CN110804195A - Preparation method of polymer fiber reinforced resin matrix composite material - Google Patents
Preparation method of polymer fiber reinforced resin matrix composite material Download PDFInfo
- Publication number
- CN110804195A CN110804195A CN201911076503.6A CN201911076503A CN110804195A CN 110804195 A CN110804195 A CN 110804195A CN 201911076503 A CN201911076503 A CN 201911076503A CN 110804195 A CN110804195 A CN 110804195A
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- China
- Prior art keywords
- fiber
- parts
- resin
- product
- weight
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 239000011347 resin Substances 0.000 title claims abstract description 121
- 229920005989 resin Polymers 0.000 title claims abstract description 121
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 239000011159 matrix material Substances 0.000 title claims abstract description 30
- 229920005594 polymer fiber Polymers 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000835 fiber Substances 0.000 claims abstract description 97
- 239000000047 product Substances 0.000 claims abstract description 83
- 238000010438 heat treatment Methods 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000011265 semifinished product Substances 0.000 claims abstract description 17
- 238000005507 spraying Methods 0.000 claims abstract description 12
- 238000005520 cutting process Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 59
- 229920006231 aramid fiber Polymers 0.000 claims description 57
- 238000003756 stirring Methods 0.000 claims description 34
- 238000001035 drying Methods 0.000 claims description 29
- 239000011491 glass wool Substances 0.000 claims description 27
- 239000003292 glue Substances 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 150000003943 catecholamines Chemical class 0.000 claims description 20
- 238000001723 curing Methods 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- 239000000654 additive Substances 0.000 claims description 15
- 230000000996 additive effect Effects 0.000 claims description 15
- 239000011230 binding agent Substances 0.000 claims description 15
- 238000004140 cleaning Methods 0.000 claims description 15
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 230000004224 protection Effects 0.000 claims description 12
- HWSSEYVMGDIFMH-UHFFFAOYSA-N 2-[2-[2-(2-methylprop-2-enoyloxy)ethoxy]ethoxy]ethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOCCOCCOC(=O)C(C)=C HWSSEYVMGDIFMH-UHFFFAOYSA-N 0.000 claims description 11
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 11
- 239000005977 Ethylene Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000006229 carbon black Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 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 claims description 10
- KOGSPLLRMRSADR-UHFFFAOYSA-N 4-(2-aminopropan-2-yl)-1-methylcyclohexan-1-amine Chemical compound CC(C)(N)C1CCC(C)(N)CC1 KOGSPLLRMRSADR-UHFFFAOYSA-N 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- KTPIWUHKYIJBCR-UHFFFAOYSA-N bis(oxiran-2-ylmethyl) cyclohex-4-ene-1,2-dicarboxylate Chemical compound C1C=CCC(C(=O)OCC2OC2)C1C(=O)OCC1CO1 KTPIWUHKYIJBCR-UHFFFAOYSA-N 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 10
- 239000003822 epoxy resin Substances 0.000 claims description 10
- 239000003063 flame retardant Substances 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 229920000647 polyepoxide Polymers 0.000 claims description 10
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 9
- 239000010436 fluorite Substances 0.000 claims description 9
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052622 kaolinite Inorganic materials 0.000 claims description 9
- 239000002480 mineral oil Substances 0.000 claims description 9
- 235000010446 mineral oil Nutrition 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- KMZHZAAOEWVPSE-UHFFFAOYSA-N 2,3-dihydroxypropyl acetate Chemical compound CC(=O)OCC(O)CO KMZHZAAOEWVPSE-UHFFFAOYSA-N 0.000 claims description 8
- 229910001868 water Inorganic materials 0.000 claims description 8
- 238000009826 distribution Methods 0.000 claims description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 7
- 239000012498 ultrapure water Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000007598 dipping method Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- SYHVBRQKMHIAJQ-UHFFFAOYSA-N 3-(2-aminoethyl)benzene-1,2-diol Chemical compound NCCC1=CC=CC(O)=C1O SYHVBRQKMHIAJQ-UHFFFAOYSA-N 0.000 claims description 5
- QCWCRPNKAZULNF-UHFFFAOYSA-N 3-aminobenzene-1,2-diol;hydrochloride Chemical compound Cl.NC1=CC=CC(O)=C1O QCWCRPNKAZULNF-UHFFFAOYSA-N 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- 150000008430 aromatic amides Chemical class 0.000 claims description 5
- 239000003518 caustics Substances 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 claims description 5
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
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- 238000007865 diluting Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- DATAGRPVKZEWHA-YFKPBYRVSA-N N(5)-ethyl-L-glutamine Chemical compound CCNC(=O)CC[C@H]([NH3+])C([O-])=O DATAGRPVKZEWHA-YFKPBYRVSA-N 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000002121 nanofiber Substances 0.000 description 4
- 239000012466 permeate Substances 0.000 description 4
- 229920001519 homopolymer Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229940026510 theanine Drugs 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- 230000006750 UV protection Effects 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000000805 composite resin Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- VNQXSTWCDUXYEZ-UHFFFAOYSA-N 1,7,7-trimethylbicyclo[2.2.1]heptane-2,3-dione Chemical compound C1CC2(C)C(=O)C(=O)C1C2(C)C VNQXSTWCDUXYEZ-UHFFFAOYSA-N 0.000 description 1
- FRPZMMHWLSIFAZ-UHFFFAOYSA-N 10-undecenoic acid Chemical compound OC(=O)CCCCCCCCC=C FRPZMMHWLSIFAZ-UHFFFAOYSA-N 0.000 description 1
- GCYHRYNSUGLLMA-UHFFFAOYSA-N 2-prop-2-enoxyethanol Chemical compound OCCOCC=C GCYHRYNSUGLLMA-UHFFFAOYSA-N 0.000 description 1
- 229920002748 Basalt fiber Polymers 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- AMFGWXWBFGVCKG-UHFFFAOYSA-N Panavia opaque Chemical compound C1=CC(OCC(O)COC(=O)C(=C)C)=CC=C1C(C)(C)C1=CC=C(OCC(O)COC(=O)C(C)=C)C=C1 AMFGWXWBFGVCKG-UHFFFAOYSA-N 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 150000008062 acetophenones Chemical class 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229930006711 bornane-2,3-dione Natural products 0.000 description 1
- KHAVLLBUVKBTBG-UHFFFAOYSA-N caproleic acid Natural products OC(=O)CCCCCCCC=C KHAVLLBUVKBTBG-UHFFFAOYSA-N 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- -1 coatings Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229960002703 undecylenic acid Drugs 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/047—Reinforcing macromolecular compounds with loose or coherent fibrous material with mixed fibrous material
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/368—Hydroxyalkylamines; Derivatives thereof, e.g. Kritchevsky bases
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- 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
- C08K7/26—Silicon- containing compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
- D06M2101/36—Aromatic polyamides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Textile Engineering (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Reinforced Plastic Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
A preparation method of a polymer fiber reinforced resin matrix composite material comprises the following steps: (1) preparing a first mixed resin; (2) heating the first mixed resin, and spraying the heated first mixed resin on fiber products made of multiple materials; (3) carrying out primary curing on the wet fiber product; (4) cutting the first solidified fiber product into a specific shape to form a semi-finished product; (5) preparing a second mixed resin; (6) and heating the second mixed resin, and spraying the heated second mixed resin onto the semi-finished product to obtain the final polymer fiber reinforced resin matrix composite. The preparation method provided by the invention is simple, the production cost is low, and the prepared polymer fiber reinforced resin matrix composite material can effectively improve the interface performance and strength and toughness, and has practical application value.
Description
Technical Field
The invention belongs to the technical field of high polymer material processing, and particularly relates to a preparation method of a high polymer fiber reinforced resin matrix composite.
Background
The resin-based composite material is a fiber reinforced material taking an organic polymer as a matrix, has excellent mechanical properties, and is usually made of fiber reinforcements such as glass wool, carbon fiber, basalt fiber or aramid fiber. The resin-based composite material has wide application in aviation, automobile and marine industries.
The existing forming method of the fiber reinforced resin matrix composite material, such as autoclave, prepreg, RTM and the like, has the defects of multiple forming procedures, long time, low efficiency, incapability of meeting the increasing requirements of mass production and application, higher manufacturing cost and limitation on the application range of the fiber reinforced resin matrix composite material.
Therefore, a preparation method of the fiber reinforced resin matrix composite material with simple processing technology and higher production efficiency is urgently needed in the field of processing of high polymer materials at present.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a polymer fiber reinforced resin matrix composite. The preparation method provided by the invention is simple, the production cost is low, and the prepared polymer fiber reinforced resin matrix composite material can effectively improve the interface performance and strength and toughness, and has practical application value.
The technical scheme adopted by the invention for solving the technical problems is a preparation method of a polymer fiber reinforced resin matrix composite, which comprises the following steps:
(1) preparing the following raw materials in parts by weight: 35-40 parts of ultra-high molecular weight PE resin, 5-8 parts of F-type epoxy resin, 15-20 parts of fluorocarbon resin, 2-2.5 parts of 1, 6-dihydroxyhexane, 0.2-0.3 part of nano titanium dioxide, 0.8-1 part of nano white carbon black and 6-8 parts of curing agent; heating and melting the ultra-high molecular weight PE resin in parts by weight at 70-80 ℃, cooling to 35-40 ℃ for protection, adding the F-type epoxy resin and the fluorocarbon resin in parts by weight, mixing and stirring at a rotating speed of 200-250 r/min for 1-2 hours, then adding other raw materials, uniformly stirring, and standing for 1-2 hours to obtain a first mixed resin;
(2) heating the mixed resin, spraying the heated mixed resin onto fiber products made of multiple materials, and stacking the fiber products made of the multiple materials together to form a wet fiber product;
(3) curing the wet fiber product for the first time to promote the first mixed resin to be cured, and then reducing the temperature to room temperature to obtain a first cured fiber product;
(4) cutting the first solidified fiber product into a specific shape, then sequentially overlapping a plurality of layers of the first solidified fiber products with the specific shape, and pressurizing to promote the first solidified fiber products of each layer to be mutually adhered to form a semi-finished product;
(5) preparing the following raw materials in parts by weight: 70-80 parts of tetrahydrophthalic acid diglycidyl ester, 20-30 parts of triethylene glycol dimethacrylate and 30-40 parts of 1, 8-menthane diamine, heating and melting the tetrahydrophthalic acid diglycidyl ester and the triethylene glycol dimethacrylate in parts by weight, cooling to 35-40 ℃ for protection, adding the 1, 8-menthane diamine in parts by weight, mixing and stirring at the rotating speed of 200-250 r/min for 1-2 hours, and standing to obtain a second mixed resin;
(6) and heating the second mixed resin, spraying the heated second mixed resin onto the semi-finished product, heating the semi-finished product to the curing temperature under a pressurized state, and performing secondary curing on the second mixed resin to obtain the final polymer fiber reinforced resin matrix composite.
Preferably, the fiber product is prepared by the following steps: uniformly mixing glass wool and modified aramid fiber, dispersing, dehydrating and drying to obtain the aramid fiber with the quantitative content of 45-48 g/m2The original product of (2); the length of the glass wool is 7-8 mm, and the diameter of the glass wool is 8-10 mu m; the length of the aramid fiber is 5-6 mm, and the diameter of the aramid fiber is 12-15 mu m; wherein the glass wool accounts for 40-45% of the total mass of the glass wool and the aramid fiber; will be provided withAfter the binder is diluted, sequentially adding a flame retardant into the binder to form a glue solution, wherein the mass fraction of the binder is 8-10%, and the mass fraction of the flame retardant is 7-8%; and completely immersing the original product into the glue solution for glue dipping to enable the glue solution to fully permeate into fibers, sucking the glue solution on the surface of the dipped original product to obtain a wet product, and drying the wet product to obtain a fiber product.
In any of the above embodiments, preferably, the ultra-high molecular weight PE resin is prepared by: heating a reaction container to a reaction temperature, vacuumizing, replacing with nitrogen, adding gasoline, an additive and a catalyst, wherein the mass ratio of ethylene to gasoline to the additive is 10: 12-15: 1-2, uniformly stirring, introducing nitrogen, continuously adding ethylene into the reaction container, controlling the pressure to be 1-1.2 MPa, reacting for 2.5-3 hours at the reaction temperature, rapidly cooling to 25-30 ℃ after the reaction is finished, filtering out the gasoline to obtain a liquid, and drying the liquid to obtain the ultra-high molecular weight PE resin, wherein the reaction temperature is 60-70 ℃.
In any of the above schemes, preferably, the additive comprises a mixture of microcrystalline kaolinite, mineral oil and fluorite powder, the weight ratio of the mixture is 2-3: 2-4: 1, and the stirring speed is 500-700 r/min.
In any of the above embodiments, the ultra-high molecular weight PE resin preferably has a viscosity average molecular weight of 500 to 600 ten thousand, an average particle diameter of 150 to 200 μm, a particle diameter distribution width (d90-d10)/d 50: 1 to 1.5, and a bulk density of 0.3 to 0.5g/cm3。
In any of the above embodiments, preferably, the modified aramid fiber is prepared by: immersing 1 part of aramid fiber into 120-150 parts of caustic alkali and 820-850 parts of ultrapure water by weight, and reacting for 5-6 h at the temperature of 50-60 ℃; after the reaction is finished, taking out the fiber, cleaning and drying; preparing a catecholamine solution by adopting a buffer reagent, water and catecholamine hydrochloride; soaking the dried aramid fiber in a catechol ethylamine solution, and oscillating for 10-12 h at the temperature of 20-30 ℃; after the reaction is finished, taking out the fiber, and cleaning and drying the fiber to obtain the aromatic amide fiber coated by the catecholamine; dispersing graphite acid in the acetin by mass under the stirring condition, and performing ultrasonic treatment to obtain a dispersion liquid; adding 1 part of theafenoxamine-coated aramid fiber into the dispersion liquid, and reacting for 4-5 hours at the temperature of 55-60 ℃; and after the reaction is finished, taking out the fiber, and cleaning and drying to obtain the modified aramid fiber.
In any of the above embodiments, preferably, the concentration of the catecholamines solution is 2g/L to 3g/L, the mass ratio of the dried aramid fibers to the catecholamines is 3 to 5:1, and the mass ratio of the graphite acid to the acetophenones is 0.3 to 0.5: 100.
the invention is obtained according to years of practical application practice and experience, adopts the best technical means and measures to carry out combined optimization, obtains the optimal technical effect, is not simple superposition and splicing of technical characteristics, and has obvious significance.
The invention has the beneficial effects that:
1. the invention realizes the continuous compounding of different types of resin and fiber products made of various materials, greatly improves the forming efficiency, reduces manual working procedures, effectively improves the consistency of the products and meets the requirement of mass manufacturing.
2. The invention gives full play to the excellent performance of the glass wool and the modified aramid fiber, can fully utilize the characteristics of the raw materials, has simple preparation process and excellent performance of the prepared composite material.
3. The ultra-high molecular weight PE resin has controllable molecular weight and narrow molecular weight distribution, and has excellent performances of wear resistance, creep resistance, static resistance and the like superior to those of common resin; the preparation method of the invention has simple production process and is suitable for large-scale production.
4. The modified fiber used in the invention has outstanding ultraviolet resistance, obviously improves the surface activity of the aramid fiber, improves the interface acting force between the fiber and the resin, and provides a material guarantee for further modification and application of the fiber.
Detailed Description
The invention is further described with reference to specific examples, but the scope of the claims is not limited thereto.
Example 1
A preparation method of a polymer fiber reinforced resin matrix composite material comprises the following steps:
(1) preparing the following raw materials in parts by weight: 35 parts of ultra-high molecular weight PE resin, 5 parts of F-type epoxy resin, 15 parts of fluorocarbon resin, 2 parts of 1, 6-dihydroxyhexane, 0.2 part of nano titanium dioxide, 0.8 part of nano white carbon black and 6 parts of curing agent; heating and melting the ultra-high molecular weight PE resin in parts by weight at 70 ℃, cooling to 35 ℃ for protection, adding the F-type epoxy resin and the fluorocarbon resin in parts by weight, mixing and stirring at a rotating speed of 200r/min for 1h, then adding other raw materials, uniformly stirring, and standing for 1h to obtain first mixed resin;
(2) heating the mixed resin, spraying the heated mixed resin onto fiber products made of multiple materials, and stacking the fiber products made of the multiple materials together to form a wet fiber product;
(3) curing the wet fiber product for the first time to promote the first mixed resin to be cured, and then reducing the temperature to room temperature to obtain a first cured fiber product;
(4) cutting the first solidified fiber product into a specific shape, then sequentially overlapping a plurality of layers of the first solidified fiber products with the specific shape, and pressurizing to promote the first solidified fiber products of each layer to be mutually adhered to form a semi-finished product;
(5) preparing the following raw materials in parts by weight: 70 parts of tetrahydrophthalic acid diglycidyl ester, 20 parts of triethylene glycol dimethacrylate and 30 parts of 1, 8-menthane diamine, heating and melting the tetrahydrophthalic acid diglycidyl ester and the triethylene glycol dimethacrylate in parts by weight, cooling to 35 ℃ for protection, adding the 1, 8-menthane diamine in parts by weight, mixing and stirring at the rotating speed of 200r/min for 1 hour, and standing to obtain a second mixed resin;
(6) and heating the second mixed resin, spraying the heated second mixed resin onto the semi-finished product, heating the semi-finished product to the curing temperature under a pressurized state, and performing secondary curing on the second mixed resin to obtain the final polymer fiber reinforced resin matrix composite.
The fiber product is prepared by the following steps: mixing glass wool and modified aramid fiber, dispersing, dewatering, and oven drying to obtain the final product with a quantitative of 45g/m2The original product of (2); the length of the glass wool is 7mm, and the diameter of the glass wool is 8 mu m; the length of the aramid fiber is 5mm, and the diameter of the aramid fiber is 12 mu m; wherein the glass wool accounts for 40 percent of the total mass of the glass wool and the aramid fiber; diluting a binder, and sequentially adding a flame retardant into the binder to form a glue solution, wherein the mass fraction of the binder is 8%, and the mass fraction of the flame retardant is 7%; and completely immersing the original product into the glue solution for glue dipping to enable the glue solution to fully permeate into fibers, sucking the glue solution on the surface of the dipped original product to obtain a wet product, and drying the wet product to obtain a fiber product.
The ultra-high molecular weight PE resin is prepared by the following steps: heating a reaction vessel to a reaction temperature, vacuumizing, replacing with nitrogen, adding gasoline, an additive and a catalyst, wherein the mass ratio of the ethylene to the gasoline to the additive is 10:12:1, uniformly stirring, introducing nitrogen, finally continuously adding the ethylene into the reaction vessel, controlling the pressure to be 1MPa, reacting at the reaction temperature for 2.5 hours, after the reaction is finished, rapidly cooling to 25 ℃, filtering out the gasoline to obtain a liquid, and drying the liquid to obtain the ultra-high molecular weight PE resin, wherein the reaction temperature is 60 ℃.
The additive comprises a mixture of microcrystalline kaolinite, mineral oil and fluorite powder, the weight ratio of the microcrystalline kaolinite to the mineral oil to the fluorite powder is 2:2:1, and the stirring speed is 500 r/min.
The viscosity average molecular weight of the ultra-high molecular weight PE resin is 500 ten thousand, the average particle size is 150 mu m, and the particle size distribution width (d90-d10)/d 50: 1, bulk density 0.3g/cm3。
The modified aramid fiber is prepared by the following steps: immersing 1 part by weight of aramid fiber in 120 parts by weight of caustic alkali and 820 parts by weight of ultrapure water, and reacting at 50 ℃ for 5 hours; after the reaction is finished, taking out the fiber, cleaning and drying; preparing a catecholamine solution by adopting a buffer reagent, water and catecholamine hydrochloride; soaking the dried aramid fiber in a catechol ethylamine solution, and oscillating for 10 hours at the temperature of 20 ℃; after the reaction is finished, taking out the fiber, and cleaning and drying the fiber to obtain the aromatic amide fiber coated by the catecholamine; dispersing graphite acid in the acetin by mass under the stirring condition, and performing ultrasonic treatment to obtain a dispersion liquid; adding 1 part of theanine-coated aramid fiber into the dispersion liquid, and reacting for 4 hours at the temperature of 55 ℃; and after the reaction is finished, taking out the fiber, and cleaning and drying to obtain the modified aramid fiber.
The concentration of the catecholamine solution is 2g/L, the mass ratio of the dried aramid fiber to the catecholamine is 3:1, and the mass ratio of the graphite acid to the acetin is 0.3: 100.
example 2
A preparation method of a polymer fiber reinforced resin matrix composite material comprises the following steps:
(1) preparing the following raw materials in parts by weight: 38 parts of ultra-high molecular weight PE resin, 6.8 parts of F-type epoxy resin, 18 parts of fluorocarbon resin, 2.2 parts of 1, 6-dihydroxyhexane, 0.24 part of nano titanium dioxide, 0.9 part of nano white carbon black and 6.7 parts of curing agent; heating and melting the ultra-high molecular weight PE resin in parts by weight at 72 ℃, cooling to 39 ℃ for protection, adding the F-type epoxy resin and the fluorocarbon resin in parts by weight, mixing and stirring at a rotating speed of 236r/min for 1.2h, then adding other raw materials, uniformly stirring, and standing for 1.6h to obtain a first mixed resin;
(2) heating the mixed resin, spraying the heated mixed resin onto fiber products made of multiple materials, and stacking the fiber products made of the multiple materials together to form a wet fiber product;
(3) curing the wet fiber product for the first time to promote the first mixed resin to be cured, and then reducing the temperature to room temperature to obtain a first cured fiber product;
(4) cutting the first solidified fiber product into a specific shape, then sequentially overlapping a plurality of layers of the first solidified fiber products with the specific shape, and pressurizing to promote the first solidified fiber products of each layer to be mutually adhered to form a semi-finished product;
(5) preparing the following raw materials in parts by weight: 73 parts of tetrahydrophthalic acid diglycidyl ester, 25 parts of triethylene glycol dimethacrylate and 37 parts of 1, 8-menthane diamine, heating and melting the tetrahydrophthalic acid diglycidyl ester and the triethylene glycol dimethacrylate in parts by weight, cooling to 38 ℃ for protection, adding the 1, 8-menthane diamine in parts by weight, mixing and stirring at the rotating speed of 240r/min for 1.5h, and standing to obtain a second mixed resin;
(6) and heating the second mixed resin, spraying the heated second mixed resin onto the semi-finished product, heating the semi-finished product to the curing temperature under a pressurized state, and performing secondary curing on the second mixed resin to obtain the final polymer fiber reinforced resin matrix composite.
The fiber product is prepared by the following steps: mixing glass wool and modified aramid fiber, dispersing, dewatering and stoving to obtain the product with quantitative content of 46.5g/m2The original product of (2); the length of the glass wool is 7.5mm, and the diameter is 9 mu m; the length of the aramid fiber is 5.5mm, and the diameter of the aramid fiber is 14 mu m; wherein the glass wool accounts for 45 percent of the total mass of the glass wool and the aramid fiber; diluting a binder, and sequentially adding a flame retardant into the binder to form a glue solution, wherein the mass fraction of the binder is 10%, and the mass fraction of the flame retardant is 7%; and completely immersing the original product into the glue solution for glue dipping to enable the glue solution to fully permeate into fibers, sucking the glue solution on the surface of the dipped original product to obtain a wet product, and drying the wet product to obtain a fiber product.
The ultra-high molecular weight PE resin is prepared by the following steps: heating a reaction vessel to a reaction temperature, vacuumizing, replacing with nitrogen, adding gasoline, an additive and a catalyst, wherein the mass ratio of the ethylene to the gasoline to the additive is 10:13:1.2, uniformly stirring, introducing nitrogen, finally continuously adding the ethylene into the reaction vessel, controlling the pressure to be 1MPa, reacting at the reaction temperature for 2.6 hours, after the reaction is finished, rapidly cooling to 28 ℃, filtering out the gasoline to obtain a liquid, and drying the liquid to obtain the ultra-high molecular weight PE resin, wherein the reaction temperature is 66 ℃.
The additive comprises a mixture of microcrystalline kaolinite, mineral oil and fluorite powder, the weight ratio of the microcrystalline kaolinite to the mineral oil to the fluorite powder is 2.5:3:1, and the stirring speed is 600 r/min.
Viscosity of the ultra-high molecular weight PE resinAverage molecular weight of 500 ten thousand, average particle diameter of 200 μm, particle size distribution width (d90-d10)/d 50: 1, bulk density 0.4g/cm3。
The modified aramid fiber is prepared by the following steps: immersing 1 part by weight of aramid fiber in 130 parts by weight of caustic alkali and 840 parts by weight of ultrapure water, and reacting at 55 ℃ for 5.5 hours; after the reaction is finished, taking out the fiber, cleaning and drying; preparing a catecholamine solution by adopting a buffer reagent, water and catecholamine hydrochloride; soaking the dried aramid fiber in a catechol ethylamine solution, and oscillating for 12h at the temperature of 20 ℃; after the reaction is finished, taking out the fiber, and cleaning and drying the fiber to obtain the aromatic amide fiber coated by the catecholamine; dispersing graphite acid in the acetin by mass under the stirring condition, and performing ultrasonic treatment to obtain a dispersion liquid; adding 1 part of theanine-coated aramid fiber into the dispersion liquid, and reacting for 4 hours at the temperature of 55 ℃; and after the reaction is finished, taking out the fiber, and cleaning and drying to obtain the modified aramid fiber.
The concentration of the catecholamine solution is 3g/L, the mass ratio of the dried aramid fiber to the catecholamine is 5:1, and the mass ratio of the graphite acid to the acetin is 0.4: 100.
in addition, in order to further improve the effect, the nano white carbon black is prepared by the following steps:
(1) adding ultrapure water into ethanol, and uniformly oscillating by ultrasonic to obtain a first solution;
(2) adding tetraethyl silicate into the first solution under ultrasonic oscillation, wherein the molar ratio of the tetraethyl silicate to ethanol is 1: 65, the molar ratio of the tetraethyl silicate to ultrapure water is 1: 5, and uniformly performing ultrasonic oscillation to obtain a second solution;
(3) regulating the pH value of the second solution to 3.8 by using hydrochloric acid with the concentration of 0.2mol/L, dropwise adding a silane coupling agent into the second solution at the speed of 1.2g/min, wherein the using amount of the silane coupling agent is 10% of the mass of tetraethyl silicate, and then stirring and reacting at the reaction temperature of 45 ℃ for 5 hours to obtain a third solution;
(4) with NH at a concentration of 0.08mol/L3·H2O adjusting the pH of the third solution to8, reacting for 2.5 hours under the condition of heat preservation to obtain nano white carbon black sol;
(5) drying, crushing and screening the nano white carbon black sol, centrifugally washing with absolute ethyl alcohol, washing with water again, drying for 18h in vacuum at 55 ℃, and grinding to obtain the final nano white carbon black.
The preparation method of the nano white carbon black has the advantages of simple process flow, mild process conditions, strong operability and high production efficiency, is suitable for industrial production, improves the reaction efficiency, improves the phenomenon that nano inorganic particles are incompatible with organic phases, can uniformly disperse nano white carbon black particles in oil-water two phases, and can be widely applied to various fields of plastics, coatings, medicines, environmental protection and the like.
Example 3
A preparation method of a polymer fiber reinforced resin matrix composite material comprises the following steps:
(1) preparing the following raw materials in parts by weight: 40 parts of ultra-high molecular weight PE resin, 8 parts of F-type epoxy resin, 20 parts of fluorocarbon resin, 2.5 parts of 1, 6-dihydroxyhexane, 0.3 part of nano titanium dioxide, 1 part of nano white carbon black and 8 parts of curing agent; heating and melting the ultra-high molecular weight PE resin in parts by weight at 80 ℃, cooling to 40 ℃ for protection, adding the F-type epoxy resin and the fluorocarbon resin in parts by weight, mixing and stirring at a rotating speed of 250r/min for 2 hours, then adding other raw materials, uniformly stirring, and standing for 2 hours to obtain first mixed resin;
(2) heating the mixed resin, spraying the heated mixed resin onto fiber products made of multiple materials, and stacking the fiber products made of the multiple materials together to form a wet fiber product;
(3) curing the wet fiber product for the first time to promote the first mixed resin to be cured, and then reducing the temperature to room temperature to obtain a first cured fiber product;
(4) cutting the first solidified fiber product into a specific shape, then sequentially overlapping a plurality of layers of the first solidified fiber products with the specific shape, and pressurizing to promote the first solidified fiber products of each layer to be mutually adhered to form a semi-finished product;
(5) preparing the following raw materials in parts by weight: 80 parts of tetrahydrophthalic acid diglycidyl ester, 30 parts of triethylene glycol dimethacrylate and 40 parts of 1, 8-menthane diamine, heating and melting the tetrahydrophthalic acid diglycidyl ester and the triethylene glycol dimethacrylate in parts by weight, cooling to 40 ℃ for protection, adding the 1, 8-menthane diamine in parts by weight, mixing and stirring at the rotating speed of 250r/min for 2 hours, and standing to obtain a second mixed resin;
(6) and heating the second mixed resin, spraying the heated second mixed resin onto the semi-finished product, heating the semi-finished product to the curing temperature under a pressurized state, and performing secondary curing on the second mixed resin to obtain the final polymer fiber reinforced resin matrix composite.
The fiber product is prepared by the following steps: mixing glass wool and modified aramid fiber, dispersing, dewatering, and oven drying to obtain the final product with a quantitative of 48g/m2The original product of (2); the length of the glass wool is 8mm, and the diameter of the glass wool is 10 mu m; the length of the aramid fiber is 6mm, and the diameter of the aramid fiber is 15 mu m; wherein the glass wool accounts for 45 percent of the total mass of the glass wool and the aramid fiber; diluting a binder, and sequentially adding a flame retardant into the binder to form a glue solution, wherein the mass fraction of the binder is 10%, and the mass fraction of the flame retardant is 8%; and completely immersing the original product into the glue solution for glue dipping to enable the glue solution to fully permeate into fibers, sucking the glue solution on the surface of the dipped original product to obtain a wet product, and drying the wet product to obtain a fiber product.
The ultra-high molecular weight PE resin is prepared by the following steps: heating a reaction vessel to a reaction temperature, vacuumizing, replacing with nitrogen, adding gasoline, an additive and a catalyst, wherein the mass ratio of the ethylene to the gasoline to the additive is 10:15:2, uniformly stirring, introducing nitrogen, finally continuously adding the ethylene into the reaction vessel, controlling the pressure to be 1.2MPa, reacting for 3 hours at the reaction temperature, after the reaction is finished, rapidly cooling to 30 ℃, filtering out the gasoline to obtain a liquid, and drying the liquid to obtain the ultra-high molecular weight PE resin, wherein the reaction temperature is 70 ℃.
The additive comprises a mixture of microcrystalline kaolinite, mineral oil and fluorite powder, the weight ratio of the microcrystalline kaolinite to the mineral oil to the fluorite powder is 3:4:1, and the stirring speed is 700 r/min.
The viscosity average molecular weight of the ultra-high molecular weight PE resin is 600 ten thousand, the average particle size is 200 mu m, and the particle size distribution width (d90-d10)/d 50: 1.5, bulk density 0.5g/cm3。
The modified aramid fiber is prepared by the following steps: immersing 1 part by weight of aramid fiber in 150 parts by weight of caustic alkali and 850 parts by weight of ultrapure water, and reacting at 60 ℃ for 6 hours; after the reaction is finished, taking out the fiber, cleaning and drying; preparing a catecholamine solution by adopting a buffer reagent, water and catecholamine hydrochloride; soaking the dried aramid fiber in a catechol ethylamine solution, and oscillating for 12h at the temperature of 30 ℃; after the reaction is finished, taking out the fiber, and cleaning and drying the fiber to obtain the aromatic amide fiber coated by the catecholamine; dispersing graphite acid in the acetin by mass under the stirring condition, and performing ultrasonic treatment to obtain a dispersion liquid; adding 1 part of theanine-coated aramid fiber into the dispersion liquid, and reacting for 5 hours at the temperature of 60 ℃; and after the reaction is finished, taking out the fiber, and cleaning and drying to obtain the modified aramid fiber.
The concentration of the catecholamine solution is 3g/L, the mass ratio of the dried aramid fiber to the catecholamine is 5:1, and the mass ratio of the graphite acid to the acetin is 0.5: 100.
in addition, to further improve the effect, the fluorocarbon resin is prepared by the following steps:
1) fully mixing vinyl acetate, 4-methyl-2-pentanone and xylene in a reaction kettle;
2) sequentially adding 2,2' -diazoisobutyronitrile, undecylenic acid and allyl hydroxyethyl ether into a reaction kettle;
3) vacuumizing the closed reaction kettle: vacuumizing a closed reaction kettle to-0.08 MPa, keeping the vacuum degree for 20min, filling nitrogen to enable the interior of the reaction kettle to reach 0.8MPa, vacuumizing again, and closing a vacuum pump; pumping 80% perfluoroethylene gas-phase monomer by a pump;
4) pumping the residual perfluoroethylene gas-phase monomer into a reaction kettle by using a pump, stirring, maintaining the reaction pressure at 0.8MPa, the stirring speed at 80 rpm, stirring for 4 hours, slowly heating the reaction kettle by using a jacket in the reaction process, and keeping the temperature in the reaction kettle at 70 ℃ for 12 hours;
5) after the perfluoroethylene gas-phase monomer is added, stopping the reaction when the reaction pressure in the kettle is reduced to 1.0MPa, recovering the perfluoroethylene gas-phase monomer, and returning to the device after the solvent is removed;
6) and (3) after the perfluoroethylene gas-phase monomer is recovered, replacing the gas in the kettle with nitrogen, cooling to below 30 ℃, reducing the pressure to 0MPa, turning off the stirrer, and discharging to obtain the fluorocarbon resin.
Testing
The polymer fiber reinforced resin matrix composite material in the above examples was measured to have a flexural strength of 120.98 + -15.76 MPa, a flexural modulus of 1.95 + -0.2 GPa and a fracture toughness of 9.05 + -0.53 kJ/m2. The fibers form a good interface with the resin, and thus both strength and toughness are significantly improved.
Comparative example: Bis-GMA/triethylene glycol dimethacrylate (weight portion ratio is 60: 55) photocuring resin system is used as a resin matrix, and camphorquinone (1% by weight) is used as an initiator. A homopolymer of 2-acrylonitrile was selected to make homopolymer nanofibers of 2-acrylonitrile. The homopolymer of 2-acrylonitrile was dissolved in a solution of formyldimethylamine in an amount of 15% by mass. The nanofibers were received on a metal receiving plate 25cm long and 18cm wide at a voltage of 16KV, a flow rate of 0.3ml/h, and a receiving distance of 16 cm. Controlling the receiving time to make the surface density of the received nanofiber membrane be 0.005-0.006 g/cm2. The diameter of the prepared nanofiber is 150-200 nm. Preparation of the dimensions of the test specimens 2X 25mm are prepared for the flexural strength, flexural modulus and fracture toughness according to ISO 10477. The bending strength of the composite material is 95.11 +/-5.33 MPa, the bending modulus is 1.40 +/-0.16 GPa and the fracture toughness is 5.1 +/-0.38 kJ/m2。
According to the embodiment, the continuous compounding of different types of resins and fiber products made of various materials is realized, the forming efficiency is greatly improved, manual working procedures are reduced, the consistency of the products is effectively improved, and the requirement of mass production is met.
The invention gives full play to the excellent performance of the glass wool and the modified aramid fiber, can fully utilize the characteristics of the raw materials, has simple preparation process and excellent performance of the prepared composite material.
The ultra-high molecular weight PE resin has controllable molecular weight and narrow molecular weight distribution, and has excellent performances of wear resistance, creep resistance, static resistance and the like superior to those of common resin; the preparation method of the invention has simple production process and is suitable for large-scale production.
The modified fiber used in the invention has outstanding ultraviolet resistance, obviously improves the surface activity of the aramid fiber, improves the interface acting force between the fiber and the resin, and provides a material guarantee for further modification and application of the fiber.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (7)
1. A preparation method of a polymer fiber reinforced resin matrix composite material is characterized by comprising the following steps:
(1) preparing the following raw materials in parts by weight: 35-40 parts of ultra-high molecular weight PE resin, 5-8 parts of F-type epoxy resin, 15-20 parts of fluorocarbon resin, 2-2.5 parts of 1, 6-dihydroxyhexane, 0.2-0.3 part of nano titanium dioxide, 0.8-1 part of nano white carbon black and 6-8 parts of curing agent; heating and melting the ultra-high molecular weight PE resin in parts by weight at 70-80 ℃, cooling to 35-40 ℃ for protection, adding the F-type epoxy resin and the fluorocarbon resin in parts by weight, mixing and stirring at a rotating speed of 200-250 r/min for 1-2 hours, then adding other raw materials, uniformly stirring, and standing for 1-2 hours to obtain a first mixed resin;
(2) heating the mixed resin, spraying the heated mixed resin onto fiber products made of multiple materials, and stacking the fiber products made of the multiple materials together to form a wet fiber product;
(3) curing the wet fiber product for the first time to promote the first mixed resin to be cured, and then reducing the temperature to room temperature to obtain a first cured fiber product;
(4) cutting the first solidified fiber product into a specific shape, then sequentially overlapping a plurality of layers of the first solidified fiber products with the specific shape, and pressurizing to promote the first solidified fiber products of each layer to be mutually adhered to form a semi-finished product;
(5) preparing the following raw materials in parts by weight: 70-80 parts of tetrahydrophthalic acid diglycidyl ester, 20-30 parts of triethylene glycol dimethacrylate and 30-40 parts of 1, 8-menthane diamine, heating and melting the tetrahydrophthalic acid diglycidyl ester and the triethylene glycol dimethacrylate in parts by weight, cooling to 35-40 ℃ for protection, adding the 1, 8-menthane diamine in parts by weight, mixing and stirring at the rotating speed of 200-250 r/min for 1-2 hours, and standing to obtain a second mixed resin;
(6) and heating the second mixed resin, spraying the heated second mixed resin onto the semi-finished product, heating the semi-finished product to the curing temperature under a pressurized state, and performing secondary curing on the second mixed resin to obtain the final polymer fiber reinforced resin matrix composite.
2. The method for preparing the polymer fiber reinforced resin matrix composite according to claim 1, wherein the fiber product is prepared by the following steps: uniformly mixing glass wool and modified aramid fiber, dispersing, dehydrating and drying to obtain the aramid fiber with the quantitative content of 45-48 g/m2The original product of (2); the length of the glass wool is 7-8 mm, and the diameter of the glass wool is 8-10 mu m; the length of the aramid fiber is 5-6 mm, and the diameter of the aramid fiber is 12-15 mu m; wherein the glass wool accounts for 40-45% of the total mass of the glass wool and the aramid fiber; diluting a binder, and sequentially adding a flame retardant into the binder to form a glue solution, wherein the mass fraction of the binder is 8-10%, and the mass fraction of the flame retardant is 7-8%; completely immersing the original product in the glue solution for glue dipping to enable the glue solution to fully penetrate between fibers, sucking the glue solution on the surface of the original product after glue dipping to obtain a wet product, and drying the wet product to obtain the wet productA fiber product.
3. The method for preparing a polymer fiber reinforced resin matrix composite material according to claim 1 or 2, wherein the ultra-high molecular weight PE resin is prepared by the following steps: heating a reaction container to a reaction temperature, vacuumizing, replacing with nitrogen, adding ethylene, gasoline and an additive, wherein the mass ratio of the ethylene to the gasoline to the additive is 10: 12-15: 1-2, uniformly stirring, introducing nitrogen, continuously adding the ethylene into the reaction container, controlling the pressure to be 1-1.2 MPa, reacting for 2.5-3 hours at the reaction temperature, rapidly cooling to 25-30 ℃ after the reaction is finished, filtering out the gasoline to obtain a liquid, and drying the liquid to obtain the ultra-high molecular weight PE resin, wherein the reaction temperature is 60-70 ℃.
4. The preparation method of the polymer fiber reinforced resin matrix composite material according to claim 1, wherein the additive comprises a mixture of microcrystalline kaolinite, mineral oil and fluorite powder, the weight ratio of the microcrystalline kaolinite, the mineral oil and the fluorite powder is 2-3: 2-4: 1, and the stirring speed is 500-700 r/min.
5. The method for preparing the polymer fiber reinforced resin matrix composite material according to claim 1, wherein the viscosity average molecular weight of the ultra-high molecular weight PE resin is 500 to 600 ten thousand, the average particle size is 150 to 200 μm, and the particle size distribution width (d90-d10)/d 50: 1 to 1.5, and a bulk density of 0.3 to 0.5g/cm3。
6. The method for preparing the polymer fiber reinforced resin matrix composite material according to claim 5, wherein the modified aramid fiber is prepared by the following steps: immersing 1 part of aramid fiber into 120-150 parts of caustic alkali and 820-850 parts of ultrapure water by weight, and reacting for 5-6 h at the temperature of 50-60 ℃; after the reaction is finished, taking out the fiber, cleaning and drying; preparing a catecholamine solution by adopting a buffer reagent, water and catecholamine hydrochloride; soaking the dried aramid fiber in a catechol ethylamine solution, and oscillating for 10-12 h at the temperature of 20-30 ℃; after the reaction is finished, taking out the fiber, and cleaning and drying the fiber to obtain the aromatic amide fiber coated by the catecholamine; dispersing graphite acid in the acetin by mass under the stirring condition, and performing ultrasonic treatment to obtain a dispersion liquid; adding 1 part of theafenoxamine-coated aramid fiber into the dispersion liquid, and reacting for 4-5 hours at the temperature of 55-60 ℃; and after the reaction is finished, taking out the fiber, and cleaning and drying to obtain the modified aramid fiber.
7. The method for preparing the polymer fiber reinforced resin matrix composite material according to claim 6, wherein the concentration of the catecholamine solution is 2-3 g/L, the mass ratio of the dried aramid fiber to the catecholamine is 3-5: 1, and the mass ratio of the graphite acid to the acetidone is 0.3-0.5: 100.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977552A (en) * | 2012-10-18 | 2013-03-20 | 国网智能电网研究院 | Fiber-enhanced resin matrix composite material and preparation method thereof |
| CN106965463A (en) * | 2017-05-05 | 2017-07-21 | 机械科学研究总院先进制造技术研究中心 | A kind of continuous fiber reinforced composites processing method |
-
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977552A (en) * | 2012-10-18 | 2013-03-20 | 国网智能电网研究院 | Fiber-enhanced resin matrix composite material and preparation method thereof |
| CN106965463A (en) * | 2017-05-05 | 2017-07-21 | 机械科学研究总院先进制造技术研究中心 | A kind of continuous fiber reinforced composites processing method |
Non-Patent Citations (1)
| Title |
|---|
| 史汉桥等: "低温用碳/环氧复合材料性能", 《宇航材料工艺》 * |
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