CN111621059A - Separation and recovery method of polyimide and blended textile thereof - Google Patents
Separation and recovery method of polyimide and blended textile thereof Download PDFInfo
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- CN111621059A CN111621059A CN202010456064.8A CN202010456064A CN111621059A CN 111621059 A CN111621059 A CN 111621059A CN 202010456064 A CN202010456064 A CN 202010456064A CN 111621059 A CN111621059 A CN 111621059A
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 147
- 239000004642 Polyimide Substances 0.000 title claims abstract description 145
- 239000004753 textile Substances 0.000 title claims abstract description 92
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000011084 recovery Methods 0.000 title claims abstract description 15
- 238000000926 separation method Methods 0.000 title claims abstract description 14
- 239000000835 fiber Substances 0.000 claims abstract description 64
- 239000000463 material Substances 0.000 claims abstract description 42
- 239000002253 acid Substances 0.000 claims abstract description 32
- 239000000243 solution Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 22
- 239000012670 alkaline solution Substances 0.000 claims abstract description 16
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 10
- 238000002791 soaking Methods 0.000 claims abstract description 10
- 239000002699 waste material Substances 0.000 claims description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000007864 aqueous solution Substances 0.000 claims description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- 239000003929 acidic solution Substances 0.000 claims description 11
- 239000003513 alkali Substances 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 239000004677 Nylon Substances 0.000 claims description 6
- 229920001778 nylon Polymers 0.000 claims description 6
- 244000025254 Cannabis sativa Species 0.000 claims description 5
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims description 5
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims description 5
- 229920000742 Cotton Polymers 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229920000297 Rayon Polymers 0.000 claims description 5
- 235000009120 camo Nutrition 0.000 claims description 5
- 235000005607 chanvre indien Nutrition 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000011487 hemp Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 239000002585 base Substances 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims description 3
- 239000004746 geotextile Substances 0.000 claims description 3
- 239000004745 nonwoven fabric Substances 0.000 claims description 3
- 239000002759 woven fabric Substances 0.000 claims description 3
- 239000011260 aqueous acid Substances 0.000 claims description 2
- 239000000975 dye Substances 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- 239000002994 raw material Substances 0.000 description 7
- 239000012752 auxiliary agent Substances 0.000 description 6
- 238000004043 dyeing Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000003472 neutralizing effect Effects 0.000 description 5
- 230000001681 protective effect Effects 0.000 description 4
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 3
- 239000003063 flame retardant Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- 208000035985 Body Odor Diseases 0.000 description 1
- 229920003369 Kevlar® 49 Polymers 0.000 description 1
- 206010040904 Skin odour abnormal Diseases 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 230000003471 anti-radiation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012775 heat-sealing material Substances 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 125000005462 imide group Chemical group 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 1
- 235000019801 trisodium phosphate Nutrition 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08J11/16—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 inorganic material
-
- 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
- D01F13/00—Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like
- D01F13/04—Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like of synthetic polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
-
- 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
Abstract
The application discloses a separation and recovery method of polyimide and blended textiles thereof, which comprises the following steps: soaking polyimide and blended textiles thereof in an acid solution for treatment for 30-60 min at 90-200 ℃ to dissolve fibers with weak acid resistance to obtain an undissolved first pretreatment material; washing the first pretreatment material with water, soaking the washed first pretreatment material in an alkaline solution for acid-base neutralization treatment, wherein the treatment time is 30-40 min, and the treatment temperature is 60-90 ℃, so as to obtain an insoluble second pretreatment material; and washing the second pretreatment material with water, and obtaining the polyimide fiber with higher purity after the second pretreatment material is washed with water. The method can separate and recover the polyimide and the blended textile thereof to obtain the polyimide fiber with higher purity, and is cheap, simple, environment-friendly and efficient.
Description
Technical Field
The application relates to the technical field of environmental protection recovery, in particular to a separation and recovery method of polyimide and blended textiles thereof.
Background
Polyimide fibers are a polymeric material containing imide rings in the main molecular chain. Because of having a highly conjugated main chain structure, the fiber has high-strength and high-modulus mechanical properties, excellent performance, thermal oxidation resistance stability, for example, the limit oxygen index is higher than that of Kevlar 49 sold in the market, excellent flame retardance, no molten drop when being baked by open fire, and self-extinguishing when being away from fire; excellent heat insulation performance, and the heat conductivity coefficient is only one dozen times of that of terylene and nylon; excellent low temperature resistance, and can not be brittle in liquid ammonia with the temperature lower than-260 ℃; the capability of resisting ultraviolet rays and radiation is strong; good spinnability and strong spinnability.
Polyimide fibers are versatile: high temperature resistant flame retardant protective clothing, parachutes, honeycomb structures and heat sealing materials, composite reinforcing agents and anti-radiation materials; manufacturing fireproof flame-retardant clothes such as protective clothes of armored troops, racing car flame-retardant clothes, flight clothes and the like; comfortable and warm functional clothes such as military clothes, casual clothes for eliminating bad body odor, special clothes for preventing biochemical weapons, medical sanitary protective clothes, high-efficiency smoke protective masks and the like are manufactured.
Polyimide fibers have such many advantages, and are highly spinnable, so that they are used in the field of civil use from a special field. As civil textiles, the polyimide can be knitted or woven, pure polyimide can be used for manufacturing textiles, and the polyimide can also be blended with other fibers; polyimide is used as civil textiles, and various colors and various functional finishes need to be dyed, so that the consumption of the polyimide textiles is very large, and how to recycle the waste polyimide textiles becomes a problem to be solved urgently. CN1026414C discloses a method for recovering polyimide film waste, CN1324789 discloses a method for recovering polyimide by using an alkali aqueous solution and sulfuric acid, CN109503614 discloses a method for recovering polyimide by using hydrazine hydrate, and CN104945268A discloses a method for recovering and processing modified polyimide film waste.
However, the existing waste polyimide textiles are usually not pure polyimide fibers, but are often blended with other fibers, or dyes and other functional auxiliaries exist on the polyimide fibers, and when the polyimide textiles are recycled in the prior art, the purity is not high, so that the subsequent industrial recycling application is influenced.
Disclosure of Invention
The technical problem mainly solved by the application is to provide a method for separating and recovering polyimide and blended textiles thereof, which can separate and recover polyimide waste textiles containing cotton, hemp, viscose, nylon and other strong acid-intolerant blended materials or polyimide waste textiles containing dyes and auxiliaries, and is low in price, simple, environment-friendly and efficient.
In order to solve the technical problem, the application adopts a technical scheme that: the separation and recovery method of the polyimide and the blended textile thereof comprises the following steps:
the waste polyimide textile is soaked in an acid solution for treatment, and the characteristics that polyimide fibers resist strong acid, and the remaining materials such as blended cotton, hemp, viscose, nylon, dye, auxiliaries and the like do not resist strong acid and are easy to decompose are utilized for preliminary separation. The treatment time is 30-60 min, the treatment temperature is 90-200 ℃, and the fibers with weak acid resistance are dissolved to obtain an undissolved first pretreatment material;
washing the first pretreatment material with water, soaking the washed first pretreatment material in an alkaline solution for acid-base neutralization treatment, wherein the treatment time is 30-40 min, and the treatment temperature is 60-90 ℃, so as to obtain an insoluble second pretreatment material;
and washing the second pretreatment material with water, and obtaining the polyimide fiber with higher purity after the second pretreatment material is washed with water.
Further, the acid solution is an acid aqueous solution, and the mass fraction of acid in the acid aqueous solution is 20-50%.
Further, the aqueous acid solution includes one or more of hydrochloric acid, sulfuric acid, and nitric acid.
Furthermore, hydrogen peroxide can be added into the acidic solution.
Further, the alkaline solution is an alkaline aqueous solution, and the mass fraction of the alkali in the alkaline aqueous solution is 5-20%.
Further, the aqueous alkali solution includes one or both of an aqueous sodium hydroxide solution and aqueous ammonia.
Furthermore, the polyimide and the blended textile thereof are one or more of waste clothing leftover materials, clothing, towels and shoes and hats, and the material of the waste polyimide textile is one or more of knitted fabrics, woven fabrics, non-woven fabrics and geotextiles.
Furthermore, the polyimide waste textile comprises polyimide textile or textile blended by polyimide and various strong acid-intolerant fibers such as cotton, hemp, viscose, nylon and the like.
Further, both the acidic solution and the basic solution are circulated.
Further, the method for separating and recovering the polyimide waste textiles is characterized in that the reaction pressure of the polyimide waste textiles in the treatment process is normal pressure or high pressure.
The application also provides a method for decomposing and recycling the polyimide and the blended textile thereof, and the polyimide and the blended textile thereof are pretreated by any one of the methods for separating and recycling the polyimide and the blended textile thereof.
The beneficial effect of this application is: different from the situation of the prior art, the application provides a separation and recovery method of polyimide and blended textiles thereof, which comprises the following steps: soaking polyimide and blended textiles thereof in an acid solution for treatment, so that fibers with weak acid resistance are dissolved, and an undissolved first pretreatment material is obtained; washing the first pretreatment material with water, soaking the washed first pretreatment material in an alkaline solution for acid-base neutralization treatment to obtain an insoluble second pretreatment material; and washing the second pretreatment material with water, and obtaining the high-purity polyimide fiber after the second pretreatment material is washed clean with water. The method can be used for treating the polyimide and the blended textile thereof or the waste polyimide textile with the dye and the auxiliary agent, can separate and recover the high-purity polyimide fiber, and is low in price, simple, environment-friendly and efficient.
Drawings
FIG. 1: the application discloses a flow schematic diagram of an embodiment of a separation and recovery method of polyimide and blended textiles thereof.
Detailed Description
In order to make the purpose, technical solution and effect of the present application clearer and clearer, the present application is further described in detail below with reference to the accompanying drawings and examples.
Referring to fig. 1, fig. 1 is a schematic flow chart of an embodiment of a separation and recovery method of polyimide and blended textiles thereof, and the method comprises the following steps:
step S101: and soaking the polyimide and the blended textile thereof in an acid solution for treatment for 30-60 min at the treatment temperature of 90-200 ℃ to dissolve the fibers with weak acid resistance, thereby obtaining an insoluble first pretreatment material.
Polyimide fibers have excellent acid resistance and are relatively difficult to be subjected to acid hydrolysis. The method comprises the steps of soaking polyimide waste textiles in an acid solution, setting the temperature range to be lower than 90-200 ℃ of thermal decomposition of polyimide, and setting the time to be 30-60 min, wherein in the time period, other relatively acid-fast fibers or dyes and auxiliaries except polyimide fibers in the polyimide and the blended textiles thereof are subjected to acidolysis, if the time is too short, materials except the polyimide fibers are not easy to treat cleanly, and if the time is too long, the polyimide fibers can also be subjected to relatively severe acidolysis to influence the yield of the polyimide fibers.
Step S102: and (3) washing the first pretreatment material, soaking the washed first pretreatment material in an alkaline solution for acid-base neutralization treatment, wherein the treatment time is 30-40 min, and the treatment temperature is 60-90 ℃, so that an insoluble second pretreatment material is obtained.
The first pretreatment material once immersed in the acidic solution is washed with water to wash away the acidic solution from the polyimide fibers. Since the acid on the polyimide fiber cannot be completely removed by only water washing, the first pretreatment material after water washing is immersed in an alkaline solution to remove the remaining acid by neutralization reaction treatment. Aiming at the relatively poor alkali resistance of polyimide, the treatment time of neutralization treatment is 30-40 min, the treatment temperature is 60-90 ℃, and the influence on polyimide fibers can be reduced as much as possible while thorough neutralization is ensured; the slightly less basic nature also allows further removal of other impurities, a small amount of polyimide can be lost, but the recovered polyimide is more pure.
Step S103: and washing the second pretreatment material with water, and obtaining the polyimide fiber with higher purity after the second pretreatment material is washed with water.
This application is handled through polyimide waste textile to the blending or the polyimide waste textile who has dyestuff and auxiliary agent, can separate and retrieve pure polyimide fiber, can retrieve for the degradation of follow-up polyimide fiber and provide pure raw and other materials, and the method is cheap, simple, environmental protection, high-efficient.
The acidic solution is a solution with a pH value of less than 7, and can be a solution of acid, or a solution of other compounds with acidic solution, such as ammonium nitrate. In one embodiment, the acid solution is an aqueous solution of an acid, wherein the mass fraction of the acid is 20% to 50%, for example, 30%, 35%, 40%, 45%, and the like, and specifically, the acid solution may be one or more of hydrochloric acid, sulfuric acid, and nitric acid. The polyimide waste textile is treated by the acid solution, and other fibers or dyes and auxiliaries which are not relatively acid-resistant except the polyimide fibers in the polyimide waste textile can be removed.
The alkaline solution refers to a solution with a pH value of more than 7, and can be a solution of alkali or a solution of other compounds with alkaline solution, such as sodium carbonate and trisodium phosphate. In one embodiment, the alkaline solution is an aqueous solution of alkali, wherein the mass fraction of the alkali is 5% to 20%, for example, 10%, 13%, 15%, 18%, etc., specifically, the aqueous solution of alkali may be one or both of an aqueous solution of sodium hydroxide and aqueous ammonia, and the alkaline solution may neutralize the acid remaining on the waste polyimide textiles.
In one embodiment, the polyimide and its blended textile include polyimide textiles or textiles blended with polyimide and various fibers. The polyimide textile is not pure polyimide fiber, and is usually attached with various dyes and auxiliary agents, or is directly blended with other fibers, such as textiles blended by polyimide and various strong acid-intolerant fibers such as cotton, hemp, viscose, nylon and the like. The waste polyimide textile can be a polyimide textile containing various auxiliaries or dyes, and can also be a textile blended by polyimide and various fibers, the textile can be made of waste clothing leftover materials, clothing, towels, shoes and hats and the like, and the material can be one or more of knitted fabrics, woven fabrics, non-woven fabrics and geotextiles.
In one embodiment, the polyimide and the blended textile thereof are soaked in an acidic solution to remove impurities other than polyimide fibers, wherein the acidic solution is in a circulating flow. Through the circulation flow of the acid solution, the polyimide waste textile can be fully contacted with the acid solution, and the separation and purification rate of the polyimide fiber is higher. The acid-treated polyimide fiber is washed by water and then soaked in an alkaline solution for neutralization reaction, wherein the alkaline solution also flows circularly, so that the neutralization reaction rate of the alkaline solution is improved. In the whole separation and recovery process of the polyimide waste textile, the reaction pressure can be normal pressure or high pressure, wherein the high pressure is higher than the normal pressure. When the reaction pressure is higher than normal pressure, the rate of each reaction can be further accelerated.
The separation and recovery method provided by the application can separate and recover pure polyimide fibers by treating the blended polyimide waste textiles or the polyimide waste textiles with the dye and the auxiliary agent, can provide pure raw materials for the degradation and recovery of the subsequent polyimide fibers, and is low in cost, simple, environment-friendly and efficient. Based on the above, the application also provides a polyimide waste textile decomposition and recovery method, which comprises the steps of carrying out pretreatment by any one of the above polyimide waste textile separation and recovery methods to obtain pure polyimide fibers, and then further decomposing the pure polyimide fibers to recover raw materials with higher purity.
The present application will be illustrated and explained below by means of several groups of specific experimental examples, which should not be construed as limiting the scope of the present application.
Example 1
Putting the waste polyimide textile into a container filled with 30% sulfuric acid aqueous solution, raising the temperature to 90 ℃ under normal pressure, reacting and stirring for 60min, removing most other fibers and dyeing auxiliaries, taking out the rest polyimide textile, washing, putting the polyimide textile into a container filled with 10% sodium hydroxide aqueous solution, neutralizing at the temperature of 60 ℃, stirring for 30-40 min, finally washing with water to obtain pure polyimide fibers, and treating the polyimide fibers by using the prior patent technology to prepare the polyimide raw material.
Example 2
Putting the waste polyimide textile into a container filled with a mixed aqueous solution of 30 mass percent sulfuric acid and 10 mass percent hydrochloric acid, raising the temperature to 120 ℃, reacting and stirring for 30-60 min, removing other fibers and dyeing auxiliaries, taking out the residual polyimide textile, washing, putting the residual polyimide textile into a container filled with 10 mass percent sodium hydroxide aqueous solution, neutralizing at 90 ℃, stirring for 30-40 min, finally washing with water to obtain pure polyimide fibers, and treating the pure polyimide fibers by utilizing the prior patent technology to prepare a polyimide raw material.
Example 3
Putting the waste polyimide textile into a mixed aqueous solution container filled with 10% sulfuric acid and 10% nitric acid, raising the temperature to 150 ℃, reacting and stirring for 30-60 min, taking out the residual polyimide textile after other fibers and dyeing auxiliaries are removed, washing, putting the residual polyimide textile into a container filled with 15% sodium hydroxide aqueous solution, neutralizing at 80 ℃, stirring for 30-40 min, finally washing with water to obtain pure polyimide fibers, and treating the pure polyimide fibers by utilizing the prior patent technology to prepare the polyimide raw material.
Example 4
Putting the waste polyimide textile into a container filled with 20% sulfuric acid solution by mass, raising the temperature to 200 ℃, reacting and stirring for 30-60 min, removing other fibers and dyeing auxiliary agents, taking out the residual polyimide textile, washing, putting the residual polyimide textile into a container filled with 3% sodium hydroxide by mass and 8% ammonia by mass, neutralizing at 70 ℃, stirring for 30-40 min, finally washing with water to obtain pure polyimide fibers, and treating the pure polyimide fibers by utilizing the prior patent technology to prepare the polyimide raw material.
Example 5
Putting the waste polyimide textile into a mixed aqueous solution container filled with 40% by mass of sulfuric acid, 5% by mass of hydrochloric acid and 5% by mass of nitric acid, raising the temperature to 90 ℃, reacting and stirring for 30-60 min, taking out the residual polyimide textile after other fibers and dyeing auxiliary agents are removed, washing with water, putting the residual polyimide textile into a mixed aqueous solution container filled with 7% by mass of sodium hydroxide and 13% by mass of ammonia, neutralizing at the temperature of 90 ℃, stirring for 30-40 min, finally washing with water to obtain pure polyimide fibers, and treating the pure polyimide fibers by utilizing the prior patent technology to prepare the polyimide raw material.
The above description is only for the purpose of illustrating embodiments of the present application and is not intended to limit the scope of the present application, and all modifications of equivalent structures and equivalent processes, which are made by the contents of the specification and the drawings of the present application or are directly or indirectly applied to other related technical fields, are also included in the scope of the present application.
Claims (10)
1. A separation and recovery method of polyimide and blended textiles thereof is characterized by comprising the following steps:
soaking polyimide and blended textiles thereof in an acid solution for treatment for 30-60 min at 90-200 ℃ to dissolve fibers with weak acid resistance to obtain an undissolved first pretreatment material;
washing the first pretreatment material with water, soaking the washed first pretreatment material in an alkaline solution for acid-base neutralization treatment, wherein the treatment time is 30-40 min, and the treatment temperature is 60-90 ℃, so that an insoluble second pretreatment material is obtained;
and washing the second pretreatment material with water, and obtaining the polyimide fiber with higher purity after the second pretreatment material is washed with water.
2. The method for separating and recovering the polyimide and the blended textile thereof according to claim 1, wherein the acidic solution is an aqueous acid solution, and the mass fraction of the acid is 20-50%.
3. The method for separating and recovering the polyimide and the blended textile thereof according to claim 2, wherein the acidic solution comprises one or more of hydrochloric acid, sulfuric acid and nitric acid.
4. The method for separating and recovering the polyimide and the blended textile thereof according to claim 1, wherein the alkaline solution is an aqueous solution of alkali, and the mass fraction of the alkali is 5-20%.
5. The method for separating and recovering the polyimide and the blended textile thereof according to claim 4, wherein the aqueous solution of the alkali comprises one or both of an aqueous solution of sodium hydroxide and aqueous ammonia.
6. The method for separating and recovering the polyimide and the blended textile thereof according to claim 1, wherein the polyimide and the blended textile thereof are from various recovered waste materials, and the polyimide and the blended textile thereof are made of one or more of knitted fabrics, woven fabrics, non-woven fabrics and geotextiles.
7. The method for separating and recovering the polyimide and the blended textile thereof according to claim 1, wherein the polyimide and the blended textile thereof comprise a polyimide textile or a textile blended by the polyimide and the strong acid-intolerant fiber, and the strong acid-intolerant fiber is one or more of cotton, hemp, viscose and nylon.
8. The method for separating and recovering polyimide and blended textiles thereof as claimed in claim 1, wherein both the acidic solution and the alkaline solution are circulated.
9. The method for separating and recovering the polyimide and the blended textile thereof according to claim 1, wherein the reaction pressure of the polyimide and the blended textile thereof in the treatment process is normal pressure or high pressure.
10. A method for decomposing and recycling polyimide and blended textiles thereof is characterized in that the polyimide and the blended textiles thereof are pretreated by the method for separating and recycling the polyimide and the blended textiles thereof according to any one of claims 1 to 9.
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| WO2024056863A1 (en) * | 2022-09-16 | 2024-03-21 | Soft Chemicals S.R.L. | Process for the recovery and recycling of textile fibers |
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