CN106810711B - A method of recycling carbon fiber from waste and old carbon fibre reinforced composite - Google Patents
A method of recycling carbon fiber from waste and old carbon fibre reinforced composite Download PDFInfo
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- CN106810711B CN106810711B CN201611247331.0A CN201611247331A CN106810711B CN 106810711 B CN106810711 B CN 106810711B CN 201611247331 A CN201611247331 A CN 201611247331A CN 106810711 B CN106810711 B CN 106810711B
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- reinforced composite
- fibre reinforced
- carbon fibre
- carbon fiber
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
Abstract
The present invention relates to the recycling of carbon fibre material more particularly to a kind of methods that carbon fiber is recycled from waste and old carbon fibre reinforced composite.The method that carbon fiber is recycled from waste and old carbon fibre reinforced composite are as follows: after carbon fibre reinforced composite pretreatment, the heat treatment of 70~110min is carried out at 400~500 DEG C, gained solid product is carbon fiber after the recovery.The method of the invention simple process, step is few, low energy consumption, it is smooth to recycle obtained carbon fiber surface, it has excellent performance, purity is high, and substantially increases the rate of recovery, in waste and old carbon fibre reinforced composite field, especially there is important application and popularization value in the waste and old carbon fibre reinforced composite recycling field of retired aircraft.
Description
Technical field
The present invention relates to the recycling of carbon fibre material, more particularly to one kind to recycle from waste and old carbon fibre reinforced composite
The method of carbon fiber.
Background technique
The great demand of China's retired aircraft in need of immediate treatment at present.Ended for the end of the year 2015, is flying 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 gradually will scrap and be recycled.It can be seen that it is retired that processing will be present in the Chinese or even whole world in coming few decades
The constant demand of aircraft.Carbon fiber (carbon fiber, abbreviation CF) is a kind of high intensity 95% or more of phosphorus content, height
The new fiber materials of modulus fibre.Carbon fiber has many excellent performances, and the axial strength and modulus of carbon fiber are high, density
Low, good corrosion resistance higher than performance, good electrical and thermal conductivity performance, electromagnetic wave shielding are good etc..
And as carbon fibre reinforced composite (the Carbon fiber for being applied to the military industry fields such as aircraft manufacturing
Reinforced polymer composites, abbreviation CFRP) recycling can achieve save resource and the energy mesh
's.Composite material recovery technology is commercialized maximum obstruction and is the market demand scarcity of regrown material, high remanufacture
The reduction of cost and regrown material performance.Currently, the composite material recovery technology of fibre reinforced includes the following three types: mechanical
Recycling, recuperation of heat and chemical recovery.
As a kind of method for recycling carbon fibre material, recuperation of heat has with low power consuming, processing capacity is strong, the rate of recovery is high
Etc. incomparable advantage, if but control the technological parameter of bad recuperation of heat method, can machinery to the carbon fiber being recovered to it is strong
Degree damages.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides one kind to recycle carbon from waste and old carbon fibre reinforced composite
The method of fiber, it may be assumed that after carbon fibre reinforced composite pretreatment, carry out 70~110min's at 400~500 DEG C
Heat treatment, gained solid product is carbon fiber after the recovery.The carbon fiber surface light that the method for the invention recycles
It is sliding, it has excellent performance, purity is high, and substantially increase the rate of recovery.
Preferably, the heat treatment is that 80~100min is heated at 420~470 DEG C.
It is furthermore preferred that the heat treatment is to heat 85~95min at 440~460 DEG C.
Further preferably, the heat treatment is to heat 90min at 450 DEG C.
Preferably, the pretreatment are as follows: after carbon fibre reinforced composite cutting, be put into dehydrated alcohol and impregnate
It to remove surface impurity, then dries within 1.5~2.5 hours.
Further, the cutting are as follows: the carbon fibre reinforced composite is cut into the segment of 0.2m × 0.2m.
It is further, described that be put into time for impregnating in dehydrated alcohol be 2 hours.
Preferably, the mode of the heating is the heating of sunlight optically focused.
The present invention provides a kind of preferred embodiments for recycling carbon fiber comprising following steps:
(1) it pre-processes: it is small that the carbon fibre reinforced composite being cut into 0.15~0.25m × 0.15~0.25m
Section, is put into dehydrated alcohol and impregnates 2~2.5 hours to remove surface impurity, then dry；
(2) heat: step (1) treated carbon fibre reinforced composite is poly- using sunlight at 450 DEG C
Light heats 90min, and gained solid product is carbon fiber after the recovery.
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 for the invention simple process, and step is few, energy
Consume low, the carbon fiber surface recycled is smooth, has excellent performance, purity is high, and substantially increase the rate of recovery.
Detailed description of the invention
Fig. 1 passes through recuperation of heat for the waste and old carbon fibre reinforced composite of the embodiment of the present invention at different temperatures and handles
The TGA figure arrived；
Fig. 2 is at 450 DEG C, and the processing time is respectively the carbon that 60min (A), 90min (B) and 120min (C) are recycled afterwards
The scanning electron microscope (SEM) photograph of fiber；
Fig. 3 is at 450 DEG C, and the processing time is the scanning electron microscope (SEM) photograph of the carbon fiber recycled after 90min.
Specific embodiment
Embodiments of the present invention are described in further detail with reference to the accompanying drawings and examples.Following embodiment is used for
Illustrate the present invention, but cannot be used to limit the scope of the invention.
Waste and old carbon fibre reinforced composite used in the embodiment of the present invention derives from retired aircraft.
Embodiment 1
A method of it recycling carbon fiber from waste and old carbon fibre reinforced composite, includes the following steps:
(1) it pre-processes: the carbon fibre reinforced composite being cut into the segment of 0.2m × 0.2m, is put into dehydrated alcohol
It is middle to impregnate 2 hours to remove surface impurity, then dry；
(2) heat: by step (1), treated that carbon fibre reinforced composite is put on sample treatment platform, 450
90min is heated using sunlight optically focused at DEG C, gained solid product is carbon fiber after the recovery.
Embodiment 2
A method of it recycling carbon fiber from waste and old carbon fibre reinforced composite, includes the following steps:
(1) it pre-processes: the carbon fibre reinforced composite being cut into the segment of 0.2m × 0.25m, is put into anhydrous second
2.5 hours are impregnated in alcohol to remove surface impurity, are then dried；
(2) heat: by step (1), treated that carbon fibre reinforced composite is put on sample treatment platform, 470
95min is heated using sunlight optically focused at DEG C, gained solid product is carbon fiber after the recovery.
Embodiment 3
A method of it recycling carbon fiber from waste and old carbon fibre reinforced composite, includes the following steps:
(1) it pre-processes: the carbon fibre reinforced composite being cut into the segment of 0.15m × 0.15m, is put into anhydrous second
1.5 hours are impregnated in alcohol to remove surface impurity, are then dried；
(2) heat: by step (1), treated that carbon fibre reinforced composite is put on sample treatment platform, 420
100min is heated using sunlight optically focused at DEG C, gained solid product is carbon fiber after the recovery.
As seen from Figure 1, carbon fibre reinforced composite is weightless in 344.1 DEG C of beginnings, and weightlessness is 1.86%.Work as heating
Mass loss 16.80% when to 436.6 DEG C.When being continuously heating to 697.0 DEG C, residual qualities 75.42%.Illustrate the carbon fiber
The pyrolysis temperature section for enhancing composite material is 344.1~436.6 DEG C.The quality for continuing carbon fiber after heating up is kept constant.
By Fig. 2, it can be seen that, the carbon fiber surface that heat treatment 60min is obtained has apparent 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 it is obtained after handling 120min
Carbon fiber surface there is apparent dent (shown in circle), illustrate that with this condition, carbon fiber surface has been destroyed.
By Fig. 3, it can be seen that, the carbon fiber surface obtained after 450 DEG C of processing 90min is smooth, and diameter is 7 μm.
In conclusion the present invention handles 90min at 450 DEG C with the technique that light thermal method recycles carbon fibre reinforced composite
The excellent properties of carbon fiber can be retained.
Comparative example 1
A method of recycling carbon fiber, substantially the same manner as Example 1, area from waste and old carbon fibre reinforced composite
Be not only that: the heat treatment of step (2) is to heat 120min using sunlight optically focused at 350 DEG C.Treated, and carbon fiber increases
Strong composite material surface has a large amount of buildup of resin, does not thoroughly remove the resin of wrap carbon fiber, multiple in fibre reinforced
There was only a small amount of carbon fiber in condensation material surface.
Comparative example 2
A method of recycling carbon fiber, substantially the same manner as Example 1, area from waste and old carbon fibre reinforced composite
Be not only that: the heat treatment of step (2) is to heat 60min using sunlight optically focused at 450 DEG C.The carbon fiber obtained after processing
Surface is smooth, but the resin being present in composite material does not have completely burnout, does not reach recycling carbon fiber material completely
The purpose of material.
Comparative example 3
A method of recycling carbon fiber, substantially the same manner as Example 1, area from waste and old carbon fibre reinforced composite
Be not only that: the heat treatment of step (2) is to heat 60min using sunlight optically focused at 600 DEG C.The carbon fiber obtained after processing
There is apparent dent in surface, illustrates that with this condition, carbon fiber surface has been destroyed, the carbon fiber of recycling loses original
The structure come, has no practical application value.
The embodiment of the present invention is given for the purpose of illustration and description, and is not exhaustively or by this to send out
It is bright to be limited to disclosed form.Many modifications and variations are obvious for the ordinary skill in the art.Choosing
Selecting and describe embodiment is and to make those skilled in the art to more preferably illustrate the principle of the present invention and practical application
It will be appreciated that the present invention is to design various embodiments suitable for specific applications with various modifications.
Claims (9)
1. a kind of method for recycling carbon fiber from waste and old carbon fibre reinforced composite, which is characterized in that by the carbon fiber
After enhancing composite material pretreatment, the heat treatment of 85~95min is carried out at 440~460 DEG C, gained solid product is back
Carbon fiber after receipts；
The mode of the heating is the heating of sunlight optically focused；
The pretreatment are as follows: after carbon fibre reinforced composite cutting, it is small to be put into immersion 1.5~2.5 in dehydrated alcohol
When to remove surface impurity, then dry.
2. the method according to claim 1, wherein the heat treatment is to heat 90min at 450 DEG C.
3. the method according to claim 1, wherein the cutting are as follows: by the carbon fibre reinforced composite
It is cut into 0.15~0.25m × 0.15~0.25m segment.
4. method according to claim 1 or 3, which is characterized in that it is described be put into time for being impregnated in dehydrated alcohol be 2~
2.5 hour.
5. described in any item methods according to claim 1~3, which comprises the steps of:
(1) it pre-processes: the carbon fibre reinforced composite being cut into 0.15~0.25m × 0.15~0.25m segment, is put
Enter to impregnate 2~2.5 hours in dehydrated alcohol to remove surface impurity, then dries；
(2) heat: step (1) treated carbon fibre reinforced composite is added at 450 DEG C using sunlight optically focused
Hot 90min, gained solid product are carbon fiber after the recovery.
6. according to the method described in claim 4, it is characterized by comprising the following steps:
(1) it pre-processes: the carbon fibre reinforced composite being cut into 0.15~0.25m × 0.15~0.25m segment, is put
Enter to impregnate 2~2.5 hours in dehydrated alcohol to remove surface impurity, then dries；
(2) heat: step (1) treated carbon fibre reinforced composite is added at 450 DEG C using sunlight optically focused
Hot 90min, gained solid product are carbon fiber after the recovery.
7. according to claim 1~3 or 6 described in any item methods, which is characterized in that the carbon fibre reinforced composite
Matrix is thermosetting resin.
8. according to the method described in claim 4, it is characterized in that, the matrix of the carbon fibre reinforced composite is thermosetting property
Resin.
9. according to the method described in claim 5, it is characterized in that, the matrix of the carbon fibre reinforced composite is thermosetting property
Resin.
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| CN106810711B true CN106810711B (en) | 2019-09-20 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN114618874B (en) * | 2022-04-01 | 2023-04-11 | 四川优比贝柠科技有限公司 | Secondary recovery process for waste of thermal insulation material |
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 |
| 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 |
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| US5292408A (en) * | 1990-06-19 | 1994-03-08 | Osaka Gas Company Limited | Pitch-based high-modulus carbon fibers and method of producing same |
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| 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 |
| 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 |
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