CN104592546A - Method for recycling waste carbon fiber/epoxy resin composite material - Google Patents
Method for recycling waste carbon fiber/epoxy resin composite material Download PDFInfo
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- CN104592546A CN104592546A CN201410834413.XA CN201410834413A CN104592546A CN 104592546 A CN104592546 A CN 104592546A CN 201410834413 A CN201410834413 A CN 201410834413A CN 104592546 A CN104592546 A CN 104592546A
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- epoxy resin
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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
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/16—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with inorganic material
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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
- C08J2300/00—Characterised by the use of unspecified polymers
- C08J2300/24—Thermosetting 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
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- 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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- Life Sciences & Earth Sciences (AREA)
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention provides a method for recycling a waste carbon fiber/epoxy resin composite material. The method for recycling the waste carbon fiber/epoxy resin composite material comprises one step of recycling the waste carbon fiber/epoxy resin composite material by utilizing a solvent method combined with a pressure method, only one step is needed in the whole process, the waste carbon fiber/epoxy resin composite material is treated at high temperature and high pressure by utilizing composite acid of inorganic acid and organic acid, a mixed solvent of organic solvents and a compound oxidizing agent, and separation is carried out, so that carbon fibers with no significant defects on surfaces and an extremely small amount of residual resin are obtained. The method for recycling the waste carbon fiber/epoxy resin composite material comprises a simple and effective step and is clean and environment-friendly.
Description
Technical field
The invention belongs to polymer recovery technology field, relate to a kind of method reclaiming same with thermosetting compound material, in particular a kind of solvent method combination pressure method reclaims the method for waste and old carbon fiber/epoxy resin composite material.
Background technology
Carbon fiber/epoxy resin composite material is widely used in multiple fields such as national defence, military project, aerospace, building, communications and transportation and the energy, and be constantly extended to emerging field, such as: in hydrogen storage method, high pressure full wound composite cylinder is the selection that application is the most general at present.Along with such matrix material is the increasing rapidly of application of these high frontiers, the junk produced grows with each passing day, but the recovery and reuse present situation of carbon fiber epoxy based composites is allowed of no optimist, if not carrying out reclaiming brings huge pollution by environment.In addition, containing a large amount of expensive carbon fiber in carbon fiber/epoxy resin composite material, the recycling work carrying out waste and old CF/EP matrix material has larger economic implications, and it reclaims renewable resources and attracts attention gradually.
At present, traditional both at home and abroad process same with thermosetting compound material has following three kinds of approach:
(1) Material Physics is pulverized, and its waste material reclaimed is included in the matrix material of a new generation;
(2) chemical recovery (such as passing through pyrolysis), wherein the recovery of polymkeric substance is as organic compound, then can be used as a kind of chemical raw material;
(3) energy recovery, makes the calorie in matrix material be effectively utilized by the mode of burning.Wherein the main method of conventional process carbon-fibre reinforced epoxy resin waste is buried and burns, mechanical disintegration absorption method.Attempt pyrolysis method, degrading solvent method (such as: cured resin can dissolve in organic solvent by acid treatment, the people such as Dang find that bisphenol F epoxy resin can decompose completely in salpeter solution, and the product of decomposition and epoxy resin and solidifying agent repolymerization generate regenerating resin) etc.
It is loaded down with trivial details to there is technique in above-mentioned three kinds of methods, and return period is longer, high energy consumption, and the carbon fiber of recovery exists the shortcomings such as length is less, surface residue is more, performance loss is larger.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of solvent method combination pressure method to reclaim the method for waste and old carbon fiber/epoxy resin composite material, the method one step completes, and can overcome above-mentioned the deficiencies in the prior art.
The present invention solves its technical problem and adopts following technical scheme:
The method of the waste and old carbon fiber/epoxy resin composite material of recovery provided by the invention, that one utilizes solvent method combination pressure method to reclaim waste and old carbon fiber/epoxy resin composite material, whole process only needs a step, with the combination solvent of mineral acid and organic acid composite acid, organic solvent and combine oxygenant and process waste and old carbon fiber/epoxy resin composite material at high temperature under high pressure, obtain separable carbon fiber and degradation solution.
The method of the waste and old carbon fiber/epoxy resin composite material of described recovery, comprises the following steps:
(1) waste and old carbon fiber/epoxy resin composite material is cut into suitable size, for subsequent use;
(2) put into reactor, add mineral acid and organic acid composite acid, organic solvent combination solvent and combine oxygenant, temperature be 80-180 DEG C, pressure heats 1.0-2.5h under being 1.0-1.4Mp;
(3) whizzer separation of carbon fiber and solution is utilized;
(4) carbon fiber washing, drying are recycled product.
In step (1), in described waste and old carbon fiber/epoxy resin composite material, reinforcement carbon fiber is the one in PAN base carbon fibre, viscose base carbon fibre, asphalt base carbon fiber.
In step (1), in described waste and old carbon fiber/epoxy resin composite material, substrate ring epoxy resins adopts the one in glycidyl ether type epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, linear aliphatic same clan epoxy resin, finger ring same clan epoxy resin.
In step (1), in described waste and old carbon fiber/epoxy resin composite material, solidifying agent is adopted to carry out crosslinking curing to substrate ring epoxy resins, this solidifying agent adopts diethylenetriamine, triethylene tetramine, polyethylene polyamine, N, one in N-diethylaminopropylamine, polyetheramine, polymeric amide, or several mixtures.
In step (2), described mineral acid adopts the one in nitric acid, phosphoric acid, hydrochloric acid, sulfuric acid.
In step (2), described organic acid adopts the one in carboxylic acid, sulfonic acid,-sulfinic acid, thionothiolic acid.
In step (2), the combination solvent of described organic solvent adopt in toluene, dimethylbenzene, acetone, ethers, alcohols two or more.
In step (2), described combination oxygenant adopt in hydrogen peroxide, nitrate, many nitro-compounds, potassium permanganate two or more.
The recovery product that the inventive method obtains, the degradation rate of its epoxy resin is >=90%.
The present invention adopts solvent method combination pressure method to reclaim the method for waste and old carbon fiber/epoxy resin composite material, has following advantage compared with traditional additive method:
1. the recovery waste and old carbon fiber/epoxy resin composite material treatment time is short, efficiency is high, has industrial applications prospect.
2. single stage method completes, and technique is simple.
3. the degradation rate of resin high (can up to more than 90%).
4. reclaiming the carbon fiber strength obtained retains high, surperficial no significant defect.
In a word, the inventive method step is succinct efficient, clean environment firendly, can ensure to be separated the carbon fiber that the cull that obtains surperficial no significant defect is few.
Embodiment
The present invention adopts solvent method combination pressure method, and it is with the combination solvent of mineral acid and organic acid composite acid, organic solvent and combine oxygenant and process waste and old carbon fiber/epoxy resin composite material at high temperature under high pressure, obtains separable carbon fiber and degradation solution.This method adds high pressure on the basis of degrading solvent method, decrease the reaction times, improve degradation effect, the treatment capacity of waste and old matrix material can be increased, (the surface resin degradation rate of the carbon fiber that recovery obtains can reach more than 90% to reclaim more complete carbon fiber, fibre strength is more than 90% of pristine fibre, can with epoxy resin compound again).
Below in conjunction with example, the present invention is further elaborated, but content of the present invention is not only confined to following exemplifying embodiment.
Embodiment 1:
Be cut into by matrix material and be about 9cm, wide about 1.5cm, the square bar that thickness is about 2mm is for subsequent use; Put into 200ml reactor, adding 20ml volume fraction is 70% aqueous acetic acid, 20ml strong phosphoric acid, 20ml acetone, 20ml benzene, 20ml30% hydrogen peroxide, 20g sodium hydrogen phosphate; 180 DEG C, degrade under 1.4Mp 2.5h; Filtering separation carbon fiber and solution, by solid product washing with acetone, then put into the carbon fiber that dry 12h at 80 DEG C, baking oven is recycled.Through test, the degradation rate of epoxy resin is 93.13%.
Embodiment 2:
Be cut into by matrix material and be about 9cm, wide about 1.5cm, the square bar that thickness is about 2mm is for subsequent use; Put into 200ml reactor, adding 20ml volume fraction is 70% aqueous acetic acid, 20m strong phosphoric acid, 20ml dme, 20ml benzene, 20ml30% hydrogen peroxide, 20g SODIUMNITRATE; 180 DEG C, degrade under 1.4Mp 2.5h; Filtering separation carbon fiber and solution, by solid product washing with acetone, then put into the carbon fiber that dry 12h at 80 DEG C, baking oven is recycled.Through test, the degradation rate of epoxy resin is 90.78%.
Embodiment 3:
Be cut into by matrix material and be about 9cm, wide about 1.5cm, the square bar that thickness is about 2mm is for subsequent use; Put into 200ml reactor, adding 20ml volume fraction is 70% aqueous acetic acid, the 20ml vitriol oil, 20ml acetone, 20ml benzene, 20ml30% hydrogen peroxide, 20g SODIUMNITRATE; 120 DEG C, degrade under 1.0Mp 2h; Filtering separation carbon fiber and solution, by solid product washing with acetone, then put into the carbon fiber that dry 12h at 80 DEG C, baking oven is recycled.Through test, the degradation rate of epoxy resin is 88.34%.
Embodiment 4:
Be cut into by matrix material and be about 9cm, wide about 1.5cm, the square bar that thickness is about 2mm is for subsequent use; Put into 200ml reactor, add 20ml concentrated nitric acid, 20ml massfraction is 37% hydrochloric acid, 20ml acetone, 20ml benzene, 20ml30% hydrogen peroxide, 20g sodium hydrogen phosphate; 180 DEG C, degrade under 1.0Mp 1.5h; Filtering separation carbon fiber and solution, by solid product washing with acetone, then put into the carbon fiber that dry 12h at 80 DEG C, baking oven is recycled.Through test, the degradation rate of epoxy resin is 83.89%.
Embodiment 5:
Be cut into by matrix material and be about 9cm, wide about 1.5cm, the square bar that thickness is about 2mm is for subsequent use; Put into 200ml reactor, add that 20ml volume fraction is 70% aqueous acetic acid, 20ml massfraction is 37% hydrochloric acid, 20ml acetone, 20ml dme, 20g SODIUMNITRATE, 20g sodium hydrogen phosphate; 120 DEG C, degrade under 1.0Mp 2h; Filtering separation carbon fiber and solution, by solid product washing with acetone, then put into the carbon fiber that dry 12h at 80 DEG C, baking oven is recycled.Through test, the degradation rate of epoxy resin is 83.67%.
Claims (10)
1. one kind is reclaimed the method for waste and old carbon fiber/epoxy resin composite material, it is characterized in that one utilizes solvent method combination pressure method to reclaim waste and old carbon fiber/epoxy resin composite material, whole process only needs a step, with the combination solvent of mineral acid and organic acid composite acid, organic solvent and combine oxygenant and process waste and old carbon fiber/epoxy resin composite material at high temperature under high pressure, obtain separable carbon fiber and degradation solution.
2. method according to claim 1, is characterized in that comprising the following steps:
(1) waste and old carbon fiber/epoxy resin composite material is cut into suitable size, for subsequent use;
(2) put into reactor, add mineral acid and organic acid composite acid, organic solvent combination solvent and combine oxygenant, temperature be 80-180 DEG C, pressure heats 1.0-2.5h under being 1.0-1.4Mp;
(3) whizzer separation of carbon fiber and solution is utilized;
(4) carbon fiber washing, drying are recycled product.
3. method according to claim 2, is characterized in that in described waste and old carbon fiber/epoxy resin composite material, and reinforcement carbon fiber is the one in PAN base carbon fibre, viscose base carbon fibre, asphalt base carbon fiber.
4. method according to claim 2, it is characterized in that in described waste and old carbon fiber/epoxy resin composite material, substrate ring epoxy resins adopts the one in glycidyl ether type epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, linear aliphatic same clan epoxy resin, finger ring same clan epoxy resin.
5. method according to claim 2, it is characterized in that in described waste and old carbon fiber/epoxy resin composite material, solidifying agent is adopted to carry out crosslinking curing to substrate ring epoxy resins, this solidifying agent adopts diethylenetriamine, triethylene tetramine, polyethylene polyamine, N, one in N-diethylaminopropylamine, polyetheramine, polymeric amide, or several mixtures.
6. method according to claim 2, is characterized in that in step (2), and described mineral acid adopts the one in nitric acid, phosphoric acid, hydrochloric acid, sulfuric acid.
7. method according to claim 2, is characterized in that in step (2), and described organic acid adopts the one in carboxylic acid, sulfonic acid,-sulfinic acid, thionothiolic acid.
8. method according to claim 2, is characterized in that in step (2), the combination solvent of described organic solvent adopt in toluene, dimethylbenzene, acetone, ethers, alcohols two or more.
9. method according to claim 2, is characterized in that in step (2), described combination oxygenant adopt in hydrogen peroxide, nitrate, many nitro-compounds, potassium permanganate two or more.
10. method according to claim 2, is characterized in that obtained recovery product, and the degradation rate of its epoxy resin is >=90%.
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| CN104592546B CN104592546B (en) | 2018-04-27 |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2016177305A1 (en) * | 2015-05-01 | 2016-11-10 | Adesso Advanced Materials Wuxi Co., Ltd. | Methods for degrading and recycling cross-linked polymers and reinforced polymer composites |
| EP3178874A1 (en) * | 2015-12-11 | 2017-06-14 | Korea Institute of Science and Technology | Method and apparatus for recovering fiber assembly from thermosetting resin composite materials and recovered fiber assembly thereby |
| CN107082582A (en) * | 2016-02-15 | 2017-08-22 | 山东理工大学 | A kind of method that fiberglass fibers waste silk prepares electroconductive glass fibre |
| CN107082557A (en) * | 2016-02-15 | 2017-08-22 | 山东理工大学 | A kind of glass fibre reinforced composion castoff regenerative glass fibre method |
| CN107082626A (en) * | 2016-02-15 | 2017-08-22 | 山东理工大学 | A kind of method for comprehensively utilizing carbon fibre reinforced composite and red mud discarded object |
| CN107082581A (en) * | 2016-02-15 | 2017-08-22 | 山东理工大学 | A kind of method of glass fiber waste silk or product normal temperature and pressure repeat glass fiber |
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