CN106750506A - A kind of method that two-step thermal processing reclaims carbon fiber - Google Patents
A kind of method that two-step thermal processing reclaims carbon fiber Download PDFInfo
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- CN106750506A CN106750506A CN201611247334.4A CN201611247334A CN106750506A CN 106750506 A CN106750506 A CN 106750506A CN 201611247334 A CN201611247334 A CN 201611247334A CN 106750506 A CN106750506 A CN 106750506A
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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
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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
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
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- 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
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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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
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08J2361/22—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
- C08J2361/24—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds with urea or thiourea
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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
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/06—Unsaturated polyesters
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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
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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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
- 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
Abstract
The invention belongs to the recycling field of carbon fibre composite, more particularly to a kind of method that two-step thermal processing reclaims carbon fiber.The method includes pretreatment and two processes of precision processing；The preprocessing process is：Carbon fibre composite is heated to 450 DEG C~600 DEG C, and is kept for 3~4 hours, then remove thermal source, cooled down；The precision processing process is：500 DEG C~550 DEG C will be heated to by the carbon fibre composite of the pretreatment, and be kept for 2~3 hours, then remove thermal source, cooled down, the solid product for finally giving is the carbon fiber after reclaiming.Recovery method of the invention can obtain the carbon fiber of small, the long and orderly high added value of the clean, extent of damage.The size and dimension of the carbon fibre reinforced composite is unrestricted, can be carried out continuously the recovery of carbon fiber, and can process large-sized carbon fibre composite, thus improves organic efficiency, has saved resource, saves cost recovery.
Description
Technical field
Carbon fiber is reclaimed the invention belongs to the recycling field of carbon fibre composite, more particularly to a kind of two-step thermal processing
Method.
Background technology
Carbon fibre reinforced high-molecular composite material (Carbon fiber reinforced polymer composites,
Abbreviation CFRP) there is the features such as density is small, specific strength and specific modulus are high, endurance life is high, fail safety characteristic is good, it is extensive
It is applied to the industries such as Aero-Space, auto industry, Wind Power Generation Industry, sports goods.It is expected that, only world's Forecast For Commercial Transport Market is to carbon
The demand of fiber is up to (2.0~3.0) × 104Ton/year.Furthermore it is contemplated that by 2025, the whole world amounted to and there will be over 8500
The business aircraft of frame is retired.In discarded carbon fibre composite, thermoplastic resin-based carbon fiber composite can be by system
Recycled into section, and be mainly buried to the conventional method that thermosetting resin is reclaimed and burn, but thermosetting resin base is compound
Can not be degraded within 50~100 years after material is buried, it is serious to environmental disruption；A large amount of cigarettes can be produced if burning disposal is carried out to it
Dirt, pernicious gas, pollute environment.
The method for reclaiming CFRP at present mainly includes Physical, solvent method and pyrolysismethod.Because Physical is needed to compound
Material is crushed, it is impossible to reclaim long fibre, therefore the method is not that the optimal of the long carbon fiber composite of high value is returned
Receiving method.Solvent method can use organic solvent or strong acid in removal process, also or under conditions of HTHP be returned
Receipts treatment, not only can generation environment pollution, some of them technique is also more complicated, causes cost recovery higher.Pyrolysis method is
The currently the only carbon fiber recovery technology in commercial applications, if but control the technological parameter of bad pyrolysismethod, can be to reclaiming
To the mechanical strength of carbon fiber cause damage, meanwhile, pyrolysismethod is subject to pyrolysis oven volumetric constraint, it is impossible to disposably process big chi
Very little carbon fiber composite.Therefore, CFRP is degraded under relatively reasonable technique, is recovered to loss in mechanical strength small
Long carbon fiber, can not only alleviate environmental pressure, reduce industry pollution, and can reduce product cost, with important warp
Ji meaning.
The content of the invention
In order to solve the above-mentioned technical problem, the invention provides a kind of method that two-step thermal processing reclaims carbon fiber, its bag
Include pretreatment and two processes of precision processing；The preprocessing process is：By carbon fibre composite, (i.e. background technology is mentioned
CFRP 450 DEG C~600 DEG C) are heated to, and are kept for 3~4 hours, then remove thermal source, cooled down；The precision processing process is：Will
By the carbon fibre composite heating (being preferably placed into heating in burner hearth) of the pretreatment to 500 DEG C~550 DEG C, and keep 2
~3 hours, thermal source is then removed, cooled down, that is, complete the process that carbon fiber is reclaimed in whole heat treatment, the solid product for finally giving
Carbon fiber after as reclaiming.
The present invention is first pre-processed to carbon fibre composite, then carries out precision processing, by the strict control to technique,
The carbon fiber of small, the long and orderly high added value of the clean, extent of damage can be obtained.And the fibre reinforced is compound
The size and dimension of material is unrestricted, can be carried out continuously the recovery of carbon fiber, thus improves organic efficiency.
Wherein, the carbon fibre composite is cooled to 30~60 DEG C by being cooled in the preprocessing process, preferably
The cooling procedure is Temperature fall.
Wherein, heating rate when being heated in the preprocessing process is 10~30 DEG C/min；And/or, the pretreatment
During mode of heating be any one in the heating of sunshine optically focused, electrical heating, heating by infrared radiation or media for heat exchange；
And/or, the heating atmosphere in the preprocessing process is have oxygen atmosphere or oxygen-free atmosphere.
The invention provides a kind of preferred scheme of the preprocessing process, i.e.,：In the heating atmosphere of ambient air
Under, the mode of heating heated using sunshine optically focused, with the heating rate of 25 DEG C/min, carbon fibre composite is heated to
500 DEG C, and kept for 3.5 hours, then naturally cool to 50 DEG C.
Wherein, the carbon fibre composite is cooled to room temperature by being cooled to during the precision processing, preferably described
Cooling procedure is Temperature fall.
Wherein, heating rate when being heated during the precision processing is 20~30 DEG C/min；And/or, the precision processing
During mode of heating for the heating of sunshine optically focused, electrical heating, fuse salt heat or heat-conducting oil heating in any one；With/
Or, the heating atmosphere during the precision processing is have oxygen atmosphere or oxygen-free atmosphere.
The invention provides a kind of preferred scheme of the precision processing process, i.e.,：Under the heating atmosphere of helium, using electricity
The mode of heating of heating, with the heating rate of 25 DEG C/min, will be heated to 550 through the pretreated carbon fibre composite
DEG C, and kept for 2.5 hours, be subsequently cooled to room temperature, that is, complete the whole process for reclaiming carbon fiber.
Wherein, during the precision processing, the heating will carried out by the carbon fibre composite of the pretreatment
It is preceding first to carry out machine cuts.
Wherein, the matrix of the carbon fibre composite is thermosetting resin；
Preferably, the thermosetting resin is epoxy resin, phenolic resin, unsaturated polyester resin, polyurethane resin, poly-
Any one in imide resin, Lauxite or furane resins.
Wherein, the form of the carbon fibre composite is fine continuous fiber, long fibre, chopped fiber, powder fiber or carbon
One or more in dimensional fabric.
Above-mentioned technical proposal of the invention has the advantages that：The present invention first carries out pre- place to carbon fibre composite
Reason, then precision processing is carried out, by the strict control to technique, small, the long and orderly height of the clean, extent of damage can be obtained
The carbon fiber of added value.The size and dimension of the carbon fibre reinforced composite is unrestricted, can be carried out continuously carbon fiber
Reclaim, thus improve organic efficiency.The optional use sunshine optically focused heating of pretreatment of the invention and precision processing process, makes
CFRP discarded objects are pre-processed with sunshine optically focused heating system, the limitation of device volume is not subject to processing, can process big
The carbon fibre composite of size, and resource has been saved, save cost recovery.
Brief description of the drawings
Fig. 1 is that the temperature of technique used by the present invention changes with time graph of a relation；
Fig. 2 is the carbon fibre composite configuration of surface figure after the before processing of the embodiment of the present invention 1；
Fig. 3 is the carbon fibre composite configuration of surface figure after the before processing of the embodiment of the present invention 2.
Specific embodiment
Embodiments of the present invention are described in further detail with reference to the accompanying drawings and examples.Following examples are used for
The present invention is illustrated, but can not be used for limiting the scope of the present invention.
The technical process of the embodiment of the present invention for details, reference can be made to accompanying drawing 1.It is carbon-fibre reinforced described in the embodiment of the present invention
Epoxy resin-based composite derives from retired aircraft.
Embodiment 1
A kind of method that two-step thermal processing reclaims carbon fiber is present embodiments provided, i.e.,：
Carbon fiber reinforced epoxy resin-based composite is chosen as salvage material, carbon-fibre reinforced epoxy resin is combined
Material is pre-processed in the form of the heating of sunshine optically focused.Pretreatment atmosphere is the air of normal temperature and pressure, and heating rate is 15
DEG C/min, 450 DEG C are heated to, and 3 hours are incubated, then naturally cool to 30 DEG C.
Pretreated carbon fibre composite is directly placed into the burner hearth for precision processing, burner hearth is hot with electrical heating
Source, is passed through helium, and is heated to 500 DEG C with the heating rate of 20 DEG C/min, after being incubated 2 hours, treats that it is cooled to room temperature, i.e., complete
Into whole removal process, the solid product for finally giving as carbon fiber.
Referring to accompanying drawing 2, the present embodiment reclaims the carbon fiber for obtaining and is compared than right side fibrillation plate.Carbon after heat treatment is fine
There is then lamination in dimension, it is apparent that establishment texture, and can be peeled off easily.The black particle that carbon fiber surface occurs
It may be the carbonization of resin in heat treatment process.Prove that resin is processed under the heat treatment condition, it is ensured that carbon fiber is obtained
High efficiente callback.
Embodiment 2
A kind of method that two-step thermal processing reclaims carbon fiber is present embodiments provided, i.e.,：
Carbon fiber reinforced epoxy resin-based composite is chosen as salvage material, carbon-fibre reinforced epoxy resin is combined
Material is pre-processed in the form of the heating of sunshine optically focused.Pretreatment atmosphere is the air of normal temperature and pressure, and heating rate is 20
DEG C/min, 500 DEG C are heated to, and 3.5 hours are incubated, then naturally cool to 40 DEG C.
Pretreated carbon fibre composite is directly placed into the burner hearth for precision processing, burner hearth is hot with electrical heating
Source, is passed through helium, and is heated to 550 DEG C with the heating rate of 25 DEG C/min, after being incubated 2.5 hours, treats that it is cooled to room temperature, i.e.,
Complete whole removal process.
Referring to accompanying drawing 3, the present embodiment reclaims the carbon fiber for obtaining and is compared than right side fibrillation plate.Carbon after heat treatment is fine
Dimension is scattered completely, and not only establishment texture is seen in layering completely, and can extract fiber precursor from the sample after intermediate treatment easily.
The micro black particle that carbon fiber surface occurs is the carbonization of resin in heat treatment process.Prove that resin has been obtained under the technique
Full pyrolysis, ensures that carbon fiber obtains clean and effective and reclaims than traditional way of recycling.
Embodiments of the invention are given for the sake of example and description, and are not exhaustively or by this to send out
It is bright to be limited to disclosed form.Many modifications and variations are for the ordinary skill in the art obvious.Choosing
It is, in order to more preferably illustrate principle of the invention and practical application, and to make one of ordinary skill in the art to select and describe embodiment
It will be appreciated that the present invention is suitable to the various embodiments with various modifications of special-purpose so as to design.
Claims (10)
1. a kind of method that two-step thermal processing reclaims carbon fiber, it is characterised in that including pretreatment and two processes of precision processing；
The preprocessing process is：Carbon fibre composite is heated to 450 DEG C~600 DEG C, and is kept for 3~4 hours, Ran Houleng
But；
The precision processing process is：500 DEG C~550 DEG C will be heated to by the carbon fibre composite of the pretreatment, and protected
Hold 2~3 hours, then cool down, the solid product for finally giving is the carbon fiber after reclaiming.
2. method according to claim 1, it is characterised in that being cooled to the carbon fiber in the preprocessing process
Composite is cooled to 30~60 DEG C, and preferably described cooling procedure is Temperature fall.
3. method according to claim 1 and 2, it is characterised in that heating rate when being heated in the preprocessing process
It is 10~30 DEG C/min；And/or, the mode of heating in the preprocessing process is the heating of sunshine optically focused, electrical heating, infrared ray
Any one in radiant heating or media for heat exchange；And/or, the heating atmosphere in the preprocessing process is have oxygen atmosphere or anaerobic
Atmosphere.
4. the method according to any one of claims 1 to 3, it is characterised in that the preprocessing process is specially：In normal temperature
Under the heating atmosphere of atmospheric air, the mode of heating heated using sunshine optically focused is fine by carbon with the heating rate of 25 DEG C/min
Dimension composite is heated to 500 DEG C, and is kept for 3.5 hours, then naturally cools to 50 DEG C.
5. the method according to any one of Claims 1 to 4, it is characterised in that being cooled to during the precision processing will
The carbon fibre composite is cooled to room temperature, and preferably described cooling procedure is Temperature fall.
6. the method according to any one of Claims 1 to 5, it is characterised in that liter when being heated during the precision processing
Warm speed is 20~30 DEG C/min；And/or, mode of heating during the precision processing is the heating of sunshine optically focused, electrical heating,
Fuse salt heat or heat-conducting oil heating in any one；And/or, heating atmosphere during the precision processing for have oxygen atmosphere or
Oxygen-free atmosphere.
7. the method according to any one of claim 1~6, it is characterised in that the precision processing process is specially：In helium
Heating atmosphere under, using electrically heated mode of heating, with the heating rate of 25 DEG C/min, will be fine through the pretreated carbon
Dimension composite is heated to 550 DEG C, and is kept for 2.5 hours, is subsequently cooled to room temperature, that is, complete the whole mistake for reclaiming carbon fiber
Journey.
8. the method according to any one of claim 1~7, it is characterised in that during the precision processing, will be by described
The carbon fibre composite of pretreatment first carries out machine cuts before the heating is carried out.
9. the method according to any one of claim 1~8, it is characterised in that the matrix of the carbon fibre composite is
Thermosetting resin；
Preferably, the thermosetting resin is epoxy resin, phenolic resin, unsaturated polyester resin, polyurethane resin, polyamides Asia
Any one in polyimide resin, Lauxite or furane resins.
10. the method according to any one of claim 1~9, it is characterised in that the form of the carbon fibre composite is
One or more in continuous fiber, long fibre, chopped fiber, powder fiber or carbon fibre fabric.
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| CN201611247334.4A CN106750506B (en) | 2016-12-29 | 2016-12-29 | A kind of method of two-step thermal processing recycling carbon fiber |
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| CN201611247334.4A CN106750506B (en) | 2016-12-29 | 2016-12-29 | A kind of method of two-step thermal processing recycling carbon fiber |
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| CN106750506A true CN106750506A (en) | 2017-05-31 |
| CN106750506B CN106750506B (en) | 2019-07-12 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4169108A4 (en) * | 2020-06-17 | 2024-05-08 | Grst Int Ltd | Method for composite delamination |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103665427A (en) * | 2013-12-11 | 2014-03-26 | 上海交通大学 | Method for recovering carbon fiber by cracking waste carbon fiber composite material |
| CN103665430A (en) * | 2013-11-21 | 2014-03-26 | 上海交通大学 | Thermolysis separation method for resin and carbon fibers in waste carbon fiber composite material |
| CN104262675A (en) * | 2014-09-01 | 2015-01-07 | 苏州德宝凯迪新材料有限公司 | Method for recovering carbon fibers from carbon fiber composite material |
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2016
- 2016-12-29 CN CN201611247334.4A patent/CN106750506B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103665430A (en) * | 2013-11-21 | 2014-03-26 | 上海交通大学 | Thermolysis separation method for resin and carbon fibers in waste carbon fiber composite material |
| CN103665427A (en) * | 2013-12-11 | 2014-03-26 | 上海交通大学 | Method for recovering carbon fiber by cracking waste carbon fiber composite material |
| CN104262675A (en) * | 2014-09-01 | 2015-01-07 | 苏州德宝凯迪新材料有限公司 | Method for recovering carbon fibers from carbon fiber composite material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4169108A4 (en) * | 2020-06-17 | 2024-05-08 | Grst Int Ltd | Method for composite delamination |
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