CN106810711A - A kind of method that carbon fiber is reclaimed from waste and old carbon fibre reinforced composite - Google Patents

A kind of method that carbon fiber is reclaimed from waste and old carbon fibre reinforced composite Download PDF

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Publication number
CN106810711A
CN106810711A CN201611247331.0A CN201611247331A CN106810711A CN 106810711 A CN106810711 A CN 106810711A CN 201611247331 A CN201611247331 A CN 201611247331A CN 106810711 A CN106810711 A CN 106810711A
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China
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fibre reinforced
carbon fiber
reinforced composite
carbon fibre
carbon
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CN106810711B (en
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梅生伟
吴磊
陈晓弢
薛小代
司杨
张韶红
陈来军
卢强
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Tsinghua University
Qinghai University
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Tsinghua University
Qinghai University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J11/00Recovery or working-up of waste materials
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/06Elements

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
  • Reinforced Plastic Materials (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Abstract

The present invention relates to the recovery of carbon fibre material, more particularly to a kind of method that carbon fiber is reclaimed from waste and old carbon fibre reinforced composite.It is described from waste and old carbon fibre reinforced composite reclaim carbon fiber method be:After the carbon fibre reinforced composite is pre-processed, the heating of 70~110min is carried out at 400~500 DEG C, gained solid product is the carbon fiber after reclaiming.The method of the invention process is simple, step is few, energy consumption is low, the carbon fiber surface that recovery is obtained is smooth, excellent performance, purity is high, and substantially increases the rate of recovery, there is important application and popularization value in waste and old carbon fibre reinforced composite field, the especially waste and old carbon fibre reinforced composite recycling field in retired aircraft.

Description

A kind of method that carbon fiber is reclaimed from waste and old carbon fibre reinforced composite
Technical field
Reclaimed from waste and old carbon fibre reinforced composite the present invention relates to the recovery of carbon fibre material, more particularly to one kind The method of carbon fiber.
Background technology
The great demand of the current retired aircraft in need of immediate treatment of China.Ended for the end of the year 2015, flown in world wide Business aircraft is about 20000 framves, and China's commercial aircraft accounts for 4000 framves, because Air Passenger machine Years Of Service is generally 25-30, on Stating type will progressively scrap and recycle.As can be seen here, in coming few decades, it is retired that the Chinese or even whole world there will be treatment The constant demand of aircraft.Carbon fiber (carbon fiber, abbreviation CF), is high intensity, height of a kind of phosphorus content more than 95% The new fiber materials of modulus fibre.Carbon fiber has many premium properties, and the axial strength and modulus of carbon fiber are high, density Low, higher than performance, good corrosion resistance, good electrical and thermal conductivity performance, electromagnetic wave shielding are good etc..
And as being applied to carbon fibre reinforced composite (the Carbon fiber of the military industry fields such as aircraft manufacturing Reinforced polymer composites, abbreviation CFRP) recycling can reach the mesh of save resources and the energy 's.The maximum obstruction of composite recovery technology commercialization is deficient, the high remanufacture of the market demand of regrown material The reduction of cost and regrown material performance.At present, the composite recovery technology of fibre reinforced includes following three kinds:Machinery Recovery, recuperation of heat and chemical recovery.
Used as a kind of method for reclaiming carbon fibre material, recuperation of heat has with low power consuming, disposal ability be strong, the rate of recovery is high Etc. incomparable advantage, if but control the technological parameter of bad recuperation of heat method, the machinery of carbon fiber that can be to being recovered to is strong Degree causes damage.
The content of the invention
In order to solve the above-mentioned technical problem, carbon is reclaimed from waste and old carbon fibre reinforced composite the invention provides one kind The method of fiber, i.e.,:After the carbon fibre reinforced composite is pre-processed, carry out 70~110min's at 400~500 DEG C Heat, gained solid product is the carbon fiber after reclaiming.The method of the invention reclaims the carbon fiber surface light for obtaining Sliding, excellent performance, purity is high, and substantially increases the rate of recovery.
Preferably, it is described to heat to heat 80~100min at 420~470 DEG C.
It is furthermore preferred that described heat to heat 85~95min at 440~460 DEG C.
Further preferably, it is described to heat to heat 90min at 450 DEG C.
Preferably, described pretreatment is:After the carbon fibre reinforced composite is cut, immersion in absolute ethyl alcohol is put into To remove surface impurity, then dry within 1.5~2.5 hours.
Further, it is described to be cut into:The carbon fibre reinforced composite is cut into the segment of 0.2m × 0.2m.
Further, the time for being put into immersion in absolute ethyl alcohol is 2 hours.
Preferably, the mode of the heating is the heating of sunshine optically focused.
The invention provides a kind of preferred scheme for reclaiming carbon fiber, it comprises the following steps:
(1) pre-process:The carbon fibre reinforced composite is cut into the small of 0.15~0.25m × 0.15~0.25m Section, is put into immersion in absolute ethyl alcohol and is then dried with removing surface impurity for 2~2.5 hours;
(2) heat:Carbon fibre reinforced composite after step (1) treatment is poly- using sunshine at 450 DEG C Light heats 90min, and gained solid product is the carbon fiber after reclaiming.
The matrix of carbon fibre reinforced composite of the present invention is thermosetting resin.
Above-mentioned technical proposal of the invention has the advantages that:The method of the invention process is simple, step is few, energy Consumption is low, and the carbon fiber surface that recovery is obtained is smooth, and excellent performance, purity is high, and substantially increases the rate of recovery.
Brief description of the drawings
Fig. 1 is processed by recuperation of heat at different temperatures for the waste and old carbon fibre reinforced composite of the embodiment of the present invention The TGA figures for arriving;
Fig. 2 is at 450 DEG C, process time is respectively 60min (A), 90min (B) and 120min (C) and reclaims the carbon for obtaining afterwards The scanning electron microscope (SEM) photograph of fiber;
Fig. 3 is at 450 DEG C, and process time is to reclaim the scanning electron microscope (SEM) photograph of the carbon fiber for obtaining after 90min.
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.
Waste and old carbon fibre reinforced composite used by the embodiment of the present invention derives from retired aircraft.
Embodiment 1
A kind of method that carbon fiber is reclaimed from waste and old carbon fibre reinforced composite, comprises the following steps:
(1) pre-process:The carbon fibre reinforced composite is cut into the segment of 0.2m × 0.2m, absolute ethyl alcohol is put into Then middle immersion is dried for 2 hours with removing surface impurity;
(2) heat:Carbon fibre reinforced composite after step (1) treatment is put on sample treatment platform, 450 90min is heated using sunshine optically focused at DEG C, gained solid product is the carbon fiber after reclaiming.
Embodiment 2
A kind of method that carbon fiber is reclaimed from waste and old carbon fibre reinforced composite, comprises the following steps:
(1) pre-process:The carbon fibre reinforced composite is cut into the segment of 0.2m × 0.25m, anhydrous second is put into 2.5 hours are soaked in alcohol to remove surface impurity, is then dried;
(2) heat:Carbon fibre reinforced composite after step (1) treatment is put on sample treatment platform, 470 95min is heated using sunshine optically focused at DEG C, gained solid product is the carbon fiber after reclaiming.
Embodiment 3
A kind of method that carbon fiber is reclaimed from waste and old carbon fibre reinforced composite, comprises the following steps:
(1) pre-process:The carbon fibre reinforced composite is cut into the segment of 0.15m × 0.15m, anhydrous second is put into 1.5 hours are soaked in alcohol to remove surface impurity, is then dried;
(2) heat:Carbon fibre reinforced composite after step (1) treatment is put on sample treatment platform, 420 100min is heated using sunshine optically focused at DEG C, gained solid product is the carbon fiber after reclaiming.
As seen from Figure 1, carbon fibre reinforced composite starts weightlessness at 344.1 DEG C, and weightlessness is 1.86%.Work as intensification To mass loss 16.80% at 436.6 DEG C.When being continuously heating to 697.0 DEG C, residual qualities are 75.42%.Illustrate the carbon fiber The pyrolysis temperature for strengthening composite is interval for 344.1~436.6 DEG C.The quality of carbon fiber keeps constant after continuing to heat up.
By Fig. 2 it can be seen that, the heat treatment carbon fiber surfaces that obtain of 60min have obvious buildup of resin, haircut mark in figure The resin of carbon fiber surface is shown;The carbon fiber surface obtained after heat treatment 90min is smooth;And obtained after processing 120min Carbon fiber surface there is obvious indenture (shown in circle), illustrate that with this understanding, carbon fiber surface has been destroyed.
By Fig. 3 it can be seen that, the carbon fiber surfaces that obtain are smooth after processing 90min at 450 DEG C, a diameter of 7 μm.
In sum, the technique of present invention photo-thermal method recovery carbon fibre reinforced composite processes 90min at 450 DEG C The excellent properties of carbon fiber can be retained.
Comparative example 1
A kind of method that carbon fiber is reclaimed from waste and old carbon fibre reinforced composite, its is substantially the same manner as Example 1, area It is not only that:The heating of step (2) heats 120min to utilize sunshine optically focused at 350 DEG C.Carbon fiber after treatment increases Strong composite material surface has substantial amounts of buildup of resin, multiple in fibre reinforced without thoroughly the resin of wrap carbon fiber is removed There was only a small amount of carbon fiber in condensation material surface.
Comparative example 2
A kind of method that carbon fiber is reclaimed from waste and old carbon fibre reinforced composite, its is substantially the same manner as Example 1, area It is not only that:The heating of step (2) heats 60min to utilize sunshine optically focused at 450 DEG C.The carbon fiber obtained after treatment Surface is smooth, but the resin being present in composite does not have completely burnout, and recovery carbon fiber material completely is not reached The purpose of material.
Comparative example 3
A kind of method that carbon fiber is reclaimed from waste and old carbon fibre reinforced composite, its is substantially the same manner as Example 1, area It is not only that:The heating of step (2) heats 60min to utilize sunshine optically focused at 600 DEG C.The carbon fiber obtained after treatment There is obvious indenture in surface, illustrates that with this understanding, carbon fiber surface has been destroyed, and the carbon fiber of recovery loses original The structure come, has no actual application value.
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. it is a kind of from waste and old carbon fibre reinforced composite reclaim carbon fiber method, it is characterised in that by the carbon fiber After enhancing composite pretreatment, the heating of 70~110min is carried out at 400~500 DEG C, gained solid product is Carbon fiber after recovery.
2. method according to claim 1, it is characterised in that the heating be heating 80 at 420~470 DEG C~ 100min。
3. method according to claim 1 and 2, it is characterised in that the heating is to heat 85 at 440~460 DEG C ~95min.
4. the method according to any one of claims 1 to 3, it is characterised in that the heating is to heat at 450 DEG C 90min。
5. the method according to any one of Claims 1 to 4, it is characterised in that the pretreatment is:The carbon fiber is increased After strong composite cutting, it is put into immersion in absolute ethyl alcohol and is then dried with removing surface impurity for 1.5~2.5 hours.
6. method according to claim 5, it is characterised in that described to be cut into:By the carbon fibre reinforced composite Cut into the segment of 0.15~0.25m × 0.15~0.25m.
7. the method according to claim 5 or 6, it is characterised in that it is described be put into time for being soaked in absolute ethyl alcohol for 2~ 2.5 hours.
8. the method according to any one of claim 1~7, it is characterised in that the mode of the heating is sunshine optically focused Heating.
9. the method according to any one of claim 1~8, it is characterised in that comprise the following steps:
(1) pre-process:The carbon fibre reinforced composite is cut into the segment of 0.15~0.25m × 0.15~0.25m, is put Enter immersion in absolute ethyl alcohol then to be dried to remove surface impurity for 2~2.5 hours;
(2) heat:Carbon fibre reinforced composite after step (1) treatment is added at 450 DEG C using sunshine optically focused Hot 90min, gained solid product is the carbon fiber after reclaiming.
10. the method according to any one of claim 1~9, it is characterised in that the base of the carbon fibre reinforced composite Body is thermosetting resin.
CN201611247331.0A 2016-12-29 2016-12-29 A method of recycling carbon fiber from waste and old carbon fibre reinforced composite Active CN106810711B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019153217A1 (en) * 2018-02-09 2019-08-15 深圳大学 Method for recovering high-performance carbon fiber from inorganic cementing material
CN111004401A (en) * 2019-12-04 2020-04-14 安徽旭升新材料有限公司 Carbon fiber-PA 66 composite material for shoe sole and processing method thereof
CN111196879A (en) * 2018-11-19 2020-05-26 航天特种材料及工艺技术研究所 Method for recovering carbon fibers from carbon fiber reinforced thermosetting resin-based composite material
CN114618874A (en) * 2022-04-01 2022-06-14 四川优比贝柠科技有限公司 Secondary recovery process for waste of thermal insulation material
CN116277616A (en) * 2023-03-03 2023-06-23 南京航空航天大学 Space recycling remanufacturing method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5292408A (en) * 1990-06-19 1994-03-08 Osaka Gas Company Limited Pitch-based high-modulus carbon fibers and method of producing same
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
CN103897213A (en) * 2014-04-10 2014-07-02 合肥工业大学 Recovery method of carbon-fiber reinforced resin-base composite material with pretreatment modes

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5292408A (en) * 1990-06-19 1994-03-08 Osaka Gas Company Limited Pitch-based high-modulus carbon fibers and method of producing same
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
CN103897213A (en) * 2014-04-10 2014-07-02 合肥工业大学 Recovery method of carbon-fiber reinforced resin-base composite material with pretreatment modes

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019153217A1 (en) * 2018-02-09 2019-08-15 深圳大学 Method for recovering high-performance carbon fiber from inorganic cementing material
CN111196879A (en) * 2018-11-19 2020-05-26 航天特种材料及工艺技术研究所 Method for recovering carbon fibers from carbon fiber reinforced thermosetting resin-based composite material
CN111004401A (en) * 2019-12-04 2020-04-14 安徽旭升新材料有限公司 Carbon fiber-PA 66 composite material for shoe sole and processing method thereof
CN114618874A (en) * 2022-04-01 2022-06-14 四川优比贝柠科技有限公司 Secondary recovery process for waste of thermal insulation material
CN116277616A (en) * 2023-03-03 2023-06-23 南京航空航天大学 Space recycling remanufacturing method
CN116277616B (en) * 2023-03-03 2024-05-17 南京航空航天大学 Space recycling remanufacturing method

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