportion, and the polyester content of the waste polyester-cotton textiles treated by the present invention is preferably 1% to 99% in terms of weight percentage, that is, the method is suitable for most of the polyester-cotton textiles.
The waste polyester cotton textile can be cut into pieces by cutting or shredding, and the size of the cut pieces is determined according to specific production conditions.
The organic acid mentioned in the invention refers to natural acid which comes from nature and can be biologically degraded, and can not be decomposed in the process of separating and recovering the waste polyester-cotton textile, and can not cause secondary pollution to the environment, such as methanesulfonic acid, oxalic acid, tartaric acid, citric acid, malic acid, formic acid, acetic acid, etc., preferably methanesulfonic acid, oxalic acid, citric acid.
The aqueous solution system of the organic acid catalyst is an aqueous solution formed by mixing organic acid (as a catalyst for subsequent degradation reaction) and water, wherein the content of the organic acid as the catalyst is 0.1-30% by weight, preferably 0.5-10% by weight, the content of the organic acid can accelerate the degradation reaction, so that the required reaction time is shortened, and in addition, the high content also can be beneficial to decomposing thicker clothes or clothes with tighter structure.
Dispersing waste polyester-cotton textile fragments in an aqueous solution system of an organic acid catalyst to obtain a mixed system with coexisting solid and liquid, wherein the solid-liquid ratio of the mixed system is 1: 30-200, preferably 1: 50-150, and the solid-to-liquid ratio is small, the reaction is relatively fast, and vice versa.
In order to degrade the cotton fibers in the waste polyester-cotton textiles, the mixed system is put into a closed high-pressure reactor, the temperature is increased to 110-180 ℃ at the temperature increase rate of 4-6 ℃/min under the stirring condition and is maintained for 0.5-3h, and the generated autogenous pressure (namely the pressure difference between the inside and the outside of the high-pressure reactor) is 0.10-1 MPa.
Under the subcritical hydrothermal condition, the cotton fibers can be subjected to degradation reaction, the polyester fibers are not affected, and the degraded cotton fibers are stripped from the textile in the form of fragments, so that the cotton fibers and the polyester fibers are separated. High temperatures or longer reaction times result in smaller sized cotton fiber pieces.
After cotton fiber and polyester fiber separate, retrieve polyester fiber and cotton fiber respectively through filterable mode, concrete step includes: filtering the mixture with a screen (such as a 20-mesh screen), cleaning to obtain a polyester fiber aggregate, vacuum-filtering the rest (the residual mixture after filtration) with a filtering membrane (such as PTFE (polytetrafluoroethylene) membrane), and cleaning to obtain cotton fiber fragments.
After the polyester fiber aggregate and the cotton fiber fragments are obtained, the polyester fiber aggregate and the cotton fiber fragments can be respectively dried in a blast oven to constant weight, and then the polyester fiber aggregate and the cotton fiber fragments are weighed to calculate the yield.
As shown in fig. 2-5, the product recovered by the method of the present invention, after being analyzed by Scanning Electron Microscope (SEM), fourier transform infrared spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), and recovery yield, is found to have a recovery rate of the polyester fiber aggregate of more than 95%, and not containing cellulose, the chemical properties thereof are basically preserved, and the polyester fiber aggregate can become a fiber raw material capable of being re-spun through mechanical opening and carding action (such as an opener, a carding machine, and the like), so as to realize the recycling of the polyester fiber; the recovery rate of the cotton fiber fragments is more than 80%, and the cotton fiber fragments do not contain polyester fibers, and can be reused as cellulose production raw materials, such as paper making raw materials entering a pulp mill.
In addition, the method does not involve the use of harmful chemical substances and a large amount of expensive solvents, but uses water as a reaction medium, and has extremely small catalyst dosage, thereby being beneficial to reducing the fiber recovery cost, improving the production efficiency and realizing the recovery and reutilization of the real green and environment-friendly polyester-cotton textiles.
Unless otherwise defined, all terms used herein have the meanings that are commonly understood by those skilled in the art.
The present invention will be further described with reference to the following examples.
Examples
The chemical reagents used in the following examples are commercially available and analytically pure reagents unless otherwise specified, and the procedures and instruments used in the following examples are those commonly used in the art unless otherwise specified. The proportions, ratios, contents, and the like described in the following examples are by weight unless otherwise specified.
Example 1
Putting 15g of waste white shirts with the ratio of polyester to cotton of 65/35 into 1.8L of aqueous solution with the citric acid content of 5%, heating the high-pressure reaction kettle to 130 ℃ at the heating rate of 5 ℃/min under the condition of stirring, and maintaining for 1.5h, so as to carry out degradation reaction on cotton fibers.
After the reaction is finished, the electric heater is closed, after the reaction kettle is cooled to room temperature, the reaction kettle is opened, and a reaction product is taken out.
Filtering the reaction product by a screen to obtain a polyester fiber aggregate, performing vacuum filtration on the residual mixed solution by a filter membrane to obtain cotton fiber fragments, cleaning the polyester fiber aggregate and the cotton fiber fragments, and drying the polyester fiber aggregate and the cotton fiber fragments in a blast oven to constant weight, wherein the recovery rate of the obtained polyester fiber aggregate is 98% and the recovery rate of the cotton fiber fragments is 83%.
Example 2
Placing 17g of waste bed sheet with the ratio of polyester to cotton of 20/80 in 1.5L of aqueous solution with the content of methanesulfonic acid of 1%, heating the high-pressure reaction kettle to 140 ℃ at the heating rate of 6 ℃/min and maintaining for 1h, and carrying out degradation reaction on cotton fibers.
After the reaction is finished, the electric heater is closed, after the reaction kettle is cooled to room temperature, the reaction kettle is opened, and a reaction product is taken out.
Filtering the reaction product by a screen to obtain a polyester fiber aggregate, performing vacuum filtration on the residual mixed solution by a filter membrane to obtain cotton fiber fragments, respectively cleaning the polyester fiber aggregate and the cotton fiber fragments, and drying the cotton fiber aggregate and the cotton fiber fragments in a blast oven to constant weight, wherein the recovery rate of the obtained polyester fiber aggregate is 99 percent, and the recovery rate of the cotton fiber fragments is 81 percent.
In conclusion, the method for separating and recycling the waste polyester-cotton textiles through the hydrothermal reaction catalyzed by the organic acid has the advantages that the process is advanced and simple, the catalyst used in the process is from the nature and can be biodegraded, the catalyst cannot be decomposed in the process, the environment cannot be polluted, and the separation, the recycling and the reutilization of the waste polyester-cotton textiles can be efficiently realized.
The embodiments described above are presented to enable those skilled in the art to make and use the invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (9)
1. A method for separating and recovering waste polyester-cotton textiles through hydrothermal reaction catalyzed by organic acid is characterized by comprising the following steps:
cutting waste polyester-cotton textiles into fragments, and dispersing the fragments in an aqueous solution system of an organic acid catalyst to obtain a mixed system;
heating the mixed system to 110-180 ℃ in a high-pressure reactor to enable the cotton fibers in the waste polyester-cotton textiles to undergo degradation reaction for 0.5-3h to obtain a mixture; and
filtering the mixture by a screen, cleaning to obtain a polyester fiber aggregate, performing vacuum filtration on the rest part by a filter membrane, cleaning to obtain cotton fiber fragments,
the method is characterized in that the content of the organic acid catalyst in the aqueous solution system is 0.1-30% by weight.
2. The method of claim 1, wherein the organic acid is methanesulfonic acid, oxalic acid, tartaric acid, citric acid, malic acid, formic acid, or acetic acid.
3. The method according to claim 1, wherein the polyester content of the polyester-cotton textile is 1-99% by weight.
4. The method according to claim 1, wherein the solid-to-liquid ratio of the mixed system is 1: 30-200.
5. The method according to claim 1, wherein the temperature of the mixed system is increased at a rate of 4-6 ℃/min under stirring.
6. The method according to claim 5, wherein the autogenous pressure is formed after the temperature of the mixed system is increased, and the autogenous pressure is 0.10-1 MPa.
7. The method of claim 1, further comprising drying the polyester fiber assemblies and the cotton fiber pieces, respectively, in a forced air oven to a constant weight.
8. The method of claim 1, further comprising subjecting the assembly of polyester fibers to a mechanical action to form a re-spinnable fiber stock.
9. The method of claim 1, further comprising reusing the cotton fiber pieces as a cellulosic production feedstock.
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| CN108456135B (en) * | 2018-01-17 | 2021-02-02 | 太原理工大学 | Method for recycling colored waste polyester-cotton fibers |
| CN110280204A (en) * | 2019-07-02 | 2019-09-27 | 任永飞 | A kind of useless chemical fibre textile degeneration system |
| CN113651312B (en) * | 2021-08-30 | 2023-01-17 | 新疆大学 | Carbon quantum dot gas-sensitive sensing material and preparation method and application thereof |
| TWI788006B (en) * | 2021-09-11 | 2022-12-21 | 南亞塑膠工業股份有限公司 | Recycling method of polyester cotton blended fabric |
| CN113862839B (en) * | 2021-09-13 | 2023-04-21 | 福建赛隆科技有限公司 | Waste polyester-cotton blended fabric separation and recovery device and recovery process and application thereof |
| DE102022000572A1 (en) * | 2022-02-15 | 2023-08-17 | EEDEN GerMan UG (haftungsbeschränkt) | Manufacture of pulp from cotton blend |
| WO2024119223A1 (en) * | 2022-12-05 | 2024-06-13 | BlockTexx Labs Pty Ltd | An improved system and mechanical processes for the separation and recycling of blended polyster and cotton textiles for re-use |
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| US3937671A (en) * | 1974-11-18 | 1976-02-10 | Textile Research Institute | Method of recovering constituents from polyester and cellulosic textile waste |
| CN106674588A (en) * | 2017-01-05 | 2017-05-17 | 太原理工大学 | Method for separating and recovering waste cotton-polyester blended fabric under subcritical water condition |
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|---|---|---|---|---|
| US3937671A (en) * | 1974-11-18 | 1976-02-10 | Textile Research Institute | Method of recovering constituents from polyester and cellulosic textile waste |
| CN106674588A (en) * | 2017-01-05 | 2017-05-17 | 太原理工大学 | Method for separating and recovering waste cotton-polyester blended fabric under subcritical water condition |
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| Title |
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| 废旧纺织品的回收再利用;陈加敏等;《纺织科技进展》;20160930 * |
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