CN106750507A - A kind of recovery method of carbon fiber enhancement resin base composite material - Google Patents
A kind of recovery method of carbon fiber enhancement resin base composite material Download PDFInfo
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- CN106750507A CN106750507A CN201710010761.9A CN201710010761A CN106750507A CN 106750507 A CN106750507 A CN 106750507A CN 201710010761 A CN201710010761 A CN 201710010761A CN 106750507 A CN106750507 A CN 106750507A
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- carbon fiber
- composite material
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- base composite
- fiber enhancement
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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
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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
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/20—Recycled plastic
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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)
- Reinforced Plastic Materials (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
The present invention relates to a kind of recovery method of carbon fiber enhancement resin base composite material, including：Discarded carbon fiber enhancement resin base composite material is cut into tabular, carbon fiber enhancement resin base composite material plate is obtained, the resin for then processing the end surfaces of composite panel two for obtaining is exposed to carbon fiber；Then under conditions of ultrasound-enhanced or microwave reinforced, burin-in process is carried out in the electrolytic solution；Exposed carbon fiber in the carbon fiber enhancement resin base composite material plate that burin-in process is obtained is connected with the anode of dc source, and graphite rod is connected with the negative electrode of dc source, is electrochemically reacted in the electrolytic solution, obtains carbon fiber, cleaning, dries, you can.The method of the present invention improves the organic efficiency of carbon fiber, and removal process is to environment non-secondary pollution and the carbon fiber mechanical property of recovery damages small.
Description
Technical field
The invention belongs to the recovery and reusing and recycling field of fibre reinforced composites, more particularly to a kind of fibre reinforced tree
The recovery method of resin-based composite.
Background technology
Carbon fiber enhancement resin base composite material has specific strength and specific modulus high, physical dimension stabilization and corrosion resistance
Can be good the advantages of, the fields such as space flight and aviation, the vehicles, electronics industry are widely used at present.Currently, fibre reinforced tree
Just in rapid growth, it has more the consumption of resin-based composite at aspects such as national defense safety, national economy and daily lifes
Important effect.
Although carbon fiber enhancement resin base composite material has the advantages that numerous, due to carbon fiber non-degradable, reaching
To service life and after the update cycle, a large amount of discarded carbon fiber enhancement resin base composite material products are dirty due to being produced to environment
Contaminate and urgently process.
The recovery method of current carbon fiber enhancement resin base composite material mainly has：Mechanical absorption method, supercritical methanol technology, hot tearing
Solution, strong acid decomposition method etc..Mechanical absorption method is that composite is crushed in the presence of mechanical force, between destruction fiber and resin
Interface binding power so that fiber is stripped out from cross-linked structure, but the carbon fiber surface for obtaining has substantial amounts of residue,
And the mechanical property of fiber damages larger.
Chinese patent CN103333360A (publication date is on October 2nd, 2013) discloses a kind of supercritical methanol technology and reclaims carbon
Carbon fiber enhancement resin base composite material after treatment is put into supercharging by the method for fiber-reinforced resin matrix compound material, the method
CO is full of to 5~30MPa2Reactor in, and the temperature in reactor is heated to 50 DEG C~500 DEG C, there is resin super
Critical reaction and decompose the carbon fiber so as to be recycled.The advantage of the method is that the resolution ratio of resin matrix is more than 95%, is obtained
The carbon fiber mechanical property loss arrived is less than 5%, and surface does not have residuals substantially.Have the disadvantage needs in the anti-of HTHP
Carried out under the conditions of answering, the requirement to consersion unit is higher, it is difficult to industrialize.
Chinese patent CN103665427A (publication date is on March 26th, 2014) discloses a kind of carbon fiber-reinforced resin
Carbon fiber enhancement resin base composite material is placed on 350 DEG C~900 DEG C by based composites thermal cracking recovery method, the method
Under high temperature anaerobic inert environments so that resin matrix occurs heat scission reaction, finally gives carbon fiber.The advantage of the method is to carry
The organic efficiency of carbon fiber high, reduces to reclaim the carbon fiber surface for obtaining and easily tie the phenomenon of carbon and is obtained so as to improve recovery
Carbon fiber mechanical property.Have the disadvantage the inert environments of the anaerobic under needing high temperature and nitrogen to protect, energy consumption is larger, is difficult industry
Change.Carbon fiber surface knot carbon phenomenon, carbon fiber mechanical property can not completely be avoided also certain decline.
Chinese patent CN1483754A (publication date is on March 24th, 2004) is disclosed a kind of decomposition using strong acid and discarded
The method of carbon fiber enhancement resin base composite material, the method by carbon fiber enhancement resin base composite material be put into 2mol/L~
In the salpeter solution of 8mol/L, being heated to 70 DEG C~90 DEG C makes resin decompose at ambient pressure, so as to reclaim obtain carbon fiber.The party
The advantage of method is no high-temperature and high-pressure conditions, and technological process is simple, and decomposition efficiency is high, and recovery obtains the clean carbon fiber in surface.
Have the disadvantage：The corrosivity of strong acid is higher, and the requirement to equipment is high, and the safety coefficient requirement to operating is higher, and rear reaction treatment is difficult,
It is big for environment pollution.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of recovery method of carbon fiber enhancement resin base composite material,
The shortcomings of the method overcomes the big pollution existing for existing recovery technology, high energy consumption, low recovery carbon fiber mechanical property.
A kind of recovery method of carbon fiber enhancement resin base composite material of the invention, including：
(1) discarded carbon fiber enhancement resin base composite material is cut into tabular, obtains carbon fiber enhancement resin base and be combined
Plate of material, the resin for then processing the end surfaces of composite panel two for obtaining is exposed to carbon fiber；
(2) the carbon fiber enhancement resin base composite material plate for obtaining treatment in step (1) is strong in ultrasound-enhanced or microwave
Under conditions of change, burin-in process is carried out in the electrolytic solution；
(3) the exposed carbon fiber in the carbon fiber enhancement resin base composite material plate for obtaining burin-in process in step (2)
It is connected with the anode of dc source, graphite rod is connected with the negative electrode of dc source, connects power supply, electrochemistry is carried out in the electrolytic solution
Reaction, obtains carbon fiber, cleans, and dries, you can.
Resin is phenolic resin, epoxy resin, maleic acid resin, makrolon, poly terephthalic acid in the step (1)
Butanediol ester or PET.
The resin can select thermosetting resin or thermoplastic resin.
The thickness of carbon fiber enhancement resin base composite material plate is 2~4mm in the step (1)；The exposed length of carbon fiber
It is 1~2cm to spend.
The method for the treatment of is in the step (1)：Use sand papering；Wherein, sand paper is Brown Alundum sand paper, white fused alumina sand paper
Or carborundum paper, preferred carborundum paper.
Ultrasound-enhanced condition is in the step (2)：Frequency range is 15KHz~60KHz, and sound pressure amplitudes virtual value is
2~26Mpa, ultrasound change turns to sinusoidal variations；Microwave reinforced condition is：Wave-length coverage is 1mm~1000mm, and frequency is
300MHz~30GHz, power is 30~600W.
The condition of burin-in process is in institute's step (2)：By the carbon fibre composite plate after polishing temperature be 70 DEG C~
20h-40h is soaked in 90 DEG C of electrolyte, 1h-2h is placed under conditions of being then -30 DEG C~-20 DEG C in temperature, placed afterwards
Temperature be 100 DEG C~120 DEG C, humidity be 60~90% environment in 4h-8h.
The burin-in process is repeated 4~8 times.
Electrolyte is molten sodium nitrate solution, potassium nitrate solution, potassium sulfate solution, sodium sulphate in institute's step (2) and step (3)
Liquid, sodium chloride solution or Klorvess Liquid, the solution concentration are 5~30wt%, and solvent is water.
The condition of electrochemical reaction is in institute's step (3)：Current density is 10~20A/m2。
Cleaning is to carry out ultrasonic vibration with distilled water to clean in the step (3)；Wherein, the condition of ultrasonic vibration is：
20KHz~80KHz, the time is 30min~60min；Dry condition is：80~95 DEG C (in baking ovens) dry 1~2h.
Beneficial effect
(1) method of the present invention improves the recovery effect of carbon fiber without all of resin matrix in degrading composite
Rate, has saved substantial amounts of electric energy；
(2) electrolyte used in the method for the present invention is green cleanliness without any pollution solution, and wide material sources, and price is just
Preferably, removal process is to environment non-secondary pollution；
(3) the carbon fiber mechanical property for obtaining that the method for the present invention is reclaimed damages small.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
(1) discarded carbon-fibre reinforced epoxy resin composite material is cut into the carbon-fibre reinforced epoxy that thickness is 2mm
Resin composite material plate.
(2) with the resin of the carborundum paper polishing end surfaces of composite panel two, the carbon fiber at composite panel two ends is made
Exposed 2cm.
(3) it is 25KHz in ultrasonic frequency, sound pressure amplitudes virtual value is for (ultrasound change is turned to just under the intensified condition of 20MPa
String change), by the carbon-fibre reinforced epoxy resin composite material plate after polishing temperature be 90 DEG C, concentration for 10wt% NaCl
20h is soaked in electrolyte, then 1h is placed in the low temperature environment that temperature is -30 DEG C, temperature is placed on afterwards for 100 DEG C, it is wet
Spend 4h in the high temperature hygrothermal environment for 80%.
(4) repeat step (3) 5 times.
(5) by carbon fiber and dc source exposed in the carbon-fibre reinforced epoxy resin composite material plate after burin-in process
Anode be connected, graphite rod is connected with the negative electrode of dc source, be placed in concentration for 20wt% NaCl solution in, formation electrochemistry
Reaction system.Connection power supply, control electric current density is 10A/m2So that as the carbon fiber enhancement resin base composite material of anode
Generation electrochemical reaction obtains carbon fiber, the electrochemical reaction time for be reacted to carbon fiber surface without resin bonding and can naturally from
Come off in resin matrix, reaction can terminate.
(6) ultrasound is first carried out under conditions of supersonic frequency is 40KHz with distilled water to the carbon fiber after electrochemical reaction
, then be put into the carbon fiber after ultrasonic vibration in the baking oven that setting temperature is 95 DEG C and dry 1 hour, so as to reclaim by concussion cleaning
Obtain the clean carbon fiber in surface.
Embodiment 2
(1) fibre reinforced PET composite is cut into the fibre reinforced that thickness is 3mm to gather
PETP composite panel.
(2) resin of the end surfaces of composite panel two is ground off with white fused alumina sand paper, makes the carbon fiber at composite panel two ends
Exposed 1cm.
(3) be 50mm in wave-length coverage, frequency is 2GHz, power for 300W it is microwave reinforced under the conditions of, after polishing
Fibre reinforced PET composite panel is 70 DEG C in temperature, and concentration is in the potassium nitrate solution of 15wt%
Immersion 30h, then places 2h in the low temperature environment that temperature is -20 DEG C, is afterwards 110 DEG C in temperature, and humidity is 70% height
5h is processed in warm and humid thermal environment.
(4) repeat step (3) 7 times.
(5) carbon fiber exposed in the carbon fibre composite plate after burin-in process is connected with the anode of dc source,
Graphite rod is connected with the negative electrode of dc source, is placed in the potassium nitrate solution that concentration is 30wt%, forms electrochemical reaction system.
Connection power supply, control electric current density is 20A/m2So that there is electrochemistry as the carbon fiber enhancement resin base composite material of anode
Reaction obtains carbon fiber, and the electrochemical reaction time is to be reacted to carbon fiber surface without resin bonding and can naturally from resin matrix
Come off, reaction can terminate.
(6) ultrasound is first carried out under conditions of supersonic frequency is 40KHz with distilled water to the carbon fiber after electrochemical reaction
, then be put into the carbon fiber after ultrasonic vibration in the baking oven that setting temperature is 80 DEG C and dry 2 hours, so as to reclaim by concussion cleaning
Obtain the clean carbon fiber in surface.
Claims (10)
1. a kind of recovery method of carbon fiber enhancement resin base composite material, including：
(1) discarded carbon fiber enhancement resin base composite material is cut into tabular, obtains carbon fiber enhancement resin base composite material
Plate, the resin for then processing the end surfaces of composite panel two for obtaining is exposed to carbon fiber；
(2) the carbon fiber enhancement resin base composite material plate for obtaining treatment in step (1) is ultrasound-enhanced or microwave reinforced
Under the conditions of, burin-in process is carried out in the electrolytic solution；
(3) the exposed carbon fiber in the carbon fiber enhancement resin base composite material plate for obtaining burin-in process in step (2) with it is straight
The anode for flowing power supply is connected, and graphite rod is connected with the negative electrode of dc source, is electrochemically reacted in the electrolytic solution, obtains carbon fine
Dimension, cleaning is dried, you can.
2. a kind of recovery method of carbon fiber enhancement resin base composite material according to claim 1, it is characterised in that institute
State resin in step (1) be phenolic resin, epoxy resin, maleic acid resin, makrolon, polybutylene terephthalate (PBT) or
PET.
3. a kind of recovery method of carbon fiber enhancement resin base composite material according to claim 1, it is characterised in that institute
The thickness for stating carbon fiber enhancement resin base composite material plate in step (1) is 2~4mm；The exposed length of carbon fiber is 1~2cm.
4. a kind of recovery method of carbon fiber enhancement resin base composite material according to claim 1, it is characterised in that institute
Stating the method processed in step (1) is：Use sand papering；Wherein, sand paper is Brown Alundum sand paper, white fused alumina sand paper or silicon carbide sand
Paper.
5. a kind of recovery method of carbon fiber enhancement resin base composite material according to claim 1, it is characterised in that institute
Stating ultrasound-enhanced condition in step (2) is：Frequency range is 15KHz~60KHz, and sound pressure amplitudes virtual value is 2~26Mpa,
Ultrasound change turns to sinusoidal variations；Microwave reinforced condition is：Wave-length coverage be 1mm~1000mm, frequency be 300MHz~
30GHz, power is 30~600W.
6. a kind of recovery method of carbon fiber enhancement resin base composite material according to claim 1, it is characterised in that institute
The condition for stating burin-in process in step (2) is：20h-40h is soaked in the electrolyte that temperature is 70 DEG C~90 DEG C, then in temperature
Spend to place 1h-2h under conditions of -30 DEG C~-20 DEG C, it is 100 DEG C~120 DEG C that temperature is placed on afterwards, and humidity is 60~90%
Environment in 4h-8h.
7. a kind of recovery method of carbon fiber enhancement resin base composite material according to claim 6, it is characterised in that institute
Burin-in process is stated to repeat 4~8 times.
8. a kind of recovery method of carbon fiber enhancement resin base composite material according to claim 1, it is characterised in that institute
Electrolyte is sodium nitrate solution, potassium nitrate solution, potassium sulfate solution, metabisulfite solution, chlorination in stating step (2) and step (3)
Sodium solution or Klorvess Liquid, the solution concentration are 5~30wt%, and solvent is water.
9. a kind of recovery method of carbon fiber enhancement resin base composite material according to claim 1, it is characterised in that institute
The condition for stating electrochemical reaction in step (3) is：Current density is 10~20A/m2。
10. the recovery method of a kind of carbon fiber enhancement resin base composite material according to claim 1, it is characterised in that
Cleaning is to carry out ultrasonic vibration with distilled water to clean in the step (3)；Wherein, the condition of ultrasonic vibration is：20KHz~
80KHz, the time is 30min~60min；Dry condition is：80~95 DEG C of 1~2h of drying.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108323169A (en) * | 2018-02-09 | 2018-07-24 | 深圳大学 | The lossless fibre reinforced composites recovery method of environmental protection |
| CN109153051A (en) * | 2018-02-09 | 2019-01-04 | 深圳大学 | The method of high-performance carbon fibre is recycled from inorganic coagulation material |
| CN109485912A (en) * | 2018-11-09 | 2019-03-19 | 深圳大学 | A kind of the electricity promotion heterocatalysis device and its control method of recycling CFRP |
| WO2020093700A1 (en) * | 2018-11-09 | 2020-05-14 | 深圳大学 | Cfrp material-based electrically-promoted heterogeneous catalysis and recovery apparatus and control method therefor |
| CN113736138A (en) * | 2021-08-24 | 2021-12-03 | 同济大学 | Recycling method of fiber reinforced composite material |
| CN114773667A (en) * | 2022-04-27 | 2022-07-22 | 北京化工大学 | Method for recycling wind power blade under mild condition by using transition metal catalyst |
| GB2615837A (en) * | 2022-03-15 | 2023-08-23 | Mdf Recovery Ltd | Method and apparatus for recovering fibres |
| TWI859709B (en) | 2022-03-31 | 2024-10-21 | 法國商費爾麥特公司 | Recycled composite material fragments and manufacturing method thereof |
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| 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 |
| CN104499039A (en) * | 2014-12-09 | 2015-04-08 | 深圳大学 | Recovery method of carbon fibers |
| CN105906836A (en) * | 2016-05-09 | 2016-08-31 | 西北工业大学 | Recovering method of carbon fiber reinforced resin matrix composite material under mild conditions |
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Patent Citations (3)
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| 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 |
| CN104499039A (en) * | 2014-12-09 | 2015-04-08 | 深圳大学 | Recovery method of carbon fibers |
| CN105906836A (en) * | 2016-05-09 | 2016-08-31 | 西北工业大学 | Recovering method of carbon fiber reinforced resin matrix composite material under mild conditions |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019153218A1 (en) * | 2018-02-09 | 2019-08-15 | 深圳大学 | Environmentally friendly non-destructive fiber-reinforced composite material recovering method |
| CN109153051A (en) * | 2018-02-09 | 2019-01-04 | 深圳大学 | The method of high-performance carbon fibre is recycled from inorganic coagulation material |
| CN108323169A (en) * | 2018-02-09 | 2018-07-24 | 深圳大学 | The lossless fibre reinforced composites recovery method of environmental protection |
| WO2019153217A1 (en) * | 2018-02-09 | 2019-08-15 | 深圳大学 | Method for recovering high-performance carbon fiber from inorganic cementing material |
| WO2020093700A1 (en) * | 2018-11-09 | 2020-05-14 | 深圳大学 | Cfrp material-based electrically-promoted heterogeneous catalysis and recovery apparatus and control method therefor |
| WO2020093503A1 (en) * | 2018-11-09 | 2020-05-14 | 深圳大学 | Electrically promoted heterogeneous catalytic device for recovering cfrp and control method thereof |
| CN109485912A (en) * | 2018-11-09 | 2019-03-19 | 深圳大学 | A kind of the electricity promotion heterocatalysis device and its control method of recycling CFRP |
| CN113736138A (en) * | 2021-08-24 | 2021-12-03 | 同济大学 | Recycling method of fiber reinforced composite material |
| CN113736138B (en) * | 2021-08-24 | 2022-04-12 | 同济大学 | Recycling method of fiber reinforced composite material |
| GB2615837A (en) * | 2022-03-15 | 2023-08-23 | Mdf Recovery Ltd | Method and apparatus for recovering fibres |
| GB2615837B (en) * | 2022-03-15 | 2024-07-24 | Mdf Recovery Ltd | Method and apparatus for recovering fibres |
| TWI859709B (en) | 2022-03-31 | 2024-10-21 | 法國商費爾麥特公司 | Recycled composite material fragments and manufacturing method thereof |
| CN114773667A (en) * | 2022-04-27 | 2022-07-22 | 北京化工大学 | Method for recycling wind power blade under mild condition by using transition metal catalyst |
| CN114773667B (en) * | 2022-04-27 | 2023-06-13 | 北京化工大学 | Method for recycling wind power blade under mild condition by using transition metal catalyst |
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