CN106432792A - Recovery process of polyimide waste - Google Patents
Recovery process of polyimide waste Download PDFInfo
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- CN106432792A CN106432792A CN201610642292.8A CN201610642292A CN106432792A CN 106432792 A CN106432792 A CN 106432792A CN 201610642292 A CN201610642292 A CN 201610642292A CN 106432792 A CN106432792 A CN 106432792A
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- polyimides
- recovery process
- waste
- old
- discarded object
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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
- C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
- C08J11/08—Recovery or working-up of waste materials of polymers without chemical reactions using selective solvents for polymer components
-
- 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
- C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
-
- 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
- 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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Water Treatment By Sorption (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a recovery process of polyimide waste. The recovery process of the polyimide waste comprises the following steps: (1) carrying out pretreatment on the polyimide waste: carrying out surface spray cleaning and ultraviolet sterilization on the polyimide waste; (2) breaking, dissolving and precipitating the polyimide waste. The recovery process of the polyimide waste disclosed by the invention has the beneficial effects of solving the problems of complex recovery process, high energy consumption and low added values of products in the prior art and providing the recovery process of the polyimide waste with simple technological process, low energy consumption, small solvent consumption and high product performances through reasonable parameter setting.
Description
Technical field
The present invention relates to resource recycling field, be specifically related to the recovery process of a kind of polyimides discarded object.
Background technology
At present, China is method and the physics side of chemical degradation to the main method of polyimides recycling waste
Method, chemical method refers to macromolecule generation degradation reaction under the effect of thermally and chemically reagent, forms the product of low-molecular-weight, produces
Thing can be further with as monomer can be polymerized again, oil product can carry out deep processing, but chemical method needs HTHP, causes consumption
Energy is high, condition is harsh, requires height to equipment material, can be to realize large-scale operation.Physical method is by cutting off, pulverizing, adding
The recycle utilization that waste or used plastics is reprocessed by the operations such as heat fusing, but the performance of various regenerated plastics is bigger than new material
For reduce, and contain a large amount of impurity.
Content of the invention
The technical problem to be solved is that in prior art, plastics recycling process is complicated, and energy consumption is high, and product adds
It is worth low problem.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：A kind of recovery process of polyimides discarded object, bag
Include following steps：
(1) pretreatment of polyimides discarded object：Polyimides discarded object is carried out surface spraying cleaning and ultraviolet kills
Bacterium；
(2) joining in pulverizer by the waste and old polyimide material collected, it is the useless of 0.1-5mm that pulverizing obtains particle diameter
Old polyimide particles；
(3) at 50-80 DEG C, described waste and old polyimide particles is put into the closed container equipped with the first organic solvent
In and stir 5-15min, make described waste and old polyimide particles rapid solution, form homogeneous phase solution；
(4) adding adsorbent in above-mentioned solution, standing forms standing liquid a moment, by described standing liquid addition hole is
400-500 purpose the first filter filters, obtains a filter residue and first-time filtrate；
(5) 45-60 DEG C, under normal pressure, by the described first-time filtrate that obtains in step (4) under stirring, add the
Two organic solvents, separate out polyimides powdery thing, and initial gross separation obtains the dirty solution containing polyimides powdery thing and solvent
Solution；
(6) step (5) is contained the dirty solution of polyimides powdery thing, centrifugal dewatering in centrifuge, obtain centrifugal filter
Liquid and sediment；Dry the polyimide powder of described sediment washing.
The invention has the beneficial effects as follows：Solve recovery process complexity in prior art, energy consumption height, low the asking of added value of product
Topic, technological process is simple, energy consumption is low, solvent-oil ratio is little to arrange offer one by rational parameter, high the gathering of properties of product
The recovery process of acid imide discarded object.
On the basis of technique scheme, the present invention can also do following improvement：
Further, described step (5) also includes, the described solvent solution obtaining described step (5), at 75-85 DEG C
At a temperature of, carry out air-distillation and be separated and recovered from the second organic solvent and the step of the first organic solvent.
Further, the recovery process of described waste and old polyimide material also includes step (7), described step (7) for
The centrifugal filtrate that described step (6) obtains adds described first organic solvent, and repeating said steps (2) is to described step
(6) step, carrying out secondary crystallization recovery.
Further, described first organic solvent is 1-METHYLPYRROLIDONE, described waste and old polyimide particles and described N-
The weight ratio of methyl pyrrolidone is 1：6-1：9.
Further, described waste and old polyimide particles and the weight ratio of described 1-METHYLPYRROLIDONE are 1：8.
Further, the hole of described first filter is 450 mesh.
Further, described second organic solvent is methyl alcohol, the body of the addition of described methyl alcohol and described first organic solvent
Long-pending ratio is 1：1-1：4.
Further, described adsorbent is activated carbon, activated alumina, the one in polymeric adsorbent.
Detailed description of the invention
Being described the principle and feature of the present invention below, example is served only for explaining the present invention, is not intended to limit
Determine the scope of the present invention.
Embodiment 1
The recovery process of a kind of polyimides discarded object of the present invention, comprises the following steps：
(1) pretreatment of polyimides discarded object：Polyimides discarded object is carried out surface spraying cleaning and ultraviolet kills
Bacterium；
(2) joining in pulverizer by the waste and old polyimide material collected, it is the waste and old of 0.1mm that pulverizing obtains particle diameter
Polyimide particles；
(3) at 50 DEG C, put into described waste and old polyimide particles in the closed container equipped with the first organic solvent
And stir 5min, make described waste and old polyimide particles rapid solution, form homogeneous phase solution；
(4) adding adsorbent in above-mentioned solution, standing forms standing liquid a moment, by described standing liquid addition hole is
400 purpose the first filters filter, obtains a filter residue and first-time filtrate；
(5) 45 DEG C, under normal pressure, by the described first-time filtrate that obtains in step (4) under stirring, add second to have
Machine solvent, separates out polyimides powdery thing, and initial gross separation obtains the dirty solution containing polyimides powdery thing and solvent solution；
(6) step (5) is contained the dirty solution of polyimides powdery thing, centrifugal dewatering in centrifuge, obtain centrifugal filter
Liquid and sediment；Dry the polyimide powder of described sediment washing.
Further, described step (5) also includes, the described solvent solution obtaining described step (5), the temperature of 75 DEG C
Under, carry out air-distillation and be separated and recovered from the second organic solvent and the step of the first organic solvent.
The recovery process of described waste and old polyimide material also includes step (7), and described step (7) is for described step
(6) centrifugal filtrate obtaining adds described first organic solvent, and repeating said steps (2) is to described step (6), carries out two
The step that secondary crystallization is reclaimed.
Described first organic solvent is 1-METHYLPYRROLIDONE, described waste and old polyimide particles and described N-methylpyrrole
The weight ratio of alkanone is 1：6.
Described second organic solvent is methyl alcohol, and the addition of described methyl alcohol is 1 with the volume ratio of described first organic solvent：
1.
Described adsorbent is activated carbon.
Embodiment 2
The recovery process of a kind of polyimides discarded object of the present invention, comprises the following steps：
(1) pretreatment of polyimides discarded object：Polyimides discarded object is carried out surface spraying cleaning and ultraviolet kills
Bacterium；
(2) joining in pulverizer by the waste and old polyimide material collected, it is the waste and old poly-of 5mm that pulverizing obtains particle diameter
Acid imide particle；
(3) at 80 DEG C, put into described waste and old polyimide particles in the closed container equipped with the first organic solvent
And stir 15min, make described waste and old polyimide particles rapid solution, form homogeneous phase solution；
(4) adding adsorbent in above-mentioned solution, standing forms standing liquid a moment, by described standing liquid addition hole is
500 purpose the first filters filter, obtains a filter residue and first-time filtrate；
(5) 60 DEG C, under normal pressure, by the described first-time filtrate that obtains in step (4) under stirring, add second to have
Machine solvent, separates out polyimides powdery thing, and initial gross separation obtains the dirty solution containing polyimides powdery thing and solvent solution；
(6) step (5) is contained the dirty solution of polyimides powdery thing, centrifugal dewatering in centrifuge, obtain centrifugal filter
Liquid and sediment；Dry the polyimide powder of described sediment washing.
Described step (5) also includes, the described solvent solution obtaining described step (5), at a temperature of 85 DEG C, carries out
Air-distillation is separated and recovered from the second organic solvent and the step of the first organic solvent.
The recovery process of described waste and old polyimide material also includes step (7), and described step (7) is for described step
(6) centrifugal filtrate obtaining adds described first organic solvent, and repeating said steps (2) is to described step (6), carries out two
The step that secondary crystallization is reclaimed.
Described first organic solvent is 1-METHYLPYRROLIDONE, described waste and old polyimide particles and described N-methylpyrrole
The weight ratio of alkanone is 1：9.
Described second organic solvent is methyl alcohol, and the addition of described methyl alcohol is 1 with the volume ratio of described first organic solvent：
4.
Described adsorbent is activated alumina.
Embodiment 3
The recovery process of a kind of polyimides discarded object of the present invention, comprises the following steps：
(1) pretreatment of polyimides discarded object：Polyimides discarded object is carried out surface spraying cleaning and ultraviolet kills
Bacterium；
(2) joining in pulverizer by the waste and old polyimide material collected, it is the waste and old poly-of 1mm that pulverizing obtains particle diameter
Acid imide particle；
(3) at 70 DEG C, put into described waste and old polyimide particles in the closed container equipped with the first organic solvent
And stir 8min, make described waste and old polyimide particles rapid solution, form homogeneous phase solution；
(4) adding adsorbent in above-mentioned solution, standing forms standing liquid a moment, by described standing liquid addition hole is
450 purpose the first filters filter, obtains a filter residue and first-time filtrate；
(5) 50 DEG C, under normal pressure, by the described first-time filtrate that obtains in step (4) under stirring, add second to have
Machine solvent, separates out polyimides powdery thing, and initial gross separation obtains the dirty solution containing polyimides powdery thing and solvent solution；
(6) step (5) is contained the dirty solution of polyimides powdery thing, centrifugal dewatering in centrifuge, obtain centrifugal filter
Liquid and sediment；Dry the polyimide powder of described sediment washing.
Described step (5) also includes, the described solvent solution obtaining described step (5), at a temperature of 78 DEG C, carries out
Air-distillation is separated and recovered from the second organic solvent and the step of the first organic solvent.
The recovery process of described waste and old polyimide material also includes step (7), and described step (7) is for described step
(6) centrifugal filtrate obtaining adds described first organic solvent, and repeating said steps (2) is to described step (6), carries out two
The step that secondary crystallization is reclaimed.
Described first organic solvent is 1-METHYLPYRROLIDONE, described waste and old polyimide particles and described N-methylpyrrole
The weight ratio of alkanone is 1：8.
Described second organic solvent is methyl alcohol, and the addition of described methyl alcohol is 1 with the volume ratio of described first organic solvent：
2.
Described adsorbent is in polymeric adsorbent.
Embodiment 4
The recovery process of a kind of polyimides discarded object of the present invention, comprises the following steps：
(1) pretreatment of polyimides discarded object：Polyimides discarded object is carried out surface spraying cleaning and ultraviolet kills
Bacterium；
(2) joining in pulverizer by the waste and old polyimide material collected, it is the waste and old poly-of 2mm that pulverizing obtains particle diameter
Acid imide particle；
(3) at 60 DEG C, put into described waste and old polyimide particles in the closed container equipped with the first organic solvent
And stir 12min, make described waste and old polyimide particles rapid solution, form homogeneous phase solution；
(4) adding adsorbent in above-mentioned solution, standing forms standing liquid a moment, by described standing liquid addition hole is
450 purpose the first filters filter, obtains a filter residue and first-time filtrate；
(5) 55 DEG C, under normal pressure, by the described first-time filtrate that obtains in step (4) under stirring, add second to have
Machine solvent, separates out polyimides powdery thing, and initial gross separation obtains the dirty solution containing polyimides powdery thing and solvent solution；
(6) step (5) is contained the dirty solution of polyimides powdery thing, centrifugal dewatering in centrifuge, obtain centrifugal filter
Liquid and sediment；Dry the polyimide powder of described sediment washing.
Described step (5) also includes, the described solvent solution obtaining described step (5), at a temperature of 82 DEG C, carries out
Air-distillation is separated and recovered from the second organic solvent and the step of the first organic solvent.
The recovery process of described waste and old polyimide material also includes step (7), and described step (7) is for described step
(6) centrifugal filtrate obtaining adds described first organic solvent, and repeating said steps (2) is to described step (6), carries out two
The step that secondary crystallization is reclaimed.
Described first organic solvent is 1-METHYLPYRROLIDONE, described waste and old polyimide particles and described N-methylpyrrole
The weight ratio of alkanone is 1：7.
Described second organic solvent is methyl alcohol, and the addition of described methyl alcohol is 1 with the volume ratio of described first organic solvent：
3.
Described adsorbent is activated carbon.
Comparative example 1
The recovery process of a kind of polyimides discarded object, comprises the following steps：
(1) joining in pulverizer by the waste and old polyimide material collected, it is the useless of 10-20mm that pulverizing obtains particle diameter
Old polyimide particles；
(2) described waste and old polyimide particles is put into equipped with in the closed container of 1-METHYLPYRROLIDONE and stir 5-
15min, makes described waste and old polyimide particles rapid solution, forms homogeneous phase solution；
(3) after above-mentioned homogeneous filtrate being filtered, filtrate adds methyl alcohol while stirring, separates out polyimides powdery thing,
And initial gross separation obtains the dirty solution containing polyimides powdery thing and solvent solution；
(4) step (3) is contained the dirty solution of polyimides powdery thing, centrifugal dewatering in centrifuge, obtain centrifugal filter
Liquid and sediment；Dry the polyimide powder of described sediment washing.
In above-described embodiment 1-4 and comparative example 1, the proterties of product and yield are as shown in Table 1：
Table one：The proterties of product and yield in above-described embodiment 1-4 and comparative example 1
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all spirit in the present invention and
Within principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (8)
1. the recovery process of a polyimides discarded object, it is characterised in that comprise the following steps：
(1) pretreatment of polyimides discarded object：Polyimides discarded object is carried out surface spraying cleaning and ultraviolet sterilization；
(2) joining in pulverizer by the waste and old polyimide material collected, it is the waste and old poly-of 0.1-5mm that pulverizing obtains particle diameter
Acid imide particle；
(3) at 50-80 DEG C, described waste and old polyimide particles is put into equipped with in the closed container of the first organic solvent simultaneously
Stirring 5-15min, makes described waste and old polyimide particles rapid solution, forms homogeneous phase solution；
(4) adding adsorbent in above-mentioned solution, standing a moment and form standing liquid, described standing liquid is added hole is 400-
500 purpose the first filters filter, obtains a filter residue and first-time filtrate；
(5) 45-60 DEG C, under normal pressure, by the described first-time filtrate that obtains in step (4) under stirring, add second to have
Machine solvent, separates out polyimides powdery thing, and initial gross separation obtains the dirty solution containing polyimides powdery thing and solvent solution；
(6) by step (5) containing the dirty solution of polyimides powdery thing, centrifugal dewatering in centrifuge, obtain centrifugal filtrate and
Sediment；Dry the polyimide powder of described sediment washing.
2. the recovery process of polyimides discarded object according to claim 1, it is characterised in that described step (5) is also wrapped
Include, the described solvent solution that described step (5) is obtained, at a temperature of 75-85 DEG C, carry out air-distillation and be separated and recovered from
Two organic solvents and the step of the first organic solvent.
3. the recovery process of polyimides discarded object according to claim 2, it is characterised in that described waste and old polyamides is sub-
The recovery process of amine material also includes step (7), and described step (7) is for adding in the centrifugal filtrate that described step (6) obtains
Described first organic solvent, and repeating said steps (2) is to described step (6), the step carrying out secondary crystallization recovery.
4. the recovery process of the polyimides discarded object according to claim 1-3 is arbitrary, it is characterised in that described first has
Machine solvent is 1-METHYLPYRROLIDONE, and described waste and old polyimide particles is 1 with the weight ratio of described 1-METHYLPYRROLIDONE：6-
1：9.
5. the recovery process of polyimides discarded object according to claim 4, it is characterised in that described waste and old polyimides
Particle is 1 with the weight ratio of described 1-METHYLPYRROLIDONE：8.
6. the recovery process of the polyimides discarded object according to claim 1-3 or 5 are arbitrary, it is characterised in that described
The hole of one filter is 450 mesh.
7. the recovery process of the polyimides discarded object according to claim 1-3 or 5 are arbitrary, it is characterised in that described
Two organic solvents are methyl alcohol, and the addition of described methyl alcohol is 1 with the volume ratio of described first organic solvent：1-1：4.
8. the recovery process of the polyimides discarded object according to claim 1-7 is arbitrary, it is characterised in that described adsorbent
For the one in activated carbon, activated alumina, polymeric adsorbent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610642292.8A CN106432792A (en) | 2016-08-08 | 2016-08-08 | Recovery process of polyimide waste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610642292.8A CN106432792A (en) | 2016-08-08 | 2016-08-08 | Recovery process of polyimide waste |
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| CN106432792A true CN106432792A (en) | 2017-02-22 |
Family
ID=58184626
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610642292.8A Pending CN106432792A (en) | 2016-08-08 | 2016-08-08 | Recovery process of polyimide waste |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111621059A (en) * | 2020-05-26 | 2020-09-04 | 苏州中纺学面料产业研究院 | Separation and recovery method of polyimide and blended textile thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101506281A (en) * | 2006-06-26 | 2009-08-12 | 沙伯基础创新塑料知识产权有限公司 | Polyimide solvent cast films having a low coefficient of thermal expansion and method of manufacture thereof |
| CN102911396A (en) * | 2012-10-22 | 2013-02-06 | 广东树业环保科技股份有限公司 | Process for recovering waste polyethylene glycol terephthalate (PET) material |
-
2016
- 2016-08-08 CN CN201610642292.8A patent/CN106432792A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101506281A (en) * | 2006-06-26 | 2009-08-12 | 沙伯基础创新塑料知识产权有限公司 | Polyimide solvent cast films having a low coefficient of thermal expansion and method of manufacture thereof |
| CN102911396A (en) * | 2012-10-22 | 2013-02-06 | 广东树业环保科技股份有限公司 | Process for recovering waste polyethylene glycol terephthalate (PET) material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111621059A (en) * | 2020-05-26 | 2020-09-04 | 苏州中纺学面料产业研究院 | Separation and recovery method of polyimide and blended textile thereof |
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Application publication date: 20170222 |