CN117264416A - CFRP waste carbonized regenerated resin matrix composite material and preparation method thereof - Google Patents
CFRP waste carbonized regenerated resin matrix composite material and preparation method thereof Download PDFInfo
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- CN117264416A CN117264416A CN202311096377.7A CN202311096377A CN117264416A CN 117264416 A CN117264416 A CN 117264416A CN 202311096377 A CN202311096377 A CN 202311096377A CN 117264416 A CN117264416 A CN 117264416A
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- 229920005989 resin Polymers 0.000 title claims abstract description 87
- 239000011347 resin Substances 0.000 title claims abstract description 87
- 239000004918 carbon fiber reinforced polymer Substances 0.000 title claims abstract description 86
- 239000002699 waste material Substances 0.000 title claims abstract description 78
- 239000011159 matrix material Substances 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical group C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 50
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 48
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 42
- 239000004917 carbon fiber Substances 0.000 claims abstract description 42
- 239000003054 catalyst Substances 0.000 claims abstract description 33
- 239000007833 carbon precursor Substances 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 29
- 239000000805 composite resin Substances 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 21
- 238000010000 carbonizing Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000003763 carbonization Methods 0.000 claims abstract description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 37
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- 238000005520 cutting process Methods 0.000 claims description 11
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- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 8
- 239000011701 zinc Substances 0.000 claims description 8
- 239000003822 epoxy resin Substances 0.000 claims description 7
- 229920000647 polyepoxide Polymers 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 6
- 239000013110 organic ligand Substances 0.000 claims description 6
- 238000000197 pyrolysis Methods 0.000 claims description 6
- 230000002194 synthesizing effect Effects 0.000 claims description 6
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
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- 150000003839 salts Chemical class 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical class [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000004952 Polyamide Substances 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 239000004642 Polyimide Substances 0.000 claims description 4
- 239000004743 Polypropylene Substances 0.000 claims description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- WJJMNDUMQPNECX-UHFFFAOYSA-N dipicolinic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=N1 WJJMNDUMQPNECX-UHFFFAOYSA-N 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 229920002647 polyamide Polymers 0.000 claims description 4
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- 229920001721 polyimide Polymers 0.000 claims description 4
- 229920001155 polypropylene Polymers 0.000 claims description 4
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 238000005470 impregnation Methods 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical class [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- MAWKLXRVKVOYLR-UHFFFAOYSA-N 4-(4-pyridin-4-ylphenyl)pyridine Chemical compound C1=NC=CC(C=2C=CC(=CC=2)C=2C=CN=CC=2)=C1 MAWKLXRVKVOYLR-UHFFFAOYSA-N 0.000 claims description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical class [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 2
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 2
- 239000005062 Polybutadiene Substances 0.000 claims description 2
- 239000004695 Polyether sulfone Substances 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000004734 Polyphenylene sulfide Substances 0.000 claims description 2
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 claims description 2
- 239000011651 chromium Chemical class 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Chemical class 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical class [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 238000006731 degradation reaction Methods 0.000 claims description 2
- URKRWCPDFVDQTD-UHFFFAOYSA-N diaminomethanesulfonic acid Chemical compound NC(N)S(O)(=O)=O URKRWCPDFVDQTD-UHFFFAOYSA-N 0.000 claims description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical class [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 239000002923 metal particle Substances 0.000 claims description 2
- 230000000149 penetrating effect Effects 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- 229920002492 poly(sulfone) Polymers 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 229920002857 polybutadiene Polymers 0.000 claims description 2
- 229920006393 polyether sulfone Polymers 0.000 claims description 2
- 229920002530 polyetherether ketone Polymers 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 2
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 2
- 229920006324 polyoxymethylene Polymers 0.000 claims description 2
- 229920000069 polyphenylene sulfide Polymers 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 2
- 239000004800 polyvinyl chloride Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229920006305 unsaturated polyester Polymers 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical class [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 claims 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims 1
- 239000007983 Tris buffer Substances 0.000 claims 1
- 239000004480 active ingredient Substances 0.000 claims 1
- 239000012466 permeate Substances 0.000 claims 1
- 229910052697 platinum Inorganic materials 0.000 claims 1
- 229920006380 polyphenylene oxide Polymers 0.000 claims 1
- 239000007858 starting material Substances 0.000 claims 1
- 238000004064 recycling Methods 0.000 abstract description 12
- 230000007613 environmental effect Effects 0.000 abstract description 7
- 229920000642 polymer Polymers 0.000 abstract description 2
- 238000007598 dipping method Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 9
- 230000007246 mechanism Effects 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- 150000003624 transition metals Chemical class 0.000 description 4
- 229920002292 Nylon 6 Polymers 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- PISLZQACAJMAIO-UHFFFAOYSA-N 2,4-diethyl-6-methylbenzene-1,3-diamine Chemical compound CCC1=CC(C)=C(N)C(CC)=C1N PISLZQACAJMAIO-UHFFFAOYSA-N 0.000 description 2
- 239000004962 Polyamide-imide Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229920006127 amorphous resin Polymers 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005087 graphitization Methods 0.000 description 2
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- 238000001556 precipitation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229940024548 aluminum oxide Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 229920013636 polyphenyl ether polymer Polymers 0.000 description 1
- 238000009656 pre-carbonization Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000002352 steam pyrolysis Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- 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
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention belongs to the technical field of polymer composite materials, and discloses a CFRP waste carbonized regenerated resin-based composite material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) preparing a porous carbon precursor by pre-carbonizing CFRP waste; (2) Adding a porous carbon precursor into the prepared metal nanocluster catalyst solution, carrying out ultrasonic treatment, dipping and drying; (3) Preparing a resin carbon/recycled carbon fiber skeleton by a direct carbonization strategy; and (4) preparing the recycled carbon fiber regenerated resin-based composite material. The composite material prepared by the invention reserves the original highly oriented woven structure of the carbon fibers in the CFRP waste, efficiently recycles the high-value carbon fibers and the resin matrix, ensures that the prepared recycled carbon fiber-resin-based composite material has good heat conduction performance and mechanical property, meets the requirements of industry and environmental protection, and provides a new idea for recycling all components of the CFRP waste.
Description
Technical Field
The invention relates to the technical field of polymer composite materials, in particular to a CFRP waste carbonized regenerated resin-based composite material and a preparation method thereof.
Background
Because the carbon fiber reinforced resin matrix Composite (CFRP) has excellent physical and chemical properties such as high strength, high modulus, high toughness, corrosion resistance and the like, the CFRP is widely applied to the fields such as aerospace, military, wind energy, automobiles, buildings, sports, medical treatment and the like. While there is an increasing global demand for CFRP, CFRP scrap generated during the forming process and CFRP waste generated at the end of the product life cycle are increasing. It was counted that prepregs produced about 30% of scrap after cutting and forming during CFRP production, and it was expected that commercial aircraft retired would produce over 17 ten thousand tons of CFRP waste by 2025. Therefore, the high-value recovery and reuse of the carbon fibers in the CFRP waste are intensively studied and explored, the importance under the sustainable development background is remarkably reflected, and along with the increasing importance of the effective utilization of resources and the environmental protection, the carbon fibers in the CFRP waste are reinjected into the production cycle, so that the raw material cost can be reduced, the dependence on natural resources can be reduced, and the method has remarkable economic and environmental significance. For example, in the ford 2018 explorer utility vehicle SUV, the rigid portion of the automotive component a-pillar brace is made of recycled carbon fiber recovered from CFRP waste, which not only maintains the required mechanical properties for each index, but also reduces the weight by 14%, which is expected to reduce the cost of 186000 dollars per year. The BMW group adopts recycled carbon fibers in its i3 electric vehicle, wherein an "ecological CFRP" process is used to decompose and reuse waste carbon fiber products to produce new vehicle body parts.
The matrix used in CFRP is mainly thermosetting resin including epoxy resin, phenolic resin, unsaturated resin, silicone resin, etc., wherein the mass fraction of carbon fiber is about 50% -70%. Currently, processes for recycling CFRP waste are mainly classified into three major categories, namely a mechanical recycling method, a chemical recycling method, and a thermal decomposition method, and the core objective of these processes is to thoroughly remove a resin matrix from waste Carbon Fiber Reinforced Polymer (CFRP) materials to obtain high-value and high-performance carbon fibers. The document of Chinese patent publication No. CN114044936B discloses a method for recovering carbon fiber resin matrix composite material by catalytic steam pyrolysis, which comprises introducing high-temperature normal-pressure steam at 200-550deg.C, and placing the carbon fiber resin matrix composite material into molten chlorinationThe surface finish of the recovered carbon fiber is good after the aluminum and titanium dioxide are treated for 20min, the tensile strength of the monofilament reaches 5.3GPa, and the retention rate is 96.6%. However, the recycling method damages the old-laid structure of the CFRP waste which is originally orderly arranged, the recycled carbon fibers are in an unordered state, the resin matrix in the waste CFRP cannot be effectively utilized, and the aim of recycling all components of the CFRP waste cannot be fulfilled. Chinese patent grant publication No. CN114773667B discloses a method for recovering wind power blades under mild conditions by using a transition metal catalyst, and the method comprises the step of throwing waste wind power blades into the transition metal catalyst K 2 [Co(SO 4 ) 2 ]Or [ CrCl ] 2 (NH 3 ) 4 ]˙Cl˙2H 2 In O solution, the carbon fiber and the low molecular weight thermoplastic polymer with clean surfaces are recovered in a microwave heating reaction kettle at 190-210 ℃ for 7-11 hours, so that the carbon fiber and the resin matrix are recovered simultaneously, but the invention is only applicable to composite materials with thermoplastic resin as the matrix, is not applicable to the recovery of CFRP with thermosetting resin as the matrix, and has the advantages of longer reaction time, higher recovery cost, more complex process and difficult realization of industrialization.
Disclosure of Invention
Based on the defects of the invention, the invention provides the CFRP waste carbonized regenerated resin matrix composite material, and the composite material can retain the original weaving structure of the carbon fibers in the waste CFRP through a novel process method, effectively recycle and reuse high-value carbon fibers and resin matrixes, so that the prepared recycled carbon fiber resin matrix composite material has good heat conduction and mechanical properties, meets the requirements of environmental protection and industry, can realize the economic and environmental protection benefits of carbon fiber recycling, and provides a novel technical idea for recycling and reusing all components of the CFRP waste.
The technical scheme adopted by the invention for achieving the purpose is as follows:
the preparation method of the CFRP waste carbonized regenerated resin matrix composite material is characterized by comprising the following steps of:
(1) Pre-carbonizing CFRP waste in inert atmosphere to prepare a porous carbon precursor, heating to 350 ℃ at a pre-carbonizing heating rate of 5-20 ℃/min, preserving heat for 5-30 min, and naturally cooling to room temperature along with a furnace; in the process of pre-pyrolysis of CFRP waste, non-carbon elements in a resin matrix continuously escape in the form of gaseous small organic molecules and pyrolysis oil to form a plurality of volatile holes and pores for subsequent catalyst impregnation;
(2) Co (NO) 3 ) 2 ﹒6H 2 O、Ni(NO 3 ) 2 ·6H 2 O、Zn(NO 3 ) 2 ·6H 2 Fully dissolving O and 2-methylimidazole in deionized water, and performing ultrasonic treatment to obtain a mixed solution; immersing the porous carbon precursor prepared in the step (1) into a mixed solution, carrying out vacuum auxiliary immersion, standing and aging at room temperature, uniformly synthesizing a three-metal nanocluster catalyst on the porous carbon precursor, and then taking out and drying to obtain the porous carbon precursor containing the catalyst;
(3) Directly carbonizing the porous carbon precursor containing the catalyst prepared in the step (2) in an inert atmosphere, heating to 400-1400 ℃ at a heating rate of 5-20 ℃/min, preserving heat, and naturally cooling to room temperature along with a furnace to prepare a resin carbon/recovered carbon fiber skeleton:
(4) Immersing the resin carbon/recycled carbon fiber skeleton prepared in the step (3) into a newly prepared resin solution, then placing the newly prepared resin solution into a vacuum bag for curing, uniformly penetrating the newly prepared resin into the resin carbon/recycled carbon fiber skeleton in the curing process, taking out the resin carbon/recycled carbon fiber skeleton after natural cooling, and polishing to obtain the recycled carbon fiber regenerated resin-based composite material, namely the CFRP waste carbonized regenerated resin-based composite material.
The CFRP waste carbonized regenerated resin-based composite material is prepared by adopting any one of the preparation methods.
The beneficial effects of the invention are as follows:
(1) According to the CFRP waste carbonization regenerated resin-based composite material and the preparation method thereof, the original highly oriented woven structure of the recycled carbon fibers in the waste CFRP is skillfully reserved by adopting a direct carbonization strategy, the high-value carbon fibers and the resin matrix in the CFRP waste are directly carbonized and regenerated and are effectively combined with a new resin matrix, and the prepared recycled carbon fiber resin-based composite material has good heat conduction and mechanical properties, has wide application prospects in various fields of aerospace, automobile manufacturing, electronic devices, building materials, sports equipment and the like, and can provide lighter, stronger, more efficient and more economical material choices for different application scenes in various fields.
(2) According to the CFRP waste carbonized regenerated resin-based composite material and the preparation method thereof, the original highly oriented structure of the carbon fiber is successfully reserved through a direct carbonization process at low temperature. The process is not only favorable for maintaining the mechanical properties of the carbon fibers, but also takes the resin carbon as a bridge to tightly connect the carbon fibers, thereby increasing the number of connection nodes. According to the method, more and more complex heat conduction channels are constructed among the carbon fibers, so that the heat conduction performance of the material is remarkably improved.
(3) The preparation method and the material designed by the invention can fully utilize the recycled carbon fiber and the resin carbon to be added into the resin-based composite material, reduce the industrial cost and lighten the environmental protection pressure, can solve the problem that the CFRP prepreg leftover materials and the CFRP wastes cannot be effectively reused, are expected to provide a new idea for recycling the whole components of the CFRP wastes, and play a positive role in promoting sustainable development and resource recycling.
(4) The CFRP waste carbonized regenerated resin-based composite material provided by the invention is a recovered carbon fiber composite material integrating heat conduction and mechanical functions, and can be widely applied to the fields of electronic component heat dissipation, thermal management materials and the like.
The foregoing is a simplified illustration of a preferred embodiment of the present invention, and the following detailed description of the invention is provided in connection with specific embodiments thereof.
Detailed Description
Examples
The preparation method of the CFRP waste carbonized regenerated resin matrix composite material provided by the embodiment comprises the following steps:
(1) And pre-carbonizing clean CFRP waste in an inert atmosphere to prepare the porous carbon precursor. The temperature rising rate of the pre-carbonization is 5-20 ℃/min, the temperature is kept for 5-30 min after the heating to 350 ℃, and the temperature is naturally cooled to the room temperature along with the furnace. In the process of CFRP waste pre-pyrolysis, non-carbon elements (such as N, O, H, etc.) in the resin matrix continuously escape in the form of gaseous small organic molecules and pyrolysis oil, forming a plurality of volatile holes and pores, and the porous structure is used for subsequent catalyst impregnation.
Wherein, the matrix of the CFRP waste is: epoxy resin, phenolic resin, polyethylene, polypropylene, polyvinyl chloride, polyacrylic acid, polyurethane, polycarbonate, polyamide, polyimide, polyoxymethylene, polyphenylene sulfide, polyether sulfone, polyether ether ketone and polyethylene terephthalate.
(2) Co (NO) 3 ) 2 ﹒6H 2 O、Ni(NO 3 ) 2 ·6H 2 O、Zn(NO 3 ) 2 ·6H 2 O and 20mmol of 2-methylimidazole were sufficiently dissolved in 100mL of deionized water, and placed in a tip ultrasonic at 240w at 25℃for 1 hour to obtain a mixed solution. Immersing the porous carbon precursor in the step (1) into the mixed solution, carrying out vacuum auxiliary immersion, standing and aging for 3-6 hours at room temperature, uniformly synthesizing a three-metal nanocluster catalyst (such as CoNiZn) on the porous carbon precursor, taking out, and drying at 60 ℃ for 24 hours. The adding proportion of the tri-metal nanocluster catalyst (CoNiZn) is 1-25% of the mass of the porous carbon precursor.
The raw materials of the three-metal nanocluster catalyst are any three of metal salts of VIII group elements such as iron, cobalt, nickel and platinum, metal salts of IVB-VIIB group elements such as titanium, vanadium, chromium and manganese, and metal salts of copper, silver, zinc and zirconium IB-IIB group elements.
The organic ligand of the trimetallic nanocluster catalyst comprises one of 2-methylimidazole, terephthalic acid, dipicolinic acid, trimesic acid, 1, 4-di (4-pyridyl) benzene, tri (4-carboxyphenyl) trifluoroboron, diaminomethanesulfonic acid, H3TAB or HTB.
Wherein the concentration of the trimetallic nanocluster catalyst is controlled to be 0.01-0.1 mol/L.
(3) And (3) directly carbonizing the porous carbon precursor containing the catalyst in the step (2) in an inert atmosphere to prepare the resin carbon/recovered carbon fiber skeleton. Heating to 400-1400 deg.c at the temperature raising rate of 5-20 deg.c/min, maintaining for 30-120 min, and cooling naturally to room temperature. The three-metal nano-cluster catalyst (CoNiZn) is formed by coordination of a metal cluster center and an organic ligand, in the high-temperature carbonization process, porous carbon formed by degradation of the organic ligand can be effectively fused with a resin carbon/recycled carbon fiber skeleton, and the metal cluster center is reduced to metal particles or metal oxide is formed to be tightly embedded in the porous carbon at high temperature, so that an effective component of resin catalytic carbon formation is formed.
The mechanism of resin catalysis and carbon formation is mainly based on a dissolution and precipitation mechanism, namely amorphous resin carbon can be dissolved into a trimetallic nanocluster to form a solid solution under a high temperature condition, carbon atoms are continuously arranged and rearranged on a transition metal/carbon interface, graphite-like structure carbon is precipitated on the surface of the trimetallic nanocluster, the graphitization degree of a resin carbon/recycled carbon fiber framework is improved, and the heat conduction and mechanical properties of the recycled carbon fiber regenerated resin matrix composite material are enhanced.
(4) Immersing the resin carbon/recycled carbon fiber skeleton in the step (3) into a newly prepared resin solution, and then placing the resin solution into a self-made vacuum bag to complete solidification. The resin curing process is completed through the steps of vacuumizing, programmed heating, exhausting and the like for a plurality of times, so that the gas in the vacuum bag can be effectively exhausted, the generation of bubbles is reduced, and the newly manufactured resin can uniformly infiltrate into the resin carbon/recycled carbon fiber skeleton. And taking out after natural cooling, and polishing to obtain the recycled carbon fiber regenerated resin-based composite material.
Wherein the newly prepared resin solution comprises one of polyimide, epoxy resin, phenolic resin, unsaturated polyester, organic silicon resin, polybutadiene resin, polyethylene, polypropylene, polystyrene, polyethylene glycol, polyvinyl alcohol, polydimethylsiloxane, polyamide, polycarbonate, polyphenyl ether and polysulfone.
As a further improvement of the present invention, the step (1) further includes a step of cutting the size of CFRP waste and then cleaning, including:
A. cutting CFRP waste into dimensions of 20mm x 10mm x 2mm using a cutter;
B. immersing the CFRP waste obtained in the step A in deionized water, placing the immersed CFRP waste in a 220w and 50Hz ultrasonic cleaner for 2 hours, and removing impurities on the surface of the CFRP waste;
C. and C, placing the clean CFRP waste obtained in the step B in an oven at 60 ℃ for drying for 24 hours.
The CFRP waste carbonized regenerated resin-based composite material is prepared by the preparation method.
The following describes several embodiments in detail.
Example 1
The preparation method of the CFRP waste carbonized regenerated resin matrix composite material provided by the embodiment specifically comprises the following steps on the basis of the embodiment:
(1) Cutting CFRP waste into blocks with the thickness of 20mm to 10mm to 2mm by using a cutting machine, immersing the blocks in deionized water, placing the blocks in a 220w and 50Hz ultrasonic cleaner for 2 hours, and removing impurities on the surface of the CFRP waste; placing the clean CFRP waste in an oven at 60 ℃ for drying for 24 hours;
(2) Pre-carbonizing the clean CFRP waste in the step (1) in a tube furnace filled with inert atmosphere to prepare a porous carbon precursor, heating to 350 ℃ at a heating rate of 10 ℃/min, preserving heat for 10min, and naturally cooling to room temperature along with the furnace;
(3) 0.5mmol Co (NO) 3 ) 2 ﹒6H 2 O、0.5mmol Ni(NO 3 ) 2 ·6H 2 O、0.5mmol Zn(NO 3 ) 2 ·6H 2 O and 20mmol of 2-methylimidazole were sufficiently dissolved in 100mL of deionized water, and placed in a tip ultrasonic at 240w at 25℃for 1 hour to obtain a mixed solution. Immersing the porous carbon precursor in the step (2) into the mixed solution, carrying out vacuum auxiliary immersion, standing and aging for 3 hours at room temperature, and uniformly synthesizing the trimetallic nanoclusters on the porous carbon precursorThe catalyst CoNiZn was then removed and dried at 60℃for 24 hours. The addition proportion of the three-metal nanocluster catalyst CoNiZn is 5% of the mass of the porous carbon precursor.
(4) And (3) directly carbonizing the porous carbon precursor containing the catalyst in the step (3) in an inert atmosphere to prepare the resin carbon/recovered carbon fiber skeleton. Heating to 1200 deg.c at 10 deg.c/min, maintaining for 120min, and cooling naturally to room temperature. The mechanism of resin catalysis and carbon formation is mainly based on a dissolution and precipitation mechanism, namely amorphous resin carbon can be dissolved into a trimetallic nanocluster to form a solid solution under a high temperature condition, carbon atoms are continuously arranged and rearranged on a transition metal/carbon interface, graphite-like structure carbon is precipitated on the surface of the trimetallic nanocluster, the graphitization degree of a resin carbon/recycled carbon fiber framework is improved, and the heat conduction and mechanical properties of the recycled carbon fiber regenerated resin matrix composite material are enhanced.
(5) 8.38g of the polyamideimide resin powder was weighed and dissolved in 50mL of N, N-dimethylformamide, and a 15wt% solution was prepared and placed in a 220w, 50Hz ultrasonic cleaner for 2 hours to uniformly dissolve. Immersing the resin carbon/recycled carbon fiber skeleton in the step (3) into the newly prepared resin solution, and then placing the resin solution into a self-made vacuum bag to complete curing (curing process: heat preservation at 60 ℃ C. For 48h, heat preservation at 80 ℃ C. For 24h, and heat preservation at 105 ℃ C. For 1h to complete curing). And taking out after natural cooling, and polishing to obtain the recycled carbon fiber/polyamide-imide composite material product.
The CFRP waste carbonized regenerated resin-based composite material prepared by the method.
Example 2
The CFRP waste carbonized regenerated resin-based composite material and the preparation method thereof provided in this embodiment are basically the same as those in embodiment 1, except that the preparation method thereof includes the steps of:
(1) Cutting CFRP waste into blocks with the thickness of 20mm to 10mm to 2mm by using a cutting machine, immersing the blocks in deionized water, placing the blocks in a 220w and 50Hz ultrasonic cleaner for 2 hours, and removing impurities on the surface of the CFRP waste; placing the clean CFRP waste in an oven at 60 ℃ for drying for 24 hours;
(2) Pre-carbonizing the clean CFRP waste in the step (1) in a tube furnace filled with inert atmosphere to prepare a porous carbon precursor, heating to 350 ℃ at a heating rate of 10 ℃/min, preserving heat for 20min, and naturally cooling to room temperature along with the furnace;
(3) 1mmol Co (NO) 3 ) 2 ﹒6H 2 O、1mmol Ni(NO 3 ) 2 ·6H 2 O、1mmol Zn(NO 3 ) 2 ·6H 2 O and 20mmol of 2-methylimidazole were sufficiently dissolved in 100mL of deionized water, and placed in a tip ultrasonic at 240w at 25℃for 1 hour to obtain a mixed solution. Immersing the porous carbon precursor in the step (2) into the mixed solution, carrying out vacuum auxiliary immersion, standing and aging for 4 hours at room temperature, uniformly synthesizing a three-metal nanocluster catalyst CoNiZn on the porous carbon precursor, and then taking out and drying at 60 ℃ for 24 hours. The addition proportion of the three-metal nanocluster catalyst CoNiZn is 5% of the mass of the porous carbon precursor.
(4) And (3) directly carbonizing the porous carbon precursor containing the catalyst in the step (3) in an inert atmosphere to prepare the resin carbon/recovered carbon fiber skeleton. Heating to 800 ℃ at a heating rate of 5 ℃/min, preserving heat for 120min, and naturally cooling to room temperature along with a furnace.
(5) 8.38g of epoxy resin powder and 3.59g of diethyltoluenediamine (DETDA) curing agent were weighed out and dissolved in 50mL of N, N-dimethylformamide, a 15wt% solution was prepared, and the mixture was placed in a 220w, 50Hz ultrasonic cleaner for 2 hours to uniformly dissolve the mixture. Immersing the resin carbon/recycled carbon fiber skeleton in the step (3) into a newly prepared resin solution, and then placing the resin solution into a self-made vacuum bag to complete curing (curing process: heat preservation at 80 ℃ for 1h, heat preservation at 100 ℃ for 2h, and heat preservation at 120 ℃ for 1h to complete curing), thus obtaining the recycled carbon fiber/epoxy resin composite material product.
Example 3
The CFRP waste carbonized regenerated resin-based composite material and the preparation method thereof provided in this embodiment are basically the same as those in embodiment 1, except that the preparation method thereof includes the steps of:
(1) Cutting CFRP waste into blocks with the thickness of 20mm to 10mm to 2mm by using a cutting machine, immersing the blocks in deionized water, placing the blocks in a 220w and 50Hz ultrasonic cleaner for 2 hours, and removing impurities on the surface of the CFRP waste; placing the clean CFRP waste in an oven at 60 ℃ for drying for 24 hours;
(2) Pre-carbonizing the clean CFRP waste in the step (1) in a tube furnace filled with inert atmosphere to prepare a porous carbon precursor, heating to 350 ℃ at a heating rate of 10 ℃/min, preserving heat for 20min, and naturally cooling to room temperature along with the furnace;
(3) In order 2mmol Co (NO 3 ) 2 ﹒6H 2 O、2mmol Ni(NO 3 ) 2 ·6H 2 O、2mmol Zn(NO 3 ) 2 ·6H 2 O and 20mmol of 2-methylimidazole were sufficiently dissolved in 100mL of deionized water, and placed in a tip ultrasonic at 240w at 25℃for 1 hour to obtain a mixed solution. Immersing the porous carbon precursor in the step (2) into the mixed solution, carrying out vacuum auxiliary immersion, standing and aging for 6 hours at room temperature, uniformly synthesizing a three-metal nanocluster catalyst CoNiZn on the porous carbon precursor, and then taking out and drying for 24 hours at 60 ℃. The addition proportion of the three-metal nanocluster catalyst CoNiZn is 5% of the mass of the porous carbon precursor.
(4) And (3) directly carbonizing the porous carbon precursor containing the catalyst in the step (3) in an inert atmosphere to prepare the resin carbon/recovered carbon fiber skeleton. Heating to 800 ℃ at a heating rate of 10 ℃/min, preserving heat for 60min, and naturally cooling to room temperature along with a furnace.
(5) 8.38g of polyamide 6 resin powder was weighed out and dissolved in 50mL of N, N-dimethylformamide, and a 15wt% solution was prepared and placed in a 220w, 50Hz ultrasonic cleaner for 2 hours to uniformly dissolve. Immersing the resin carbon/recycled carbon fiber skeleton in the step (4) into a newly prepared polyamide 6 resin solution, and then placing the resin carbon/recycled carbon fiber skeleton into a self-made vacuum bag to complete curing (curing process: heat preservation at 60 ℃ for 12h, heat preservation at 100 ℃ for 12h, heat preservation at 180 ℃ for 2h and heat preservation for 24h to complete curing), thus obtaining the recycled carbon fiber/polyamide 6 composite material product.
Application example 1
The CFRP waste carbonized regenerated resin-based composite materials prepared in examples 1 to 3 were tested for heat conductivity, tensile strength and flexural strength, and the results are shown in the following table.
The test results show that the CFRP waste carbonized regenerated resin-based composite material prepared in the embodiments 1-3 has good heat conduction and mechanical properties, and can realize the aim of recycling all components of the CFRP waste.
The composite material prepared by the embodiment of the invention reserves the original highly oriented woven structure of the carbon fibers in the CFRP waste, efficiently recycles the high-value carbon fibers and the resin matrix, ensures that the prepared recycled carbon fiber-resin-based composite material has good heat conducting property and mechanical property, meets the requirements of industry and environmental protection, and provides a new idea for recycling all components of the CFRP waste.
The above-mentioned embodiments are merely preferred embodiments of the present invention, and the technical scope of the present invention is not limited in any way, so that the technical features that are the same as or similar to the above-mentioned embodiments of the present invention are all within the scope of the present invention.
Claims (10)
1. The preparation method of the CFRP waste carbonized regenerated resin matrix composite material is characterized by comprising the following steps of:
(1) Pre-carbonizing CFRP waste in inert atmosphere to prepare a porous carbon precursor, heating to 350 ℃ at a pre-carbonizing heating rate of 5-20 ℃/min, preserving heat for 5-30 min, and naturally cooling to room temperature along with a furnace; in the process of pre-pyrolysis of CFRP waste, non-carbon elements in a resin matrix continuously escape in the form of gaseous small organic molecules and pyrolysis oil to form a plurality of volatile holes and pores for subsequent catalyst impregnation;
(2) Co (NO) 3 ) 2 ﹒6H 2 O、Ni(NO 3 ) 2 ·6H 2 O、Zn(NO 3 ) 2 ·6H 2 Fully dissolving O and 2-methylimidazole in deionized water, and performing ultrasonic treatment to obtain a mixed solution; immersing the porous carbon precursor prepared in the step (1) into a mixed solution, carrying out vacuum auxiliary immersion, standing and aging at room temperature, uniformly synthesizing a three-metal nanocluster catalyst on the porous carbon precursor, and then taking out and drying to obtain the porous carbon precursor containing the catalyst;
(3) Directly carbonizing the porous carbon precursor containing the catalyst prepared in the step (2) in an inert atmosphere, heating to 400-1400 ℃ at a heating rate of 5-20 ℃/min, preserving heat, and naturally cooling to room temperature along with a furnace to prepare a resin carbon/recovered carbon fiber skeleton:
(4) Immersing the resin carbon/recycled carbon fiber skeleton prepared in the step (3) into a newly prepared resin solution, then placing the newly prepared resin solution into a vacuum bag for curing, uniformly penetrating the newly prepared resin into the resin carbon/recycled carbon fiber skeleton in the curing process, taking out the resin carbon/recycled carbon fiber skeleton after natural cooling, and polishing to obtain the recycled carbon fiber regenerated resin-based composite material, namely the CFRP waste carbonized regenerated resin-based composite material.
2. The method of manufacturing according to claim 1, wherein the step (1) further includes a step of cutting and cleaning CFRP waste, including:
A. cutting CFRP waste into dimensions of 20mm x 10mm x 2mm using a cutter;
B. immersing the CFRP waste obtained in the step A in deionized water, and placing the immersed CFRP waste in an ultrasonic cleaner to remove impurities on the surface of the CFRP waste;
C. and C, placing the clean CFRP waste obtained in the step B into an oven for drying.
3. The method of claim 1, wherein the matrix of CFRP waste in step (1) is one or a combination of several of epoxy resin, phenolic resin, polyethylene, polypropylene, polyvinyl chloride, polyacrylic acid, polyurethane, polycarbonate, polyamide, polyimide, polyoxymethylene, polyphenylene sulfide, polyethersulfone, polyetheretherketone, and polyethylene terephthalate.
4. The preparation method of claim 1, wherein the addition ratio of the trimetallic nanocluster catalyst in the step (2) is 1-25% of the mass of the porous carbon precursor; the concentration of the trimetallic nanocluster catalyst is 0.01-0.1 mol/L.
5. The method of claim 1, wherein the starting material of the trimetallic nanocluster catalyst of step (2) comprises any three combinations of group VIII metal salts of iron, cobalt, nickel, platinum, group IVB-VIIB metal salts of titanium, vanadium, chromium, manganese, copper, silver, zinc, zirconium IB-IIB metal salts.
6. The method of preparing of claim 1, wherein the organic ligand of the trimetallic nanocluster catalyst of step (2) comprises one of 2-methylimidazole, terephthalic acid, dipicolinic acid, trimellitic acid, 1, 4-bis (4-pyridyl) benzene, tris (4-carboxyphenyl) trifluoroboron, diaminomethanesulfonic acid, H3TAB, or HTB.
7. The method according to claim 1, wherein in the step (3), the trimetallic nanocluster catalyst is formed by coordinating a metal cluster center with an organic ligand, and in the high-temperature carbonization process, porous carbon formed by degradation of the organic ligand can be effectively fused with a resin carbon/recycled carbon fiber skeleton, and the metal cluster center is reduced to metal particles or forms metal oxide tightly embedded in the porous carbon at high temperature to form an active ingredient of resin catalytic carbon formation.
8. The method of claim 1, wherein the newly formulated resin solution of step (4) is: polyimide, epoxy resin, phenolic resin, unsaturated polyester, organic silicon resin, polybutadiene resin, polyethylene, polypropylene, polystyrene, polyethylene glycol, polyvinyl alcohol, polydimethylsiloxane, polyamide, polycarbonate, polyphenylene oxide and polysulfone.
9. The method of manufacturing of claim 1, wherein step (4) further comprises: immersing the resin carbon/recycled carbon fiber skeleton into a newly prepared resin solution, and then placing the resin solution into a vacuum bag for curing, wherein the newly prepared resin uniformly permeates into the resin carbon/recycled carbon fiber skeleton in the curing process, specifically: the resin curing procedure is completed through the steps of vacuumizing, programmed heating and exhausting for many times, so that the gas in the vacuum bag is effectively exhausted, the generation of bubbles is reduced, and the newly manufactured resin is uniformly permeated into the resin carbon/recovered carbon fiber skeleton.
10. A CFRP waste carbonized regenerated resin-based composite material, characterized in that it is prepared by the preparation method of any one of claims 1 to 9.
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