CN113105717B - High-temperature-resistant carbon fiber composite material and preparation method thereof - Google Patents
High-temperature-resistant carbon fiber composite material and preparation method thereof Download PDFInfo
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 86
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 86
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229920001661 Chitosan Polymers 0.000 claims abstract description 62
- 239000003822 epoxy resin Substances 0.000 claims abstract description 49
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 49
- 239000003292 glue Substances 0.000 claims abstract description 33
- BSYJHYLAMMJNRC-UHFFFAOYSA-N 2,4,4-trimethylpentan-2-ol Chemical compound CC(C)(C)CC(C)(C)O BSYJHYLAMMJNRC-UHFFFAOYSA-N 0.000 claims abstract description 28
- 150000001875 compounds Chemical class 0.000 claims abstract description 26
- ANYWGXDASKQYAD-UHFFFAOYSA-N 5-nitroisoindole-1,3-dione Chemical compound [O-][N+](=O)C1=CC=C2C(=O)NC(=O)C2=C1 ANYWGXDASKQYAD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims description 89
- 238000010438 heat treatment Methods 0.000 claims description 87
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 64
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 48
- 239000000243 solution Substances 0.000 claims description 47
- 239000000203 mixture Substances 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 26
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 18
- 239000004202 carbamide Substances 0.000 claims description 18
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 16
- 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 claims description 12
- HZEOUPCNUWSUFL-UHFFFAOYSA-N 4,5,5-trimethyl-4-pentan-3-yl-1H-imidazole Chemical compound C(C)C(C1(N=CNC1(C)C)C)CC HZEOUPCNUWSUFL-UHFFFAOYSA-N 0.000 claims description 12
- RQEOBXYYEPMCPJ-UHFFFAOYSA-N 4,6-diethyl-2-methylbenzene-1,3-diamine Chemical compound CCC1=CC(CC)=C(N)C(C)=C1N RQEOBXYYEPMCPJ-UHFFFAOYSA-N 0.000 claims description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 10
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 8
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 8
- 239000011609 ammonium molybdate Substances 0.000 claims description 8
- 229940010552 ammonium molybdate Drugs 0.000 claims description 8
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 229940048181 sodium sulfide nonahydrate Drugs 0.000 claims description 8
- WMDLZMCDBSJMTM-UHFFFAOYSA-M sodium;sulfanide;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[SH-] WMDLZMCDBSJMTM-UHFFFAOYSA-M 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 238000004132 cross linking Methods 0.000 abstract description 10
- 229920005989 resin Polymers 0.000 abstract description 10
- 239000011347 resin Substances 0.000 abstract description 10
- 125000003277 amino group Chemical group 0.000 abstract description 6
- 230000009477 glass transition Effects 0.000 abstract description 6
- RBTKNAXYKSUFRK-UHFFFAOYSA-N heliogen blue Chemical compound [Cu].[N-]1C2=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=NC([N-]1)=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=N2 RBTKNAXYKSUFRK-UHFFFAOYSA-N 0.000 abstract description 6
- 239000011159 matrix material Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 21
- 229910052802 copper Inorganic materials 0.000 description 20
- 239000010949 copper Substances 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 239000003063 flame retardant Substances 0.000 description 7
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 5
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 238000007259 addition reaction Methods 0.000 description 2
- 125000006615 aromatic heterocyclic group Chemical group 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- -1 flame retardant compound Chemical class 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 229920002430 Fibre-reinforced plastic Polymers 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011151 fibre-reinforced plastic Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a high-temperature-resistant carbon fiber composite material and a preparation method thereof. Comprises epoxy resin glue solution, 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, chitosan compound and carbon fiber; the carbon fiber and the resin matrix are bonded by chitosan, and tetramino copper phthalocyanine prepared by adding 4-nitrophthalimide can form covalent bonds between the carbon fiber and the epoxy resin by amino groups on the tetramino copper phthalocyanine and participate in the curing of the epoxy resin, so that the interface crosslinking density between the carbon fiber and the epoxy resin is enhanced; the composite material prepared by the invention has good practicability and production value by enhancing the interface crosslinking and strength between the carbon fiber and the resin matrix, improving the glass transition temperature of the interface and improving the high temperature resistance of the composite material.
Description
Technical Field
The invention relates to the technical field, in particular to a high-temperature-resistant carbon fiber composite material and a preparation method thereof.
Background
Carbon fiber is a fiber with extremely high carbon content, has high strength and high modulus, and heat resistance is first-called, and is often used for being compounded with materials such as resin, ceramic and the like to strengthen the strength and heat resistance of a composite material.
However, the effect of compounding the carbon fiber and the resin material is not ideal, the heat resistance between the carbon fiber and the resin interface is relatively poor, and when the temperature of the composite material is increased, the bonding strength of the interface is low, the interface is easy to break, the compounding effect of the carbon fiber and the resin is poor, the mechanical property is low, and the heat resistance is reduced.
Aiming at the problems, the invention provides a high-temperature-resistant carbon fiber composite material and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant carbon fiber composite material and a preparation method thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
the high-temperature-resistant carbon fiber composite material comprises epoxy resin glue solution, 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, chitosan composite and carbon fiber.
Further, in the carbon fiber composite material, 35-45 parts of epoxy resin glue solution, 1-2 parts of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 7-9 parts of chitosan composite and 5-10 parts of carbon fiber by weight.
Further, the epoxy resin is mainly prepared from triglycidyl para-aminophenol, 3, 5-diethyl-2, 4-toluenediamine, 3, 5-diethyl-2, 6-toluenediamine, diaminodiphenyl sulfone and diethyl tetramethyl imidazole.
Further, the chitosan compound is mainly prepared from chitosan, 4-nitrophthalimide, urea and copper chloride.
The preparation method of the high-temperature-resistant carbon fiber composite material comprises the following steps:
s1: preparing a chitosan compound from 4-nitrophthalimide, urea, copper chloride and chitosan;
s2: reacting carbon fiber with chitosan complex and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to prepare a mixture;
s3: and (3) blending the mixture with epoxy resin glue solution to prepare the composite material.
Further, the step S1:
(1) Mixing 4-nitrophthalimide with quinoline, adding urea, heating in a water bath, stirring uniformly, ultrasonically oscillating, placing in an oil bath pot, heating in the oil bath, introducing nitrogen, adding copper chloride and ammonium molybdate, stirring uniformly, standing for a period of time, filtering, washing, drying, placing in N, N-dimethylformamide, heating in the water bath, adding sodium sulfide nonahydrate, stirring uniformly, ultrasonically oscillating, standing for a period of time, filtering, flushing and drying to obtain a substance A;
(2) Placing chitosan into an acetic acid aqueous solution, uniformly stirring, adding a substance A, heating in a water bath, uniformly stirring, ultrasonically oscillating, adding glutaraldehyde, heating in the water bath, uniformly stirring, and standing for a period of time to obtain a chitosan compound;
in the step S1, the carbon fiber and a resin matrix are bonded by chitosan, and tetraminophthalocyanine copper prepared by adding 4-nitrophthalimide is added, so that the tetraminophthalocyanine copper and chitosan form a cross-linking network, the amino group and the hydroxyl group on the chitosan and the amino group on the tetraminophthalocyanine copper form a cross-linking network, the bonding degree is higher, simultaneously, the amino group on the tetraminophthalocyanine copper can form a covalent bond between the carbon fiber and the epoxy resin and participate in the curing of the epoxy resin, the effect of a bridge is achieved, the carbon fiber and the epoxy resin are connected, the interface cross-linking density between the carbon fiber and the epoxy resin is enhanced, and meanwhile, the strength of an interface is improved due to the rigid aromatic heterocyclic structure of the tetraminophthalocyanine copper, so that the glass transition temperature of the interface is increased, and the high temperature resistance of the composite material is improved;
further, the step S2:
(1) Placing carbon fiber in a Soxhlet extractor, adding acetone solution, heating, refluxing for a period of time, and drying for use;
(2) Placing the chitosan compound in N, N-dimethylformamide, uniformly stirring, adding 9, 10-dihydro-9 oxa-10-phosphaphenanthrene-10-oxide, placing in an oil bath pot, heating in the oil bath, heating for a period of time, uniformly stirring, standing for a period of time, adding the carbon fiber treated in step (1), uniformly stirring, and performing ultrasonic vibration to obtain a mixture;
in the step S2, 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide reacts with copper tetraminophthalocyanine, wherein a phosphorus hydrogen bond in the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and a carbon nitrogen double bond in the copper tetraminophthalocyanine are subjected to an addition reaction, and a rigid aromatic heterocycle is added at the interface between carbon fiber and epoxy resin, so that the interface strength is further improved, and meanwhile, a novel flame retardant compound is formed, and the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is not easy to fall off after addition, so that the flame retardant effect is better;
meanwhile, because of pi-pi interaction between the carbon fiber and the copper tetraminophthalocyanine, the copper tetraminophthalocyanine and the carbon fiber have high bonding strength, and the interface strength is improved;
further, the step S3:
(1) Heating triglycidyl para-aminophenol in a water bath, adding 3, 5-diethyl-2, 4-toluenediamine, 3, 5-diethyl-2, 6-toluenediamine, diaminodiphenyl sulfone and diethyl tetramethylimidazole, and uniformly stirring to obtain epoxy resin glue solution;
(2) Mixing the mixture with epoxy resin glue solution, heating in water bath, carrying out ultrasonic vibration, uniformly stirring, and curing to obtain a composite material;
in the step S3, copper and organic matters coordinate to form tetramino copper phthalocyanine, the tetraamino copper phthalocyanine is compounded with carbon fibers, and the copper and the carbon fibers are mutually crosslinked to form a conductive network, so that the antistatic performance of the composite material is improved.
Further, the step S1:
(1) Mixing 4-nitrophthalimide with quinoline, adding urea, heating to 60 ℃ in a water bath, mechanically stirring for 10-20 min, ultrasonically oscillating for 5min, placing in an oil bath pot, heating to 185 ℃ in the oil bath, introducing nitrogen, adding copper chloride and ammonium molybdate, mechanically stirring for 3-4 h, standing for 10min, filtering, washing with hydrogen chloride and sodium hydroxide for 3-4 times in sequence, washing with deionized water to neutrality, placing in an oven, drying at 80 ℃ for 20-30 min, placing in N, N-dimethylformamide, heating to 55 ℃ in the water bath, adding sodium sulfide nonahydrate, mechanically stirring for 30-40 min, ultrasonically oscillating for 10-20 min, standing for 1-2 h, filtering, washing with deionized water for 3-4 times, placing in the oven, and drying at 60 ℃ for 3h to obtain a substance A;
(2) Placing chitosan into an acetic acid aqueous solution, mechanically stirring for 10-20 min, adding a substance A, heating in a water bath to 40 ℃, mechanically stirring for 10-15 min, ultrasonically oscillating for 5min, adding glutaraldehyde, heating in a water bath to 80 ℃, mechanically stirring for 20-30 min, and standing for 1-2 h to obtain a chitosan compound;
further, the step S2:
(1) Placing the carbon fiber in a Soxhlet extractor, adding an acetone solution, heating to 80 ℃, refluxing for 40-60 hours, placing in an oven, and drying at 60 ℃ for 3-4 hours for later use;
(2) Placing the chitosan compound in N, N-dimethylformamide, mechanically stirring for 10-20 min, adding 9, 10-dihydro-9 oxa-10-phosphaphenanthrene-10-oxide, placing in an oil bath pot, heating the oil bath to 150 ℃, stopping heating after heating for 10min, mechanically stirring for 20-30 min, standing for 1-2 h, adding the carbon fiber treated in step (1), mechanically stirring for 2-3 h, and carrying out ultrasonic oscillation for 40min to obtain a mixture;
further, the step S3:
(1) Heating triglycidyl para-aminophenol to 75 ℃ in a water bath, adding 3, 5-diethyl-2, 4-toluenediamine, 3, 5-diethyl-2, 6-toluenediamine, diaminodiphenyl sulfone and diethyl tetramethylimidazole, and mechanically stirring for 1-2 hours to obtain epoxy resin glue solution;
(2) And (3) mixing the mixture with epoxy resin glue solution, heating in a water bath to 85 ℃, carrying out ultrasonic oscillation for 30min, mechanically stirring for 6-8 h, and curing to obtain the composite material.
Further, the curing in S3 is a staged curing, and the first stage is: curing for 2h at 80 ℃; and a second stage: curing for 3 hours at 100 ℃; and a third stage: curing for 2h at 130 ℃; fourth stage: curing at 170℃for 1h.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a high-temperature-resistant carbon fiber composite material and a preparation method thereof. Comprises epoxy resin glue solution, 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, chitosan compound and carbon fiber. The carbon fiber and the resin matrix are bonded by chitosan, and the tetraminophthalocyanine copper prepared by 4-nitrophthalimide is added, so that the tetraminophthalocyanine copper and the chitosan form cross-linking, amino groups and hydroxyl groups on the chitosan form a cross-linking network, the bonding degree is higher, meanwhile, the amino groups on the tetraminophthalocyanine copper can form covalent bonds between the carbon fiber and the epoxy resin and participate in the curing of the epoxy resin, the effect of a bridge is achieved, the carbon fiber and the epoxy resin are connected, the interface cross-linking density between the carbon fiber and the epoxy resin is enhanced, and meanwhile, the strength of an interface is improved due to the rigid aromatic heterocyclic structure of the tetraminophthalocyanine copper, so that the glass transition temperature of the interface is increased, and the high temperature resistance of the composite material is improved;
meanwhile, because of pi-pi interaction between the carbon fiber and the copper tetraminophthalocyanine, the copper tetraminophthalocyanine and the carbon fiber have high bonding strength, and the interface strength is improved;
reacting 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with tetraminocopper phthalocyanine, wherein a phosphorus hydrogen bond in the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and a carbon nitrogen double bond in the tetraminocopper phthalocyanine are subjected to addition reaction, and a rigid aromatic heterocycle is added at the interface between carbon fiber and epoxy resin, so that the interface strength is further improved, a novel flame retardant compound is formed, and the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is not easy to fall off after addition, so that the flame retardant effect is better;
copper and organic matter coordinate to form tetramino copper phthalocyanine, the tetraamino copper phthalocyanine is compounded with carbon fibers, and the copper and the carbon fibers are mutually crosslinked to form a conductive network, so that the antistatic performance of the composite material is improved;
the high-temperature-resistant carbon fiber composite material prepared by the invention has the advantages of improving the glass transition temperature of the interface, improving the high-temperature resistance of the composite material and having good practicability and production value by strengthening the interface crosslinking and strength between the carbon fiber and the resin matrix.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the high-temperature-resistant carbon fiber composite material comprises the following steps:
s1: preparing a chitosan compound from 4-nitrophthalimide, urea, copper chloride and chitosan;
s2: reacting carbon fiber with chitosan complex and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to prepare a mixture;
s3: and (3) blending the mixture with epoxy resin glue solution to prepare the composite material.
Wherein S1:
(1) Mixing 4-nitrophthalimide with quinoline, adding urea, heating to 60 ℃ in a water bath, mechanically stirring for 10min, ultrasonically oscillating for 5min, placing in an oil bath pot, heating in the oil bath to 185 ℃, introducing nitrogen, adding copper chloride and ammonium molybdate, mechanically stirring for 3h, standing for 10min, filtering, washing with hydrogen chloride and sodium hydroxide for 3 times in sequence, washing with deionized water to neutrality, placing in an oven, drying at 80 ℃ for 20min, placing in N, N-dimethylformamide, heating in the water bath to 55 ℃, adding sodium sulfide nonahydrate, mechanically stirring for 30min, ultrasonically oscillating for 10min, standing for 1h, filtering, washing with deionized water for 3 times, placing in the oven, and drying at 60 ℃ for 3h to obtain a substance A;
(2) Placing chitosan in acetic acid water solution, mechanically stirring for 10min, adding substance A, heating in water bath to 40deg.C, mechanically stirring for 10min, ultrasonic oscillating for 5min, adding glutaraldehyde, heating in water bath to 80deg.C, mechanically stirring for 20min, and standing for 1 hr to obtain chitosan compound;
wherein S2:
(1) Placing 5 parts of carbon fibers in a Soxhlet extractor, adding an acetone solution, heating to 80 ℃, refluxing for 40 hours, placing in an oven, and drying at 60 ℃ for 3 hours for later use;
(2) Placing 7 parts of chitosan compound in N, N-dimethylformamide, mechanically stirring for 10min, adding 1 part of 9, 10-dihydro-9 oxa-10-phosphaphenanthrene-10-oxide, placing in an oil bath pot, heating to 150 ℃ in an oil bath, stopping heating after heating for 10min, mechanically stirring for 20min, standing for 1h, adding the carbon fiber treated in step (1), mechanically stirring for 2h, and carrying out ultrasonic vibration for 40min to obtain a mixture;
wherein, S3:
(1) Heating triglycidyl para-aminophenol to 75 ℃ in a water bath, adding 3, 5-diethyl-2, 4-toluenediamine, 3, 5-diethyl-2, 6-toluenediamine, diaminodiphenyl sulfone and diethyl tetramethylimidazole, and mechanically stirring for 1h to obtain epoxy resin glue solution;
(2) And (3) mixing the mixture with 35 parts of epoxy resin glue solution, heating in a water bath to 85 ℃, carrying out ultrasonic vibration for 30min, mechanically stirring for 6h, and curing to obtain the composite material.
Example 2
The preparation method of the high-temperature-resistant carbon fiber composite material comprises the following steps:
s1: preparing a chitosan compound from 4-nitrophthalimide, urea, copper chloride and chitosan;
s2: reacting carbon fiber with chitosan complex and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to prepare a mixture;
s3: and (3) blending the mixture with epoxy resin glue solution to prepare the composite material.
Wherein S1:
(1) Mixing 4-nitrophthalimide with quinoline, adding urea, heating to 60 ℃ in a water bath, mechanically stirring for 15min, ultrasonically oscillating for 5min, placing in an oil bath pot, heating in the oil bath to 185 ℃, introducing nitrogen, adding copper chloride and ammonium molybdate, mechanically stirring for 4h, standing for 10min, filtering, washing with hydrogen chloride and sodium hydroxide for 4 times in sequence, washing with deionized water to neutrality, placing in an oven, drying at 80 ℃ for 25min, placing in N, N-dimethylformamide, heating in the water bath to 55 ℃, adding sodium sulfide nonahydrate, mechanically stirring for 35min, ultrasonically oscillating for 15min, standing for 2h, filtering, washing with deionized water for 4 times, placing in the oven, and drying at 60 ℃ for 3h to obtain a substance A;
(2) Placing chitosan in acetic acid water solution, mechanically stirring for 15min, adding substance A, heating in water bath to 40deg.C, mechanically stirring for 13min, ultrasonic oscillating for 5min, adding glutaraldehyde, heating in water bath to 80deg.C, mechanically stirring for 25min, and standing for 2 hr to obtain chitosan compound;
wherein S2:
(1) Placing 8 parts of carbon fibers in a Soxhlet extractor, adding an acetone solution, heating to 80 ℃, refluxing for 50 hours, placing in an oven, and drying for 4 hours at 60 ℃ for later use;
(2) Placing 8 parts of chitosan compound in N, N-dimethylformamide, mechanically stirring for 15min, adding 1.5 parts of 9, 10-dihydro-9 oxa-10-phosphaphenanthrene-10-oxide, placing in an oil bath pot, heating the oil bath to 150 ℃, stopping heating after heating for 10min, mechanically stirring for 25min, standing for 2h, adding the carbon fiber treated in step (1), mechanically stirring for 3h, and performing ultrasonic vibration for 40min to obtain a mixture;
wherein, S3:
(1) Heating triglycidyl para-aminophenol to 75 ℃ in a water bath, adding 3, 5-diethyl-2, 4-toluenediamine, 3, 5-diethyl-2, 6-toluenediamine, diaminodiphenyl sulfone and diethyl tetramethylimidazole, and mechanically stirring for 2 hours to obtain epoxy resin glue solution;
(2) And (3) mixing the mixture with 40 parts of epoxy resin glue solution, heating in a water bath to 85 ℃, carrying out ultrasonic vibration for 30min, mechanically stirring for 7h, and curing to obtain the composite material.
Example 3
The preparation method of the high-temperature-resistant carbon fiber composite material comprises the following steps:
s1: preparing a chitosan compound from 4-nitrophthalimide, urea, copper chloride and chitosan;
s2: reacting carbon fiber with chitosan complex and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to prepare a mixture;
s3: and (3) blending the mixture with epoxy resin glue solution to prepare the composite material.
Wherein S1:
(1) Mixing 4-nitrophthalimide with quinoline, adding urea, heating to 60 ℃ in a water bath, mechanically stirring for 20min, ultrasonically oscillating for 5min, placing in an oil bath pot, heating in the oil bath to 185 ℃, introducing nitrogen, adding copper chloride and ammonium molybdate, mechanically stirring for 4h, standing for 10min, filtering, washing with hydrogen chloride and sodium hydroxide for 4 times in sequence, washing with deionized water to neutrality, placing in an oven, drying at 80 ℃ for 30min, placing in N, N-dimethylformamide, heating in the water bath to 55 ℃, adding sodium sulfide nonahydrate, mechanically stirring for 40min, ultrasonically oscillating for 20min, standing for 2h, filtering, washing with deionized water for 4 times, placing in the oven, and drying at 60 ℃ for 3h to obtain a substance A;
(2) Placing chitosan in acetic acid water solution, mechanically stirring for 20min, adding substance A, heating in water bath to 40deg.C, mechanically stirring for 15min, ultrasonic oscillating for 5min, adding glutaraldehyde, heating in water bath to 80deg.C, mechanically stirring for 30min, and standing for 2 hr to obtain chitosan compound;
wherein S2:
(1) Placing 10 parts of carbon fiber in a Soxhlet extractor, adding an acetone solution, heating to 80 ℃, refluxing for 60 hours, placing in an oven, and drying for 4 hours at 60 ℃ for later use;
(2) Placing 9 parts of chitosan compound in N, N-dimethylformamide, mechanically stirring for 20min, adding 2 parts of 9, 10-dihydro-9 oxa-10-phosphaphenanthrene-10-oxide, placing in an oil bath pot, heating to 150 ℃ in an oil bath, stopping heating after heating for 10min, mechanically stirring for 30min, standing for 2h, adding the carbon fiber treated in step (1), mechanically stirring for 3h, and carrying out ultrasonic vibration for 40min to obtain a mixture;
wherein, S3:
(1) Heating triglycidyl para-aminophenol to 75 ℃ in a water bath, adding 3, 5-diethyl-2, 4-toluenediamine, 3, 5-diethyl-2, 6-toluenediamine, diaminodiphenyl sulfone and diethyl tetramethylimidazole, and mechanically stirring for 1-2 hours to obtain epoxy resin glue solution;
(2) And (3) mixing the mixture with 45 parts of epoxy resin glue solution, heating in a water bath to 85 ℃, carrying out ultrasonic vibration for 30min, mechanically stirring for 8h, and curing to obtain the composite material.
Comparative example 1
The preparation method of the high-temperature-resistant carbon fiber composite material comprises the following steps:
s1: and (3) blending the carbon fiber, chitosan, 9, 10-dihydro-9 oxa-10-phosphaphenanthrene-10-oxide and the epoxy resin glue solution to prepare the composite material.
Wherein S1:
(1) Placing carbon fiber in a Soxhlet extractor, adding acetone solution, heating to 80 ℃, refluxing for 50 hours, placing in an oven, and drying at 60 ℃ for 4 hours for later use;
(2) Heating triglycidyl para-aminophenol to 75 ℃ in a water bath, adding 3, 5-diethyl-2, 4-toluenediamine, 3, 5-diethyl-2, 6-toluenediamine, diaminodiphenyl sulfone and diethyl tetramethylimidazole, and mechanically stirring for 2 hours to obtain epoxy resin glue solution;
(3) 8 parts of carbon fiber, 8 parts of chitosan, 1.5 parts of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 40 parts of epoxy resin glue solution are mixed, heated to 85 ℃ in a water bath, ultrasonically vibrated for 30min, mechanically stirred for 7h, and cured to obtain the composite material.
Comparative example 2
The preparation method of the high-temperature-resistant carbon fiber composite material comprises the following steps:
s1: preparing a chitosan compound from 4-nitrophthalimide, urea, copper chloride and chitosan;
s2: reacting carbon fiber with chitosan complex to obtain a mixture;
s3: and (3) blending the mixture with epoxy resin glue solution to prepare the composite material.
Wherein S1:
(1) Mixing 4-nitrophthalimide with quinoline, adding urea, heating to 60 ℃ in a water bath, mechanically stirring for 15min, ultrasonically oscillating for 5min, placing in an oil bath pot, heating in the oil bath to 185 ℃, introducing nitrogen, adding copper chloride and ammonium molybdate, mechanically stirring for 4h, standing for 10min, filtering, washing with hydrogen chloride and sodium hydroxide for 4 times in sequence, washing with deionized water to neutrality, placing in an oven, drying at 80 ℃ for 25min, placing in N, N-dimethylformamide, heating in the water bath to 55 ℃, adding sodium sulfide nonahydrate, mechanically stirring for 35min, ultrasonically oscillating for 15min, standing for 2h, filtering, washing with deionized water for 4 times, placing in the oven, and drying at 60 ℃ for 3h to obtain a substance A;
(2) Placing chitosan in acetic acid water solution, mechanically stirring for 15min, adding substance A, heating in water bath to 40deg.C, mechanically stirring for 13min, ultrasonic oscillating for 5min, adding glutaraldehyde, heating in water bath to 80deg.C, mechanically stirring for 25min, and standing for 2 hr to obtain chitosan compound;
wherein S2:
(1) Placing carbon fiber in a Soxhlet extractor, adding acetone solution, heating to 80 ℃, refluxing for 50 hours, placing in an oven, and drying at 60 ℃ for 4 hours for later use;
(2) Placing 8 parts of chitosan compound in N, N-dimethylformamide, mechanically stirring for 15min, adding 8 parts of carbon fiber treated in the step (1), mechanically stirring for 3h, and ultrasonically oscillating for 40min to obtain a mixture;
wherein, S3:
(1) Heating triglycidyl para-aminophenol to 75 ℃ in a water bath, adding 3, 5-diethyl-2, 4-toluenediamine, 3, 5-diethyl-2, 6-toluenediamine, diaminodiphenyl sulfone and diethyl tetramethylimidazole, and mechanically stirring for 2 hours to obtain epoxy resin glue solution;
(2) And (3) mixing the mixture with 40 parts of epoxy resin glue solution, heating in a water bath to 85 ℃, carrying out ultrasonic vibration for 30min, mechanically stirring for 7h, and curing to obtain the composite material.
Comparative example 3
The preparation method of the high-temperature-resistant carbon fiber composite material comprises the following steps:
s1: and (3) blending the carbon fiber, chitosan and epoxy resin glue solution to prepare the composite material.
Wherein S1:
(1) Placing carbon fiber in a Soxhlet extractor, adding acetone solution, heating to 80 ℃, refluxing for 50 hours, placing in an oven, and drying at 60 ℃ for 4 hours for later use;
(2) Heating triglycidyl para-aminophenol to 75 ℃ in a water bath, adding 3, 5-diethyl-2, 4-toluenediamine, 3, 5-diethyl-2, 6-toluenediamine, diaminodiphenyl sulfone and diethyl tetramethylimidazole, and mechanically stirring for 2 hours to obtain epoxy resin glue solution;
(3) 8 parts of carbon fiber, 8 parts of chitosan and 40 parts of epoxy resin glue solution are mixed, heated in a water bath to 85 ℃, subjected to ultrasonic vibration for 30min, mechanically stirred for 7h, and cured to obtain the composite material.
Experiment one (high temperature resistance)
Using examples 1 to 3 and comparative examples 1 to 3 as experimental samples, the samples were prepared to have dimensions of 15mm by 3mm in length and width and height, placed in an oven, heated to 150 ℃, and the shear strength of the samples was measured and recorded.
Experiment II (flame retardant property)
The combustion behavior was measured according to GB/T2406.2-2009 oxygen index method for plastics, part 2, using examples 1 to 3 and comparative examples 1 to 3 as experimental samples: room temperature experiments test samples were tested and data recorded.
Experiment III (antistatic Property)
Samples were tested and data recorded in accordance with GB/T15738-1995 test method for conductivity of conductive and antistatic fiber-reinforced plastics, using examples 1 to 3 and comparative examples 1 to 3 as experimental samples.
Experimental data
Data analysis
From the data, examples 1 to 3 were found to have the best heat resistance, flame retardancy and antistatic properties, and example 2 was found to have the best properties;
compared with the embodiment 2, the comparative example 1 lacks the copper tetraminophthalocyanine prepared from 4-nitrophthalimide, urea and copper chloride, so that the interface strength between the carbon fiber and the epoxy resin is low, the glass transition temperature is very easy to damage, the shear strength is low, the copper and the carbon fiber are lack to form a conductive network, the volume resistivity is poor, and the 9, 10-dihydro-9 oxa-10-phosphaphenanthrene-10-oxide is easy to fall off, and the flame retardant effect is poor;
the lack of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in comparative example 2 resulted in poor flame retardant efficiency compared to example 2;
in comparison to example 2, comparative example 3 lacks 4-nitrophthalimide, urea, copper chloride and 9, 10-dihydro-9 oxa-10-phosphaphenanthrene-10-oxide, which performs the worst;
in conclusion, the high-temperature-resistant carbon fiber composite material prepared by the invention has the advantages of improving the glass transition temperature of the interface and the high-temperature resistance of the composite material by enhancing the interface crosslinking and strength between the carbon fiber and the resin matrix, and has good practicability and production value.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. The high temperature resistant carbon fiber composite material is characterized in that: the carbon fiber composite material comprises, by weight, 35-45 parts of epoxy resin glue solution, 1-2 parts of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 7-9 parts of chitosan composite and 5-10 parts of carbon fiber;
the chitosan compound is prepared from chitosan, 4-nitrophthalimide, urea and copper chloride;
the epoxy resin glue solution is prepared from triglycidyl para-aminophenol, 3, 5-diethyl-2, 4-toluenediamine, 3, 5-diethyl-2, 6-toluenediamine, diaminodiphenyl sulfone and diethyl tetramethyl imidazole;
the preparation method of the high-temperature-resistant carbon fiber composite material comprises the following steps: the method comprises the following steps: s1: preparing a chitosan compound from 4-nitrophthalimide, urea, copper chloride and chitosan; s2: reacting carbon fiber with chitosan complex and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to prepare a mixture; s3: blending the mixture with epoxy resin to prepare a composite material;
the S1: (1) Mixing 4-nitrophthalimide with quinoline, adding urea, heating in a water bath, stirring uniformly, ultrasonically oscillating, placing in an oil bath pot, heating in the oil bath, introducing nitrogen, adding copper chloride and ammonium molybdate, stirring uniformly, standing for a period of time, filtering, washing, drying, placing in N, N-dimethylformamide, heating in the water bath, adding sodium sulfide nonahydrate, stirring uniformly, ultrasonically oscillating, standing for a period of time, filtering, flushing and drying to obtain a substance A; (2) Placing chitosan into an acetic acid aqueous solution, uniformly stirring, adding a substance A, heating in a water bath, uniformly stirring, ultrasonically oscillating, adding glutaraldehyde, heating in the water bath, uniformly stirring, and standing for a period of time to obtain a chitosan compound; the S2: (1) Placing carbon fiber in a Soxhlet extractor, adding acetone solution, heating, refluxing for a period of time, and drying for use; (2) Placing the chitosan compound in N, N-dimethylformamide, uniformly stirring, adding 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, placing in an oil bath pot, heating in the oil bath, heating for a period of time, uniformly stirring, standing for a period of time, adding the carbon fiber treated in step (1), uniformly stirring, and performing ultrasonic vibration to obtain a mixture; the S3: (1) Heating triglycidyl para-aminophenol in a water bath, adding 3, 5-diethyl-2, 4-toluenediamine, 3, 5-diethyl-2, 6-toluenediamine, diaminodiphenyl sulfone and diethyl tetramethylimidazole, and uniformly stirring to obtain epoxy resin glue solution; (2) And (3) mixing the mixture with epoxy resin glue solution, heating in a water bath, carrying out ultrasonic vibration, uniformly stirring, and curing to obtain the composite material.
2. The method for preparing the high-temperature-resistant carbon fiber composite material according to claim 1, which is characterized in that: the S1: (1) Mixing 4-nitrophthalimide with quinoline, adding urea, heating to 60 ℃ in a water bath, mechanically stirring for 10-20 min, ultrasonically oscillating for 5min, placing in an oil bath pot, heating to 185 ℃ in the oil bath, introducing nitrogen, adding copper chloride and ammonium molybdate, mechanically stirring for 3-4 h, standing for 10min, filtering, washing with hydrogen chloride and sodium hydroxide for 3-4 times in sequence, washing with deionized water to neutrality, placing in an oven, drying at 80 ℃ for 20-30 min, placing in N, N-dimethylformamide, heating to 55 ℃ in a water bath, adding sodium sulfide nonahydrate, mechanically stirring for 30-40 min, ultrasonically oscillating for 10-20 min, standing for 1-2 h, filtering, washing with deionized water for 3-4 times, placing in the oven, and drying at 60 ℃ for 3h to obtain a substance A; (2) Placing chitosan into an acetic acid aqueous solution, mechanically stirring for 10-20 min, adding a substance A, heating in a water bath to 40 ℃, mechanically stirring for 10-15 min, ultrasonically oscillating for 5min, adding glutaraldehyde, heating in a water bath to 80 ℃, mechanically stirring for 20-30 min, and standing for 1-2 h to obtain a chitosan compound; the S2: (1) Placing the carbon fiber in a Soxhlet extractor, adding an acetone solution, heating to 80 ℃, refluxing for 40-60 hours, placing in an oven, and drying at 60 ℃ for 3-4 hours for later use; (2) Placing the chitosan compound in N, N-dimethylformamide, mechanically stirring for 10-20 min, adding 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, placing in an oil bath pot, heating the oil bath to 150 ℃, stopping heating after heating for 10min, mechanically stirring for 20-30 min, standing for 1-2 h, adding the carbon fiber treated in step (1), mechanically stirring for 2-3 h, and carrying out ultrasonic oscillation for 40min to obtain a mixture; the S3: (1) Heating triglycidyl para-aminophenol to 75 ℃ in a water bath, adding 3, 5-diethyl-2, 4-toluenediamine, 3, 5-diethyl-2, 6-toluenediamine, diaminodiphenyl sulfone and diethyl tetramethylimidazole, and mechanically stirring for 1-2 hours to obtain epoxy resin glue solution; (2) And (3) mixing the mixture with epoxy resin glue solution, heating in a water bath to 85 ℃, carrying out ultrasonic oscillation for 30min, mechanically stirring for 6-8 h, and curing to obtain the composite material.
3. The method for preparing the high-temperature-resistant carbon fiber composite material according to claim 2, which is characterized in that: the curing in the step S3 is staged curing, and the first stage is: curing for 2h at 80 ℃; and a second stage: curing for 3 hours at 100 ℃; and a third stage: curing for 2h at 130 ℃; fourth stage: curing at 170℃for 1h.
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