CN108727770A - Flame-retardant high-strength lightweight phenolic resin and preparation method thereof - Google Patents
Flame-retardant high-strength lightweight phenolic resin and preparation method thereof Download PDFInfo
- Publication number
- CN108727770A CN108727770A CN201810335174.1A CN201810335174A CN108727770A CN 108727770 A CN108727770 A CN 108727770A CN 201810335174 A CN201810335174 A CN 201810335174A CN 108727770 A CN108727770 A CN 108727770A
- Authority
- CN
- China
- Prior art keywords
- phenolic resin
- flame
- retardant high
- strength lightweight
- 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.)
- Withdrawn
Links
- 239000005011 phenolic resin Substances 0.000 title claims abstract description 159
- 229920001568 phenolic resin Polymers 0.000 title claims abstract description 159
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 title claims abstract description 158
- 239000003063 flame retardant Substances 0.000 title claims abstract description 75
- 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 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000000835 fiber Substances 0.000 claims abstract description 75
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000002994 raw material Substances 0.000 claims abstract description 33
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000004088 foaming agent Substances 0.000 claims abstract description 23
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 22
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000004094 surface-active agent Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- -1 polyethylene Polymers 0.000 claims description 37
- 150000001299 aldehydes Chemical class 0.000 claims description 17
- 239000013078 crystal Substances 0.000 claims description 10
- 239000004698 Polyethylene Substances 0.000 claims description 9
- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 claims description 9
- 229920000573 polyethylene Polymers 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 8
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 8
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical group O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 5
- YMWUJEATGCHHMB-UHFFFAOYSA-N dichloromethane Natural products ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- IWDCLRJOBJJRNH-UHFFFAOYSA-N p-cresol Chemical compound CC1=CC=C(O)C=C1 IWDCLRJOBJJRNH-UHFFFAOYSA-N 0.000 claims description 5
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 claims description 4
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 4
- STNJBCKSHOAVAJ-UHFFFAOYSA-N Methacrolein Chemical compound CC(=C)C=O STNJBCKSHOAVAJ-UHFFFAOYSA-N 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 4
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 claims description 4
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 4
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical group [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 4
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 4
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 4
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 4
- 229920002866 paraformaldehyde Polymers 0.000 claims description 4
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 4
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- XPIJMQVLTXAGME-UHFFFAOYSA-N 1,1-dimethoxycyclohexane Chemical compound COC1(OC)CCCCC1 XPIJMQVLTXAGME-UHFFFAOYSA-N 0.000 claims description 2
- BGJSXRVXTHVRSN-UHFFFAOYSA-N 1,3,5-trioxane Chemical compound C1OCOCO1 BGJSXRVXTHVRSN-UHFFFAOYSA-N 0.000 claims description 2
- 229910017083 AlN Inorganic materials 0.000 claims description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 claims description 2
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 2
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 2
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 238000003763 carbonization Methods 0.000 claims description 2
- 229940113088 dimethylacetamide Drugs 0.000 claims description 2
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims description 2
- 239000003365 glass fiber Substances 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims description 2
- CQRYARSYNCAZFO-UHFFFAOYSA-N salicyl alcohol Chemical compound OCC1=CC=CC=C1O CQRYARSYNCAZFO-UHFFFAOYSA-N 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 2
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 claims description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims 1
- 235000011054 acetic acid Nutrition 0.000 claims 1
- 235000019439 ethyl acetate Nutrition 0.000 claims 1
- 235000019253 formic acid Nutrition 0.000 claims 1
- 238000001802 infusion Methods 0.000 claims 1
- 239000011787 zinc oxide Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 24
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 abstract 2
- 239000011162 core material Substances 0.000 description 24
- 239000011248 coating agent Substances 0.000 description 21
- 238000000576 coating method Methods 0.000 description 21
- 238000004080 punching Methods 0.000 description 12
- 238000005507 spraying Methods 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 9
- 238000011056 performance test Methods 0.000 description 8
- 239000002585 base Substances 0.000 description 7
- 239000000839 emulsion Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 229910021389 graphene Inorganic materials 0.000 description 7
- 125000000524 functional group Chemical group 0.000 description 6
- 238000000197 pyrolysis Methods 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Substances C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 5
- 210000000481 breast Anatomy 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000003822 epoxy resin Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 229920000647 polyepoxide Polymers 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000012783 reinforcing fiber Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 238000005452 bending Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 150000004985 diamines Chemical class 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical class [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 235000019399 azodicarbonamide Nutrition 0.000 description 3
- 230000003139 buffering effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 229910003978 SiClx Inorganic materials 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 239000010426 asphalt Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000005255 carburizing Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical group CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 2
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- QWVGKYWNOKOFNN-UHFFFAOYSA-N o-cresol Chemical compound CC1=CC=CC=C1O QWVGKYWNOKOFNN-UHFFFAOYSA-N 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 229940045998 sodium isethionate Drugs 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- 150000005208 1,4-dihydroxybenzenes Chemical class 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 239000004156 Azodicarbonamide Substances 0.000 description 1
- RZYKUPXRYIOEME-UHFFFAOYSA-N CCCCCCCCCCCC[S] Chemical compound CCCCCCCCCCCC[S] RZYKUPXRYIOEME-UHFFFAOYSA-N 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 235000019082 Osmanthus Nutrition 0.000 description 1
- 241000333181 Osmanthus Species 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 125000005227 alkyl sulfonate group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- BTBJBAZGXNKLQC-UHFFFAOYSA-N ammonium lauryl sulfate Chemical compound [NH4+].CCCCCCCCCCCCOS([O-])(=O)=O BTBJBAZGXNKLQC-UHFFFAOYSA-N 0.000 description 1
- XOZUGNYVDXMRKW-AATRIKPKSA-N azodicarbonamide Chemical compound NC(=O)\N=N\C(N)=O XOZUGNYVDXMRKW-AATRIKPKSA-N 0.000 description 1
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical class NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
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- 238000013036 cure process Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
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- 238000001125 extrusion Methods 0.000 description 1
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- 239000007789 gas Substances 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- IIYFAKIEWZDVMP-UHFFFAOYSA-N linear paraffin C13 Natural products CCCCCCCCCCCCC IIYFAKIEWZDVMP-UHFFFAOYSA-N 0.000 description 1
- 150000002672 m-cresols Chemical class 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical class [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 235000012254 magnesium hydroxide Nutrition 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- SXJVFQLYZSNZBT-UHFFFAOYSA-N nonane-1,9-diamine Chemical compound NCCCCCCCCCN SXJVFQLYZSNZBT-UHFFFAOYSA-N 0.000 description 1
- 150000002883 o-cresols Chemical class 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 125000003170 phenylsulfonyl group Chemical group C1(=CC=CC=C1)S(=O)(=O)* 0.000 description 1
- 229920001921 poly-methyl-phenyl-siloxane Polymers 0.000 description 1
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
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- 238000003466 welding Methods 0.000 description 1
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- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
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- C—CHEMISTRY; METALLURGY
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Abstract
The present invention relates to phenolic resins fields, and in particular to flame-retardant high-strength lightweight phenolic resin and preparation method thereof, the preparation method of the flame-retardant high-strength lightweight phenolic resin include the following steps：(1) in organic solvent after mixing by raw material phenol, first part's raw material aldehyde, catalyst, long fibre, improved silica, foaming agent and surfactant that length is 5~20 microns, flow back 3~5h at 80~120 DEG C, obtains prepolymer；(2) staple fiber and the second part raw material aldehyde that length is 0.3~2 micron are added into prepolymer, then flow back at 90~110 DEG C 1~2h, forms gel；(3) Gel heat-treatment：Gel is placed into 1~3h in the steam that pressure is 150~500kPa, temperature is 130~200 DEG C, then cools to room temperature, obtains flame-retardant high-strength lightweight phenolic resin.The flame-retardant high-strength lightweight phenolic resin being prepared by this method has the characteristics that fire-retardant, intensity is high.
Description
Technical field
The present invention relates to phenolic resins fields, and in particular to flame-retardant high-strength lightweight phenolic resin and its preparation side
Method.
Background technology
In recent years, automotive light weight technology has become the emphasis direction of automotive field development instantly, and Lightweight Technology can not only
It the problem of enough its environmental pollutions of effective solution, realizes the target of energy-saving and emission-reduction, also largely reduces automobile making
Cost has prodigious economic benefit for present used automobile.
Currently, the method for automotive light weight technology includes mainly the section using light material and reduction door-plate.Reduce door-plate
Section namely reduces the thickness of door-plate, although the overall weight of automobile can be reduced, it can also cause automobile door plate is strong
Degree reduces, and in collision, will produce serious deformation, reduces the safety of automobile.Using light material refer to using light weight,
The steel material of the current car door of the big material substitution of intensity, currently, common light material has aluminium alloy extrusions, high-strength complex
Resin and carbon fibre material.Wherein, high-intensity resin relies on itself small proportion, sound-insulating and heat-insulating, corrosion-resistant, absorption impact energy
Amount, many advantages, such as specific strength is high, at low cost, easy processing, good decorating effect, already as light material in automotive light weight technology
Development trend.
Phenolic resin starting material is easy to get, cheap, and production technology and equipment are simple, and product has excellent machinery
Property, heat resistance, cold resistance, electrical insulating property, dimensional stability, molding processibility, anti-flammability and smokiness, there is extensive use
On the way, still, conventional unmodified phenolic resin brittleness is big, poor toughness, largely limits the exploitation of high performance material.
Invention content
Of the existing technology in order to overcome the problems, such as, an object of the present invention is to provide a kind of flame-retardant high-strength lightweight phenol
The preparation method of urea formaldehyde, the flame-retardant high-strength lightweight phenolic resin being prepared by this method is with fire-retardant, intensity is high
Feature.
The second object of the present invention is to provide a kind of flame-retardant high-strength lightweight phenolic resin.
To achieve the goals above, the present invention provides a kind of preparation method of flame-retardant high-strength lightweight phenolic resin, including
Following steps：
(1) by raw material phenol, first part's raw material aldehyde, catalyst, the long fibre that length is 5~20 microns, modified titanium dioxide
In organic solvent after mixing, flow back 3~5h at 80~120 DEG C, obtains pre-polymerization for silicon, foaming agent and surfactant
Object；
(2) staple fiber and the second part raw material aldehyde that length is 0.3~2 micron, ultrasonic disperse 30 are added into prepolymer
~60min, then flow back at 90~110 DEG C 1~2h, forms gel；
(3) Gel heat-treatment：Gel is placed 1 in the steam that pressure is 150~500kPa, temperature is 130~200 DEG C
~3h, then cools to room temperature, and obtains flame-retardant high-strength lightweight phenolic resin.
The present invention also provides a kind of flame-retardant high-strength lightweight phenolic resin being prepared according to the above method.
Through the above technical solutions, the present invention has the following technical effects：
(1) by the way that staple fiber and long fibre is compound, staple fiber can be made to be inserted into the hole of long fibre and phenolic resin
The phenomenon that in gap, improving long stapled dispersion degree, avoiding the occurrence of long fibre aggregation winding improves the uniformity of phenolic resin and steady
It is qualitative.
(2) it is used in mixed way by phenolic resin and foaming agent, can play the role of buffering external force, improved automobile and travelling
Stability in the process.Phenolic resin containing foaming agent is subjected to pyrolysis in the steam of solvent, on the one hand can
So that foaming agent is decomposed at high temperature, generate stomata, on the other hand, additionally it is possible to avoid phenolic resin that solvent volatilization occurs at high temperature
And the phenomenon that causing the internal structure of phenolic resin to cure.Phenolic resin is subjected to pyrolysis under high pressure, makes phenolic aldehyde tree
Fat is reduced the decomposition rate of foaming agent by stronger external pressure, reduces the generating rate of bubble, improves the uniform of pore opening
Property, make foamed phenolic resin that there is uniform internal structure.
Specific implementation mode
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
In order to reduce the quality of phenolic resin, the intensity of phenolic resin is improved, it is light that the present invention provides a kind of flame-retardant high-strength
Matter phenolic resin, the flame-retardant high-strength lightweight are made of raw material, and on the basis of 100 parts by weight of raw material phenol, the raw material includes
The substance of following parts by weight：100 parts by weight of raw material phenol, 30~120 parts by weight of raw material aldehyde, 10~48 parts by weight of staple fiber, long fibre
Tie up 10~30 parts by weight, 12~40 parts by weight of improved silica, 6~20 parts by weight of foaming agent, 2~10 weight of surfactant
Part, 10~30 parts by weight of catalyst, 200~360 parts by weight of organic solvent.
The length of the staple fiber is 0.3~2 micron；The long stapled length is 5~20 microns.
In the present invention, by the way that the different reinforcing fiber of two kinds of length is added in phenolic resin, it can be handed between long fibre
Fork is wrapped in the inside of phenolic resin, plays the role of improving phenolic resin bending property, staple fiber can be dispersed in asphalt mixtures modified by epoxy resin
Inside fat, play the role of improving epoxy resin intensity；In addition, staple fiber can also be dispersed in inside long fibre, long fibre is avoided
Undue agglomeration is tieed up, can not disperse, to make phenolic resin chemistry inside be unevenly distributed, improve the uniform of phenolic resin
Property.
In the present invention, a large amount of functional group is contained by the surface of improved silica, it can be with phenolic resin strand
On functional group react, make between improved silica and phenolic resin the formation connection with chemical bond, to make dioxy
There is very high binding force between SiClx and phenolic resin, and can be uniformly dispersed in phenolic resin, it can not only be notable
The intensity of phenolic resin system is improved, while also improving the uniformity of phenolic resin.
It in the present invention, is used in mixed way by phenolic resin and foaming agent, phenolic resin foam, phenolic resin bubble can be generated
Foam can not only reduce the quality of system, additionally it is possible to play the role of buffering external force, sound insulation, improve automobile in the process of moving
Stability and soundproof effect.
In the present invention, the content of each substance is an important factor for influencing phenolic resin performance, under preferable case, with raw material phenol
On the basis of 100 parts by weight, the feedstock composition includes the substance of following parts by weight：100 parts by weight of raw material phenol, raw material aldehyde 30~
120 parts by weight, 24~36 parts by weight of staple fiber, 16~24 parts by weight of long fibre, 20~36 parts by weight of improved silica, foaming
6~20 parts by weight of agent, 2~10 parts by weight of surfactant, 10~30 parts by weight of catalyst, 240~300 weight of organic solvent
Part.
According to the present invention, the raw material phenol can be o-cresol, m-cresol, p-cresol, to hydroxymethylphenol, neighbour
At least one of benzenediol, resorcinol and hydroquinone；Raw material aldehyde can be formaldehyde, acetaldehyde, propionic aldehyde, butyraldehyde, methacrylaldehyde,
At least one of cyclohexanone dimethylacetal, benzaldehyde, furfural, heterocyclic aldehydes, paraformaldehyde and metaformaldehyde.
In the present invention, the content of long fibre and staple fiber is an important factor for influencing phenolic resin mechanical property, if long
The content of fiber is low, then can reduce the tensile strength of phenolic resin, and the content of staple fiber is low can also reduce the strong of phenolic resin
Degree, in order to obtain the phenolic resin of high intensity, under preferable case, the staple fiber and the long stapled mass ratio be (1~
1.6)：1.
In the present invention, catalyst can promote the generation of phenolic resin, improve polymerisation efficiency, under preferable case, institute
It is alkaline matter to state catalyst, it is further preferred that the catalyst is selected from alkali metal hydroxide, alkaline-earth metal hydroxide
At least one of object, carbonate and bicarbonate.
According to the present invention, reinforcing fiber is an important factor for playing enhancing phenolic resin mechanical property in the present invention, wherein
Staple fiber is to improve the important materials of phenolic resin intensity, and under preferable case, the reinforcing fiber should have higher intensity,
In the case of further preferably, the staple fiber is selected from calcium sulfate crystal whiskers, alumina whisker, silicon carbide whisker, carbonization boron whisker, two
Zirconium oxide whisker, aluminium nitride whisker, ZnOw, magnesium sulfate crystal whisker, glass fibre, potassium titanate crystal whisker, magnesium sulfate crystal whisker and
At least one of silicon nitride crystal whisker；And the staple fiber of the present invention has good thermal conductivity, avoids accumulation of heat, improves simultaneously
The intensity and flame retardant property of phenolic resin, under preferable case, the average diameter of the reinforcing fiber is 50~150nm.
The bending property and tensile strength of phenolic resin are improved in the present invention by long fibre, the long fibre should have
Higher intensity and high tenacity, under preferable case, the long fibre is polyethylene fibre, the Weight-average molecular of the polyethylene fibre
Measure Mw >=1 × 106。
In the present invention, foaming agent can occur to thermally decompose and form bubble inside phenolic resin at high temperature, to shape
At foamed phenolic resin, since carburizing reagent can occur at high temperature for phenolic resin, the foaming agent selected by the present invention
Decomposition temperature should be less than the carburizing temperature of phenolic resin.Under preferable case, the foaming agent is selected from the double benzene sulfonyls of 4,4- oxos
Hydrazine, azodicarbonamide, N, at least one of N '-dinitrosopentamethlyene tetramines.
In the present invention, a large amount of active function groups are contained on the surface of the improved silica, can be with phenolic resin table
The functional group in face is chemically reacted, and makes the formation connection with chemical bond between improved silica and phenolic resin, to make
There is very high binding force between improved silica and phenolic resin, and can be uniformly dispersed in phenolic resin, not only
The intensity of phenolic resin system can be significantly improved, while also improving the uniformity of phenolic resin.It is described to change under preferable case
Property silica be selected from least one of hydroxyl modification silica and amino modified silica；Further preferred situation
Under, the average diameter of the improved silica is 100~300nm.
Under preferable case, the surfactant is selected from dodecyl alcohol polyoxyethylene ether sodium sulfate, dodecyl sulphate
Ammonium, lauryl sodium sulfate, dodecyl benzene sulfonic acid, sodium secondary alkyl sulfonate, fatty alcohol sodium isethionate, N- lauroyl musculamines
At least one of sour sodium, coconut acyl methyl taurine sodium, α-sodium olefin sulfonate, dodecyl phosphide ester triethanolamine.
The present invention does not have the type of organic solvent special requirement, can be common organic molten in phenolic resin synthesis
Agent, under preferable case, the organic solvent is selected from acetone, n,N-Dimethylformamide, N-Methyl pyrrolidone, N, N- dimethyl
Acetamide, dimethylacetylamide, dichloromethane, triethyl phosphate, chloroform, toluene, ethyl alcohol, acetic acid, ethyl acetate, first
At least one of acid, chloroform, tetrahydrofuran, atoleine and dimethyl sulfoxide (DMSO).
The present invention also provides a kind of preparation methods of flame-retardant high-strength lightweight phenolic resin, include the following steps：
(1) by raw material phenol, first part's raw material aldehyde, catalyst, the long fibre that length is 5~20 microns, modified titanium dioxide
In organic solvent after mixing, flow back 3~5h at 80~120 DEG C, obtains pre-polymerization for silicon, foaming agent and surfactant
Object；
(2) staple fiber and the second part raw material aldehyde that length is 0.3~2 micron, ultrasonic disperse 30 are added into prepolymer
~60min, then flow back at 90~110 DEG C 1~2h, forms gel；
(3) Gel heat-treatment：Gel is placed 1 in the steam that pressure is 150~500kPa, temperature is 130~200 DEG C
~3h, then cools to room temperature, and obtains flame-retardant high-strength lightweight phenolic resin.
In the present invention, phenolic resin monomer, catalyst, long fibre, improved silica and surfactant are existed first
Prepolymerization reaction is carried out in organic solvent, foaming agent is coated on inside phenolic resin performed polymer, and long fibre is made uniformly to disperse
Inside phenolic resin, there is higher binding force between phenolic resin.Then adding staple fiber, the reaction was continued, can make
Staple fiber enters in phenolic resin that the reaction was continued, and staple fiber is inserted into the hole of long fibre and phenolic resin, improves length
The dispersion degree of fiber avoids the occurrence of long fibre and assembles the phenomenon for winding and causing phenolic resin internal structure otherness big.
Improved silica can be chemically reacted with the functional group of phenolic surface, and in the form of chemical bond with
Phenolic resin combines, and not only increases the binding force of silica and phenolic resin, while improving silica in phenolic aldehyde tree
Dispersing uniformity in fat significantly improves the intensity of phenolic resin.The present invention finally to phenolic resin carry out high-temperature process, one
Aspect can make the progress of curing reaction, on the other hand, foaming agent be made to decompose at high temperature, be formed inside phenolic resin more
Pore structure.
Phenolic resin containing foaming agent is carried out pyrolysis by the present invention in the steam of solvent, on the one hand can be made
Foaming agent decomposes at high temperature, generates stomata, on the other hand, additionally it is possible to due to avoid phenolic resin from occurring to occur admittedly because of solvent
Change reaction, avoids occurring the big phenomenon of material internal structure differentiation in integrated molding.Phenolic resin is carried out under high pressure
Pyrolysis makes phenolic resin by stronger external pressure, slows down the effusion of gas in phenolic resin, reduces the decomposition of foaming agent
Speed reduces the generating rate of bubble, improves the uniformity of pore opening, and foamed phenolic resin is made to have uniform internal junction
Structure.
According to the present invention, the weight ratio of first part's raw material aldehyde and second part raw material aldehyde is (3~6)：1.
The density for the flame-retardant high-strength lightweight phenolic resin being prepared according to the above method is 36.25~39.14kg/
m3。
The present invention also provides a kind of lightweight automotive cover board, including inner core and the coating coated in core surface, the core materials
Using flame-retardant high-strength lightweight phenolic resin according to the present invention.
It is the coating packet in terms of 100 by the weight of epoxy resin under the preferable case of the present invention in embodiment
Include the substance of following parts by weight：100 parts of phenolic resin, 30~58 parts of butyl methacrylate, redox graphene 5~15
Part, 2~6 parts of levelling agent, 10~18 parts of curing agent.
Preferably, the levelling agent is selected from dimethyl silicone polymer and/or polymethylphenylsiloxane；The curing agent can
With using ethylenediamine, hexamethylene diamine, methyl cyclohexyl diamine, 1,4- butanediamine, 1,5- pentanediamines, 2- methyl-1s, 5- pentanediamines, 2- fourths
Base -2- ethyl -1,5- pentanediamines, 1,6- hexamethylene diamines, 2,2,4- trimethylhexane diamines, 2,4,4- trimethylhexane diamines, 1,8- are pungent
Diamines, 2- methyl-1s, 8- octamethylenediamines, 1,9-nonamethylene diamine, 1,10- decamethylene diamines, 1,11- hendecanes diamines, 1,12- dodecanes two
Amine, 1,13- tridecane diamines, 1,14- tetradecanes diamines, 1,15- pentadecanes diamines, 2- methyl -2,4-PD, 1,16- ten
At least one of six alkane diamines and 1,18-1,14- octadecamethylene diamines, dimethythiotoluene diamine.
The present invention also provides a kind of preparation methods of lightweight automotive cover board, include the following steps：
(1) prepared by core material：The core material is by flame-retardant high-strength lightweight phenolic resin punch forming according to the present invention
It is made, preparation method is referring to the present invention previously with regard to the description of the preparation method of flame-retardant high-strength lightweight phenolic resin.
(2) coating spraying：By modified epoxy, butyl methacrylate, redox graphene, levelling agent, wetting
Agent, curing agent are uniformly mixed in organic solvent, form coating emulsion, coating emulsion is then sprayed on core surfaces, are cured
Afterwards, coating is formed.
Under preferable case, the stamping forming technique is：Press temperature is 60-140 DEG C, pressure 5-25MPa, punching press
Time is 2-20min, and after punching press, the temperature of diel and product is reduced to room temperature within 10min.
In the case of, according to the invention it is preferred to, the cure process is to cure 30min at 120 DEG C.
In the present invention, the core material using flame-retardant high-strength light-weight foam phenolic resin as automobile door plate, foamable phenolic tree
Fat core material has the characteristics that light weight compared with existing steel core material, and the quality of automobile can be greatly lowered, in addition, this
Invention prepares automobile cover plate by integrally formed method, avoids, using the method connecting components of welding, further reduced
The quality of automobile cover plate reduces the oil consumption of automobile, plays energy-saving and emission-reduction to reduce the resistance that automobile generates during form
Work.
In the present invention, by the way that the different reinforcing fiber of two kinds of length is added in phenolic resin, it can be handed between long fibre
Fork is wrapped in the inside of phenolic resin, plays the role of improving phenolic resin bending property, staple fiber can be dispersed in asphalt mixtures modified by epoxy resin
Inside fat, play the role of improving epoxy resin intensity, by the way that long fibre and staple fiber to be used cooperatively, staple fiber point can be made
It is dispersed in inside long fibre, avoids long fibre undue agglomeration, can not disperse, to make phenolic resin chemistry inside be unevenly distributed
It is even, and influence the performance of phenolic resin.
In the present invention, a large amount of functional group is contained by the surface of improved silica, it can be with phenolic resin strand
On functional group react, make between improved silica and phenolic resin the formation connection with chemical bond, to make dioxy
There is very high binding force between SiClx and phenolic resin, and can be uniformly dispersed in phenolic resin, it can not only be notable
The intensity of phenolic resin system is improved, while also improving the uniformity of phenolic resin.
It in the present invention, is used in mixed way by phenolic resin and foaming agent, can play the role of buffering external force, improve automobile
Stability in the process of moving.Phenolic resin containing foaming agent is subjected to pyrolysis, a side in the steam of solvent
Face can be such that foaming agent decomposes at high temperature, generate stomata, on the other hand, additionally it is possible to avoid phenolic resin from occurring at high temperature molten
The phenomenon that agent volatilizees and the internal structure of phenolic resin is caused to cure.Phenolic resin is subjected to pyrolysis under high pressure, is made
Phenolic resin is reduced the decomposition rate of foaming agent by stronger external pressure, reduces the generating rate of bubble, improves pore opening
Uniformity makes foamed phenolic resin have uniform internal structure.
The present invention will be described in detail by way of examples below.In following embodiment, various kinds is tested using drainage
The density of product.The tensile property of each sample is tested according to the method for GB/T1447-2005.According to the method for GB/T1449-2005
Survey the examination bending property of each sample.The elongation at break of each sample is tested according to the method for GB/T1040.1-2006.According to GB/
The impact flexibility of the method test each sample of T1451-2005.According to UL94《Equipment and the examination of the flammable performance of device component material
It tests》In testing vertical flammability method, determine the flame retardant rating of composite material.Batten size：Long 125 ± 5mm, wide by 13.0 ±
0.5mm, 1.5 ± 0.2mm of thickness.
Embodiment 1
(1) prepared by flame-retardant high-strength lightweight phenolic resin：
By 100g o-cresols, 100g metaformaldehydes, 20g sodium hydroxides, the polyethylene fibre that 25g length is 15 microns
(Mw=4.5 × 106), 30g average diameters be 150 nanometers of amino modified silica, 15g azodicarbonamides and 5gN- months
In 280g N-Methyl pyrrolidones after mixing, flow back osmanthus acyl musculamine acid sodium 4h at 100 DEG C, obtains prepolymer；To pre-
30g length is added in polymers then to flow back at 100 DEG C for 1 micron of staple fiber and 20g metaformaldehydes, ultrasonic disperse 45min
1.5h forms gel；
Gel heat-treatment：Gel is placed in the N-Methyl pyrrolidone steam that pressure is 250kPa, temperature is 200 DEG C
1.5h is then cooled to room temperature, and obtains flame-retardant high-strength lightweight phenolic resin；
Flame-retardant high-strength lightweight phenolic resin is placed in mold, is 100 DEG C in temperature, under conditions of pressure is 15MPa,
After punching press, room temperature is reduced within 10min by punching press 10min for the temperature of diel and product；
(2) preparation of lightweight automotive cover board：
Using aforementioned flame-retardant high-strength lightweight phenolic resin as core material, in core surfaces spraying abrasion-proof layer, spraying abrasion-proof layer
The step of include：By 100g phenolic resin, 30g butyl methacrylates, 12g redox graphenes, 3g polymethyl-benzene base silicon
Oxygen alkane, 16g 2,2,4- trimethylhexane diamines are uniformly mixed in dimethylacetylamide, form coating emulsion, then by coating breast
Liquid is sprayed on core surfaces, cures 30min at 120 DEG C, forms coating；
The performance test results of prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Embodiment 2
(1) prepared by flame-retardant high-strength lightweight phenolic resin：
By 100g m-cresols, 100g paraformaldehydes, 15g sodium hydroxides, the polyethylene fibre that 16g length is 16 microns
(Mw=3 × 106), 20g average diameters be 200 nanometers amino modified silica, 10g 4,4- oxobenzenesulfonyl hydrazide and
In 240g atoleines after mixing, flow back 8g dodecyl benzene sulfonic acid 3.5h at 100 DEG C, obtains prepolymer；To pre-
The staple fiber and 25g paraformaldehydes that addition 24g length is 500 nanometers in polymers, ultrasonic disperse 45min, then next time at 100 DEG C
1h is flowed, gel is formed；
Gel heat-treatment：Gel is placed into 2h in the atoleine steam that pressure is 300kPa, temperature is 150 DEG C, so
Postcooling obtains flame-retardant high-strength lightweight phenolic resin to room temperature；
Flame-retardant high-strength lightweight phenolic resin is placed in mold, is 120 DEG C, pressure 20MPa in temperature, punching press
After punching press, room temperature is reduced within 10min by 5min for the temperature of diel and product；
(2) preparation of lightweight automotive cover board：
Using aforementioned flame-retardant high-strength lightweight phenolic resin as core material, in core surfaces spraying abrasion-proof layer, spraying abrasion-proof layer
The step of include：By 100g phenolic resin, 30g butyl methacrylates, 12g redox graphenes, 3g polymethyl-benzene base silicon
Oxygen alkane, 16g 2,2,4- trimethylhexane diamines are uniformly mixed in dimethylacetylamide, form coating emulsion, then by coating breast
Liquid is sprayed on core surfaces, cures 30min at 120 DEG C, forms coating.
The performance test results of prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Embodiment 3
(1) prepared by flame-retardant high-strength lightweight phenolic resin：
By 100g p-methyl phenols, 30g formaldehyde, 25g magnesium hydroxides, the polyethylene fibre (Mw=9 that 24g length is 8 microns
×106), 36g average diameters be 250 nanometers hydroxyl modification silica, 18gN, N '-dinitrosopentamethlyene tetramines and
In 30g n,N-dimethylacetamide after mixing, flow back 6g fatty alcohols sodium isethionate 4.5h at 100 DEG C, obtains
Prepolymer；36g length is added into prepolymer for 1.5 microns of staple fiber and 10g formaldehyde, ultrasonic disperse 45min then to exist
Flow back 1.5h at 110 DEG C, forms gel；
Gel heat-treatment：Gel is put in the DMAC N,N' dimethyl acetamide steam that pressure is 200kPa, temperature is 180 DEG C
2.5h is set, is then cooled to room temperature, flame-retardant high-strength lightweight phenolic resin is obtained；
Flame-retardant high-strength lightweight phenolic resin is placed in mold, is 80 DEG C, pressure 10MPa in temperature, punching press
After punching press, room temperature is reduced within 10min by 15min for the temperature of diel and product；
(2) preparation of lightweight automotive cover board：
Using aforementioned flame-retardant high-strength lightweight phenolic resin as core material, in core surfaces spraying abrasion-proof layer, spraying abrasion-proof layer
The step of include：By 100g phenolic resin, 30g butyl methacrylates, 12g redox graphenes, 3g polymethyl-benzene base silicon
Oxygen alkane, 16g 2,2,4- trimethylhexane diamines are uniformly mixed in dimethylacetylamide, form coating emulsion, then by coating breast
Liquid is sprayed on core surfaces, after solidification, forms coating.
The performance test results of prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Embodiment 4
(1) prepared by flame-retardant high-strength lightweight phenolic resin：
By 100g hydroquinones, 55g acetaldehyde, 10g potassium hydroxide, the polyethylene fibre (Mw=that 10g length is 20 microns
1.5×106), 12g average diameters be 100 nanometers of hydroxyl modification silica, 6g azodicarbonamides and 2g dodecyl sulphur
In 200g dimethylacetylamides after mixing, flow back sour sodium 5h at 80 DEG C, obtains prepolymer；It is added into prepolymer
The staple fiber and 10g acetaldehyde, ultrasonic disperse 30min that 10g length is 2 microns, then flow back at 110 DEG C 2h, forms gel；
Gel heat-treatment：Gel is placed in the dimethylacetylamide steam that pressure is 150kPa, temperature is 200 DEG C
1h is then cooled to room temperature, and obtains flame-retardant high-strength lightweight phenolic resin；
Flame-retardant high-strength lightweight phenolic resin is placed in mold, is 60 DEG C, pressure 25MPa in temperature, punching press
After punching press, room temperature is reduced within 10min by 20min for the temperature of diel and product；
(2) preparation of lightweight automotive cover board：
Using aforementioned flame-retardant high-strength lightweight phenolic resin as core material, in core surfaces spraying abrasion-proof layer, spraying abrasion-proof layer
The step of include：By 100g phenolic resin, 30g butyl methacrylates, 12g redox graphenes, 3g polymethyl-benzene base silicon
Oxygen alkane, 16g 2,2,4- trimethylhexane diamines are uniformly mixed in dimethylacetylamide, form coating emulsion, then by coating breast
Liquid is sprayed on core surfaces, cures 30min at 120 DEG C, forms coating.
The performance test results of prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Embodiment 5
(1) prepared by flame-retardant high-strength lightweight phenolic resin：
By 100g phenol, 30g formaldehyde, 30g sodium hydroxides, 30g length be 5 microns polyethylene fibre (Mw=1 ×
106), 40g average diameters be 300 nanometers of amino modified silica, 20g 4,4- oxobenzenesulfonyl hydrazide and 10g dodecanes
In 360g tetrahydrofurans after mixing, flow back base alcohol polyethenoxy ether sodium sulfate 3h at 120 DEG C, obtains prepolymer；To
48g length is added in prepolymer then to flow back at 90 DEG C for 300 nanometers of staple fiber and 5g formaldehyde, ultrasonic disperse 60min
2h forms gel；
Gel is placed into 3h in the tetrahydrofuran steam that pressure is 500kPa, temperature is 130 DEG C, is subsequently cooled to room
Temperature obtains flame-retardant high-strength lightweight phenolic resin；
Flame-retardant high-strength lightweight phenolic resin is placed in mold, is 140 DEG C, pressure 5MPa, punching press 2min in temperature,
After punching press, the temperature of diel and product is reduced to room temperature within 10min；
(2) preparation of lightweight automotive cover board：
Using aforementioned flame-retardant high-strength lightweight phenolic resin as core material, in core surfaces spraying abrasion-proof layer, spraying abrasion-proof layer
The step of include：By 100g phenolic resin, 30g butyl methacrylates, 12g redox graphenes, 3g polymethyl-benzene base silicon
Oxygen alkane, 16g 2,2,4- trimethylhexane diamines are uniformly mixed in dimethylacetylamide, form coating emulsion, then by coating breast
Liquid is sprayed on core surfaces, cures 30min at 120 DEG C, forms coating.
The performance test results of prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Comparative example 1
According to the method for embodiment 3, the difference is that, short fibre is not added in the preparation of flame-retardant high-strength lightweight phenolic resin
Dimension, the performance test results of prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Comparative example 2
According to the method for embodiment 3, the difference is that, do not add long fibre in the preparation of flame-retardant high-strength lightweight phenolic resin
Dimension, the performance test results of prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Comparative example 3
According to the method for embodiment 3, the difference is that, foaming is not added in the preparation of flame-retardant high-strength lightweight phenolic resin
The performance test results of agent, prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Comparative example 4
According to the method for embodiment 1, the difference is that, Gel heat-treatment carries out under normal pressure, is as follows；
(1) prepared by flame-retardant high-strength lightweight phenolic resin：
Gel process for preparing is the same as embodiment 1；
Gel heat-treatment：Gel is placed into 1.5h in the N-Methyl pyrrolidone steam that temperature is 200 DEG C, is then cooled down
To room temperature, flame-retardant high-strength lightweight phenolic resin is obtained；
The punch forming process of flame-retardant high-strength lightweight phenolic resin is the same as embodiment 1；
(2) the preparation method is the same as that of Example 1 for lightweight automotive cover board, the property of prepared flame-retardant high-strength lightweight phenolic resin
Energy test result is as shown in table 1.
The performance table of each flame-retardant high-strength lightweight phenolic resin in 1 Examples 1 to 5 of table and comparative example 1~4
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In the skill of the present invention
In art conception range, technical scheme of the present invention can be carried out a variety of simple variants, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, belongs to
Protection scope of the present invention.
Claims (10)
1. a kind of preparation method of flame-retardant high-strength lightweight phenolic resin, which is characterized in that be used to prepare the flame-retardant high-strength
The feedstock composition of lightweight phenolic resin includes：Raw material phenol, raw material aldehyde, staple fiber, long fibre, improved silica, foaming agent,
Surfactant, catalyst and organic solvent；The preparation method comprises the following steps：
(1) long fibre, improved silica, hair for being 5~20 microns by raw material phenol, first part's raw material aldehyde, catalyst, length
In organic solvent after mixing, flow back 3~5h at 80~120 DEG C, obtains prepolymer for infusion and surfactant；
(2) staple fiber and second part raw material aldehyde that addition length is 0.3~2 micron into prepolymer, ultrasonic disperse 30~
60min, then flow back at 90~110 DEG C 1~2h, forms gel；
(3) Gel heat-treatment：Gel placed in the steam that pressure is 150~500kPa, temperature is 130~200 DEG C to 1~
3h is then cooled to room temperature, and obtains flame-retardant high-strength lightweight phenolic resin.
2. the preparation method of flame-retardant high-strength lightweight phenolic resin according to claim 1, wherein with 100 weight of raw material phenol
On the basis of measuring part, the feedstock composition includes the substance of following parts by weight：100 parts by weight of raw material phenol, 30~120 weight of raw material aldehyde
Measure part, 10~48 parts by weight of staple fiber, 10~30 parts by weight of long fibre, 12~40 parts by weight of improved silica, foaming agent 6~
20 parts by weight, 2~10 parts by weight of surfactant, 10~30 parts by weight of catalyst, 200~360 parts by weight of organic solvent；
The length of the staple fiber is 0.3~2 micron；The long stapled length is 5~20 microns.
3. the preparation method of flame-retardant high-strength lightweight phenolic resin according to claim 1 or 2, wherein the staple fiber
It is (1~1.6) with the long stapled mass ratio：1.
4. the preparation method of flame-retardant high-strength lightweight phenolic resin according to claim 1, wherein first part's raw material aldehyde
Weight ratio with second part raw material aldehyde is (3~6)：1.
5. the preparation method of flame-retardant high-strength lightweight phenolic resin according to claim 1, wherein the raw material phenol is selected from
O-cresol, m-cresol, p-cresol, at least one in hydroxymethylphenol, catechol, resorcinol and hydroquinone
Kind；
The raw material aldehyde is selected from formaldehyde, acetaldehyde, propionic aldehyde, butyraldehyde, methacrylaldehyde, cyclohexanone dimethylacetal, benzaldehyde, furfural, miscellaneous
At least one of ring aldehyde, paraformaldehyde, metaformaldehyde.
6. the preparation method of flame-retardant high-strength lightweight phenolic resin according to claim 1, wherein the staple fiber is selected from
Calcium sulfate crystal whiskers, alumina whisker, silicon carbide whisker, carbonization boron whisker, zirconium dioxide whisker, aluminium nitride whisker, zinc oxide are brilliant
At least one of palpus, magnesium sulfate crystal whisker, glass fibre, potassium titanate crystal whisker, magnesium sulfate crystal whisker and silicon nitride crystal whisker；
A diameter of 50~150nm of the staple fiber.
7. the preparation method of flame-retardant high-strength lightweight phenolic resin according to claim 1 or 5, wherein the long fibre
For polyethylene fibre, weight average molecular weight Mw >=1 × 10 of the polyethylene fibre6。
8. the preparation method of flame-retardant high-strength lightweight phenolic resin according to claim 1, wherein the catalyst is selected from
At least one of alkali metal hydroxide, alkaline earth metal hydroxide, carbonate and bicarbonate.
9. the preparation method of flame-retardant high-strength lightweight phenolic resin according to claim 1, wherein the organic solvent choosing
From acetone, N,N-dimethylformamide, N-Methyl pyrrolidone, DMAC N,N' dimethyl acetamide, dimethylacetylamide, dichloromethane
Alkane, triethyl phosphate, chloroform, toluene, ethyl alcohol, acetic acid, ethyl acetate, formic acid, chloroform, tetrahydrofuran, atoleine and
At least one of dimethyl sulfoxide (DMSO).
10. a kind of flame-retardant high-strength lightweight phenolic resin, which is characterized in that the flame-retardant high-strength lightweight phenolic resin is by right
It is required that the preparation method described in any one of 1 to 9 is prepared.
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| CN111548573A (en) * | 2020-05-09 | 2020-08-18 | 中国船舶重工集团公司第七二五研究所 | A kind of fiber-reinforced phenolic resin composite hollow sphere and preparation method thereof |
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Application publication date: 20181102 |