CN111073035B - Method for rapidly degrading and recycling polyimide material - Google Patents
Method for rapidly degrading and recycling polyimide material Download PDFInfo
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- CN111073035B CN111073035B CN201911270699.2A CN201911270699A CN111073035B CN 111073035 B CN111073035 B CN 111073035B CN 201911270699 A CN201911270699 A CN 201911270699A CN 111073035 B CN111073035 B CN 111073035B
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- polyimide
- polyimide material
- filtering
- recycling
- soaking
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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
-
- 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
- C08J11/18—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 organic material
- C08J11/28—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 organic material by treatment with organic compounds containing nitrogen, sulfur or phosphorus
-
- 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
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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
Abstract
The invention relates to a method for rapidly degrading and recycling a polyimide material, belonging to the fields of light chemical industry and material synthesis technology. The method comprises the steps of soaking a polyimide material in dimethyl sulfoxide serving as a solvent, and heating to fully swell the material; filtering the swelled polyimide material to be dry and then soaking the polyimide material in alkali liquor with the mass concentration of 1-15% at constant temperature; stirring and decomposing into small molecular compounds; filtering, distilling the filtrate to separate out small molecular compounds, filtering, purifying and recovering. The method changes the molecular chain arrangement structure of the polyimide material through solvent dissolution and swelling, enlarges the material pores, and enables the alkali liquor to be quickly diffused into the material to destroy the molecular structure of the material, thereby realizing the quick degradation of the polyimide material. The invention can quickly degrade and decompose the scrapped polyimide material, promote the recycling of chemical raw materials and reduce the production cost; but also respond to ecological environment protection.
Description
Technical Field
The invention relates to the fields of light chemical industry and material synthesis, in particular to a method for rapidly degrading and recycling a polyimide material.
Technical Field
The polyimide fiber has the obvious characteristics of high temperature resistance, can work for a long time at the high temperature of 300 ℃ and can be used as a flame retardant material. However, the excellent heat resistance makes the degradation difficult, and in view of this situation, it is particularly significant to develop a green method for rapidly degrading polyimide materials.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides a method for quickly degrading and recycling a polyimide material, which can realize quick degradation, decomposition and recycling of the polyimide material, promote the recycling of chemical raw materials and reduce the production cost.
The technical problem to be solved by the present invention is achieved by the following technical means. The invention relates to a method for rapidly degrading and recycling a polyimide material, which is characterized by comprising the following steps: the method comprises the following steps:
(1) soaking the polyimide material in dimethyl sulfoxide solvent, heating to 60-120 deg.c to swell the material;
(2) taking out the swelled polyimide material, draining, soaking in 1-15 wt% alkali solution, and keeping the alkali solution at a constant temperature of 60-100 ℃;
(3) stirring and decomposing into small molecular compounds;
(4) filtering, distilling the filtrate to separate out small molecular compounds, filtering, purifying and recovering.
The invention discloses a method for rapidly degrading and recycling polyimide materials, which further adopts the preferable technical scheme that: the polyimide material in the step (1) is selected from a polyimide film, a polyimide plate, a polyimide fiber and a polyimide part. Or the rest products which are made of polyimide and can be recycled for the second time.
The invention discloses a method for rapidly degrading and recycling polyimide materials, which further adopts the preferable technical scheme that: and (4) filtering the filtrate obtained in the step (4) and reusing the filtrate obtained in the step (2) by adding alkali liquor.
The invention discloses a method for rapidly degrading and recycling polyimide materials, which further adopts the preferable technical scheme that: the heating temperature in the step (1) is 80-100 ℃.
The invention discloses a method for rapidly degrading and recycling polyimide materials, which further adopts the preferable technical scheme that: the mass concentration of the alkali liquor in the step (2) is 5-10%.
The invention discloses a method for rapidly degrading and recycling polyimide materials, which further adopts the preferable technical scheme that: the alkali liquor in the step (2) is NaOH aqueous solution.
The invention discloses a method for rapidly degrading and recycling polyimide materials, which further adopts the preferable technical scheme that: the rotating speed of the stirring in the step (3) is 30-120 r/min.
The invention discloses a method for rapidly degrading and recycling polyimide materials, which further adopts the preferable technical scheme that: the soaking time in the step (1) is 15-30 minutes.
Compared with the prior art, the invention has the beneficial effects that:
1. the method can quickly degrade and decompose the scrapped polyimide material, promote the recycling of chemical raw materials and reduce the production cost; respond to ecological environmental protection.
The method changes the molecular chain arrangement structure of the polyimide material through solvent dissolution and swelling, enlarges the material pores, and enables the alkali liquor to be quickly diffused into the material to destroy the molecular structure of the material, thereby realizing the quick degradation of the polyimide material.
Detailed description of the invention
The technical solutions in the embodiments of the present invention will be clearly and completely described 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.
Embodiment 1, a method for rapidly degrading and recycling a polyimide material, comprising the steps of:
(1) soaking the polyimide material in dimethyl sulfoxide solvent, heating to 60 deg.c to swell the material;
(2) taking out the swelled polyimide material, draining, soaking in 1% NaOH aqueous solution, and keeping the alkali solution at the constant temperature of 60 ℃; the soaking time is 15 minutes;
(3) stirring at the rotating speed of 30r/min, and decomposing into small molecular compounds;
(4) filtering, distilling the filtrate to separate out small molecular compounds, filtering, purifying and recovering.
The polyimide material is a recycled waste polyimide plate.
And (4) repeatedly using the filtrate obtained by filtering in the step (4) in the step (2), and repeatedly using the filtrate by supplementing alkali liquor to the required concentration.
Embodiment 2, a method for rapidly degrading and recycling a polyimide material, comprising the steps of:
(1) soaking the polyimide material in dimethyl sulfoxide solvent, heating to 120 deg.c to swell the material;
(2) taking out the swelled polyimide material, draining, soaking in 15% NaOH water solution for 30 min, and keeping the alkali solution at constant temperature to 100 ℃;
(3) stirring at the rotating speed of 120r/min, and decomposing into small molecular compounds;
(4) filtering, distilling the filtrate to separate out small molecular compounds, filtering, purifying and recovering.
The polyimide material is recycled waste imide fibers; and (4) adding a proper amount of NaOH aqueous solution into the filtrate obtained by filtering in the step (4) for repeatedly using in the step (2).
Embodiment 3, a method for rapidly degrading and recycling a polyimide material, comprising the steps of:
(1) soaking the polyimide material in dimethyl sulfoxide solvent, heating to 80 deg.c to swell the material;
(2) taking out the swelled polyimide material, draining, soaking in 5% NaOH water solution for 20 min, and keeping the alkali solution at the constant temperature of 80 ℃;
(3) stirring at 80r/min, and decomposing into small molecular compounds;
(4) filtering, distilling the filtrate to separate out small molecular compounds, filtering, purifying and recovering.
The polyimide material in the step (1) is selected from a polyimide film, a polyimide plate, a polyimide fiber and a polyimide part.
And (4) repeatedly using the filtrate obtained by filtering in the step (4) in the step (2) by supplementing NaOH aqueous solution.
Embodiment 4, a method for rapidly degrading and recycling a polyimide material, comprising the steps of:
(1) soaking a polyimide material in dimethyl sulfoxide serving as a solvent, and heating to 100 ℃ to fully swell the material;
(2) taking out the swelled polyimide material, draining, soaking in 10% NaOH water solution for 25 min, and keeping the alkali solution at the constant temperature of 85 ℃;
(3) stirring and decomposing into small molecular compounds;
(4) filtering, distilling the filtrate to separate out small molecular compounds, filtering, purifying and recovering.
The polyimide material in the step (1) is selected from a polyimide film, a polyimide plate, a polyimide fiber and a polyimide part. And (4) filtering the filtrate obtained in the step (4) and reusing the filtrate obtained in the step (2) by adding alkali liquor.
The recovered material has high purity and can be reused.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (1)
1. A method for rapidly degrading and recycling a polyimide material is characterized by comprising the following steps:
(1) soaking the polyimide material in dimethyl sulfoxide solvent, heating to 80 deg.c to swell the material;
(2) taking out the swelled polyimide material, draining, soaking in 5% NaOH water solution for 20 min, and keeping the alkali solution at the constant temperature of 80 ℃;
(3) stirring at 80r/min, and decomposing into small molecular compounds;
(4) filtering, distilling the filtrate to separate out small molecular compounds, filtering, purifying and recovering;
the polyimide material in the step (1) is selected from a polyimide film, a polyimide plate, a polyimide fiber and a polyimide part;
and (4) repeatedly using the filtrate obtained by filtering in the step (4) in the step (2) by supplementing NaOH aqueous solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911270699.2A CN111073035B (en) | 2019-12-12 | 2019-12-12 | Method for rapidly degrading and recycling polyimide material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911270699.2A CN111073035B (en) | 2019-12-12 | 2019-12-12 | Method for rapidly degrading and recycling polyimide material |
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| Publication Number | Publication Date |
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| CN111073035A CN111073035A (en) | 2020-04-28 |
| CN111073035B true CN111073035B (en) | 2022-04-26 |
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| CN201911270699.2A Active CN111073035B (en) | 2019-12-12 | 2019-12-12 | Method for rapidly degrading and recycling polyimide material |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113429623B (en) * | 2021-06-17 | 2022-05-31 | 中国科学院山西煤炭化学研究所 | Method for preparing polyamic acid by degrading polyimide resin |
| CN113354527A (en) * | 2021-06-17 | 2021-09-07 | 中国科学院山西煤炭化学研究所 | Method for degrading polyimide material by microwave |
| CN113372212A (en) * | 2021-06-17 | 2021-09-10 | 中国科学院山西煤炭化学研究所 | Method for recovering polyimide by selectively breaking imide bonds |
| CN115318717A (en) * | 2022-08-05 | 2022-11-11 | 华虹半导体(无锡)有限公司 | Method for removing residual glue on heating plate PI of baking unit |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1324789A (en) * | 2001-06-26 | 2001-12-05 | 中国科学院长春应用化学研究所 | Polyimide hydrolyzing recovery process |
| JP2006124530A (en) * | 2004-10-29 | 2006-05-18 | Toray Ind Inc | Method for alkaline hydrolysis of polyimide and method for recovering low molecular weight compound |
| CN101519359A (en) * | 2009-04-16 | 2009-09-02 | 李汉毅 | Method for recovering polyimide through hydrolysis |
| JP2013087148A (en) * | 2011-10-14 | 2013-05-13 | Toray Ind Inc | Method for alkaline hydrolysis of polyimide and method for recovery of low molecular weight compound and metal from polyimide metal laminate |
| CN109503614A (en) * | 2018-12-04 | 2019-03-22 | 宏威高新材料有限公司 | A method of recycling polyimides waste |
| CN109942816A (en) * | 2019-04-09 | 2019-06-28 | 中国科学院兰州化学物理研究所 | A kind of preparation method of Thermocurable polyimide |
-
2019
- 2019-12-12 CN CN201911270699.2A patent/CN111073035B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1324789A (en) * | 2001-06-26 | 2001-12-05 | 中国科学院长春应用化学研究所 | Polyimide hydrolyzing recovery process |
| JP2006124530A (en) * | 2004-10-29 | 2006-05-18 | Toray Ind Inc | Method for alkaline hydrolysis of polyimide and method for recovering low molecular weight compound |
| CN101519359A (en) * | 2009-04-16 | 2009-09-02 | 李汉毅 | Method for recovering polyimide through hydrolysis |
| JP2013087148A (en) * | 2011-10-14 | 2013-05-13 | Toray Ind Inc | Method for alkaline hydrolysis of polyimide and method for recovery of low molecular weight compound and metal from polyimide metal laminate |
| CN109503614A (en) * | 2018-12-04 | 2019-03-22 | 宏威高新材料有限公司 | A method of recycling polyimides waste |
| CN109942816A (en) * | 2019-04-09 | 2019-06-28 | 中国科学院兰州化学物理研究所 | A kind of preparation method of Thermocurable polyimide |
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| CN111073035A (en) | 2020-04-28 |
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