TW201300446A - 由具有液態樹脂組份之聚胺甲酸酯組成物構成之貯存安定性聚胺甲酸酯預浸體,及由彼製成之模製品 - Google Patents
由具有液態樹脂組份之聚胺甲酸酯組成物構成之貯存安定性聚胺甲酸酯預浸體,及由彼製成之模製品 Download PDFInfo
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- TW201300446A TW201300446A TW101110159A TW101110159A TW201300446A TW 201300446 A TW201300446 A TW 201300446A TW 101110159 A TW101110159 A TW 101110159A TW 101110159 A TW101110159 A TW 101110159A TW 201300446 A TW201300446 A TW 201300446A
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- Prior art keywords
- hydroxide
- ammonium
- prepreg
- fiber
- tetraethylammonium
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims abstract description 129
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 126
- 239000007788 liquid Substances 0.000 title claims abstract description 62
- 229920005989 resin Polymers 0.000 title claims abstract description 58
- 239000011347 resin Substances 0.000 title claims abstract description 58
- 238000000465 moulding Methods 0.000 title abstract description 3
- 229920005862 polyol Polymers 0.000 claims abstract description 30
- 150000003077 polyols Chemical class 0.000 claims abstract description 30
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 99
- 239000000835 fiber Substances 0.000 claims description 73
- 238000000034 method Methods 0.000 claims description 66
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- PCHXZXKMYCGVFA-UHFFFAOYSA-N 1,3-diazetidine-2,4-dione Chemical group O=C1NC(=O)N1 PCHXZXKMYCGVFA-UHFFFAOYSA-N 0.000 claims description 44
- 238000004519 manufacturing process Methods 0.000 claims description 43
- 239000003795 chemical substances by application Substances 0.000 claims description 28
- 239000003054 catalyst Substances 0.000 claims description 27
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- -1 inorganic acid anions Chemical class 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 23
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- 238000002844 melting Methods 0.000 claims description 22
- 230000008018 melting Effects 0.000 claims description 22
- BWLBGMIXKSTLSX-UHFFFAOYSA-N 2-hydroxyisobutyric acid Chemical compound CC(C)(O)C(O)=O BWLBGMIXKSTLSX-UHFFFAOYSA-N 0.000 claims description 21
- 238000005470 impregnation Methods 0.000 claims description 20
- 125000001931 aliphatic group Chemical group 0.000 claims description 16
- 238000004132 cross linking Methods 0.000 claims description 15
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 14
- 125000000524 functional group Chemical group 0.000 claims description 14
- 239000011521 glass Substances 0.000 claims description 14
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 14
- 239000012948 isocyanate Substances 0.000 claims description 13
- 239000000126 substance Substances 0.000 claims description 13
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 12
- LCTONWCANYUPML-UHFFFAOYSA-M Pyruvate Chemical compound CC(=O)C([O-])=O LCTONWCANYUPML-UHFFFAOYSA-M 0.000 claims description 12
- 239000003365 glass fiber Substances 0.000 claims description 12
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 12
- 239000004917 carbon fiber Substances 0.000 claims description 11
- 229920000728 polyester Polymers 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 11
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 10
- 239000004744 fabric Substances 0.000 claims description 10
- NHGXDBSUJJNIRV-UHFFFAOYSA-M tetrabutylammonium chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CCCC NHGXDBSUJJNIRV-UHFFFAOYSA-M 0.000 claims description 10
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 10
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 9
- 239000000654 additive Substances 0.000 claims description 9
- 239000002981 blocking agent Substances 0.000 claims description 9
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 9
- 150000002513 isocyanates Chemical class 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 8
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical group OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims description 8
- 229920000570 polyether Polymers 0.000 claims description 8
- FPGGTKZVZWFYPV-UHFFFAOYSA-M tetrabutylammonium fluoride Chemical compound [F-].CCCC[N+](CCCC)(CCCC)CCCC FPGGTKZVZWFYPV-UHFFFAOYSA-M 0.000 claims description 8
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 7
- 239000004760 aramid Substances 0.000 claims description 7
- 229920006231 aramid fiber Polymers 0.000 claims description 7
- 230000000903 blocking effect Effects 0.000 claims description 7
- 239000000155 melt Substances 0.000 claims description 7
- 239000000178 monomer Substances 0.000 claims description 7
- 239000011527 polyurethane coating Substances 0.000 claims description 7
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 7
- WJIOHMVWGVGWJW-UHFFFAOYSA-N 3-methyl-n-[4-[(3-methylpyrazole-1-carbonyl)amino]butyl]pyrazole-1-carboxamide Chemical compound N1=C(C)C=CN1C(=O)NCCCCNC(=O)N1N=C(C)C=C1 WJIOHMVWGVGWJW-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
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 6
- WDJHALXBUFZDSR-UHFFFAOYSA-M acetoacetate Chemical compound CC(=O)CC([O-])=O WDJHALXBUFZDSR-UHFFFAOYSA-M 0.000 claims description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 6
- 125000005442 diisocyanate group Chemical group 0.000 claims description 6
- UAOMVDZJSHZZME-UHFFFAOYSA-N diisopropylamine Chemical compound CC(C)NC(C)C UAOMVDZJSHZZME-UHFFFAOYSA-N 0.000 claims description 6
- 150000002118 epoxides Chemical class 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000004745 nonwoven fabric Substances 0.000 claims description 6
- 239000004417 polycarbonate Substances 0.000 claims description 6
- 229920000515 polycarbonate Polymers 0.000 claims description 6
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- 150000002148 esters Chemical class 0.000 claims description 5
- 239000002657 fibrous material Substances 0.000 claims description 5
- 229910052736 halogen Inorganic materials 0.000 claims description 5
- 150000002367 halogens Chemical class 0.000 claims description 5
- 150000007524 organic acids Chemical class 0.000 claims description 5
- 150000004714 phosphonium salts Chemical group 0.000 claims description 5
- 229920003023 plastic Polymers 0.000 claims description 5
- 239000004033 plastic Substances 0.000 claims description 5
- 229920000058 polyacrylate Polymers 0.000 claims description 5
- 229920000768 polyamine Polymers 0.000 claims description 5
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 5
- SEACXNRNJAXIBM-UHFFFAOYSA-N triethyl(methyl)azanium Chemical compound CC[N+](C)(CC)CC SEACXNRNJAXIBM-UHFFFAOYSA-N 0.000 claims description 5
- NIPLIJLVGZCKMP-UHFFFAOYSA-M Neurine Chemical compound [OH-].C[N+](C)(C)C=C NIPLIJLVGZCKMP-UHFFFAOYSA-M 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 4
- HTZCNXWZYVXIMZ-UHFFFAOYSA-M benzyl(triethyl)azanium;chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC1=CC=CC=C1 HTZCNXWZYVXIMZ-UHFFFAOYSA-M 0.000 claims description 4
- NDKBVBUGCNGSJJ-UHFFFAOYSA-M benzyltrimethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)CC1=CC=CC=C1 NDKBVBUGCNGSJJ-UHFFFAOYSA-M 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- 238000010276 construction Methods 0.000 claims description 4
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 4
- FHGDVMFLEMHKBX-UHFFFAOYSA-N ethanol;triethyl(methyl)azanium Chemical compound CCO.CC[N+](C)(CC)CC FHGDVMFLEMHKBX-UHFFFAOYSA-N 0.000 claims description 4
- 150000004679 hydroxides Chemical class 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- JZLKJRFMBQFOLE-UHFFFAOYSA-N methanol triethyl(methyl)azanium Chemical compound CO.C[N+](CC)(CC)CC JZLKJRFMBQFOLE-UHFFFAOYSA-N 0.000 claims description 4
- MOVBJUGHBJJKOW-UHFFFAOYSA-N methyl 2-amino-5-methoxybenzoate Chemical compound COC(=O)C1=CC(OC)=CC=C1N MOVBJUGHBJJKOW-UHFFFAOYSA-N 0.000 claims description 4
- 125000005496 phosphonium group Chemical group 0.000 claims description 4
- DVUVKWLUHXXIHK-UHFFFAOYSA-N tetraazanium;tetrahydroxide Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[OH-].[OH-].[OH-].[OH-] DVUVKWLUHXXIHK-UHFFFAOYSA-N 0.000 claims description 4
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 4
- CIFIGXMZHITUAZ-UHFFFAOYSA-M tetraethylazanium;benzoate Chemical compound CC[N+](CC)(CC)CC.[O-]C(=O)C1=CC=CC=C1 CIFIGXMZHITUAZ-UHFFFAOYSA-M 0.000 claims description 4
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 4
- IEVVGBFMAHJELO-UHFFFAOYSA-M tetramethylazanium;benzoate Chemical compound C[N+](C)(C)C.[O-]C(=O)C1=CC=CC=C1 IEVVGBFMAHJELO-UHFFFAOYSA-M 0.000 claims description 4
- QGAKFUJUPKPDCN-UHFFFAOYSA-M tetraoctylazanium;fluoride Chemical compound [F-].CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)CCCCCCCC QGAKFUJUPKPDCN-UHFFFAOYSA-M 0.000 claims description 4
- DCFYRBLFVWYBIJ-UHFFFAOYSA-M tetraoctylazanium;hydroxide Chemical compound [OH-].CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)CCCCCCCC DCFYRBLFVWYBIJ-UHFFFAOYSA-M 0.000 claims description 4
- JAJRRCSBKZOLPA-UHFFFAOYSA-M triethyl(methyl)azanium;hydroxide Chemical compound [OH-].CC[N+](C)(CC)CC JAJRRCSBKZOLPA-UHFFFAOYSA-M 0.000 claims description 4
- MNWUNZHJAPWUOT-UHFFFAOYSA-M trihexyl(tetradecyl)azanium;hydroxide Chemical compound [OH-].CCCCCCCCCCCCCC[N+](CCCCCC)(CCCCCC)CCCCCC MNWUNZHJAPWUOT-UHFFFAOYSA-M 0.000 claims description 4
- OQZAQBGJENJMHT-UHFFFAOYSA-N 1,3-dibromo-5-methoxybenzene Chemical compound COC1=CC(Br)=CC(Br)=C1 OQZAQBGJENJMHT-UHFFFAOYSA-N 0.000 claims description 3
- ATOUXIOKEJWULN-UHFFFAOYSA-N 1,6-diisocyanato-2,2,4-trimethylhexane Chemical compound O=C=NCCC(C)CC(C)(C)CN=C=O ATOUXIOKEJWULN-UHFFFAOYSA-N 0.000 claims description 3
- QGLRLXLDMZCFBP-UHFFFAOYSA-N 1,6-diisocyanato-2,4,4-trimethylhexane Chemical compound O=C=NCC(C)CC(C)(C)CCN=C=O QGLRLXLDMZCFBP-UHFFFAOYSA-N 0.000 claims description 3
- HSNJERRVXUNQLS-UHFFFAOYSA-N 1-(4-tert-butylphenyl)propan-2-one Chemical compound CC(=O)CC1=CC=C(C(C)(C)C)C=C1 HSNJERRVXUNQLS-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Natural products CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- NAUBYZNGDGDCHH-UHFFFAOYSA-N N=C=O.N=C=O.CCCC(C)C Chemical compound N=C=O.N=C=O.CCCC(C)C NAUBYZNGDGDCHH-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 229920003235 aromatic polyamide Polymers 0.000 claims description 3
- VBQDSLGFSUGBBE-UHFFFAOYSA-N benzyl(triethyl)azanium Chemical compound CC[N+](CC)(CC)CC1=CC=CC=C1 VBQDSLGFSUGBBE-UHFFFAOYSA-N 0.000 claims description 3
- FKPSBYZGRQJIMO-UHFFFAOYSA-M benzyl(triethyl)azanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC1=CC=CC=C1 FKPSBYZGRQJIMO-UHFFFAOYSA-M 0.000 claims description 3
- YOUGRGFIHBUKRS-UHFFFAOYSA-N benzyl(trimethyl)azanium Chemical compound C[N+](C)(C)CC1=CC=CC=C1 YOUGRGFIHBUKRS-UHFFFAOYSA-N 0.000 claims description 3
- KFSZGBHNIHLIAA-UHFFFAOYSA-M benzyl(trimethyl)azanium;fluoride Chemical compound [F-].C[N+](C)(C)CC1=CC=CC=C1 KFSZGBHNIHLIAA-UHFFFAOYSA-M 0.000 claims description 3
- JGCWKVKYRNXTMD-UHFFFAOYSA-N bicyclo[2.2.1]heptane;isocyanic acid Chemical compound N=C=O.N=C=O.C1CC2CCC1C2 JGCWKVKYRNXTMD-UHFFFAOYSA-N 0.000 claims description 3
- XXKOQQBKBHUATC-UHFFFAOYSA-N cyclohexylmethylcyclohexane Chemical compound C1CCCCC1CC1CCCCC1 XXKOQQBKBHUATC-UHFFFAOYSA-N 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 claims description 3
- 150000003512 tertiary amines Chemical class 0.000 claims description 3
- QSUJAUYJBJRLKV-UHFFFAOYSA-M tetraethylazanium;fluoride Chemical compound [F-].CC[N+](CC)(CC)CC QSUJAUYJBJRLKV-UHFFFAOYSA-M 0.000 claims description 3
- ZYSDERHSJJEJDS-UHFFFAOYSA-M tetrakis-decylazanium;hydroxide Chemical compound [OH-].CCCCCCCCCC[N+](CCCCCCCCCC)(CCCCCCCCCC)CCCCCCCCCC ZYSDERHSJJEJDS-UHFFFAOYSA-M 0.000 claims description 3
- HNRXDBMBQAOWFV-UHFFFAOYSA-M tetraoctadecylazanium;hydroxide Chemical compound [OH-].CCCCCCCCCCCCCCCCCC[N+](CCCCCCCCCCCCCCCCCC)(CCCCCCCCCCCCCCCCCC)CCCCCCCCCCCCCCCCCC HNRXDBMBQAOWFV-UHFFFAOYSA-M 0.000 claims description 3
- OSBSFAARYOCBHB-UHFFFAOYSA-N tetrapropylammonium Chemical compound CCC[N+](CCC)(CCC)CCC OSBSFAARYOCBHB-UHFFFAOYSA-N 0.000 claims description 3
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims description 3
- QVOFCQBZXGLNAA-UHFFFAOYSA-M tributyl(methyl)azanium;hydroxide Chemical compound [OH-].CCCC[N+](C)(CCCC)CCCC QVOFCQBZXGLNAA-UHFFFAOYSA-M 0.000 claims description 3
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical group C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 3
- HADKRTWCOYPCPH-UHFFFAOYSA-M trimethylphenylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C1=CC=CC=C1 HADKRTWCOYPCPH-UHFFFAOYSA-M 0.000 claims description 3
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 claims description 3
- UHAUNWBFEUXSNO-UHFFFAOYSA-N (2,3,4-trimethylphenyl)azanium;iodide Chemical compound [I-].CC1=CC=C([NH3+])C(C)=C1C UHAUNWBFEUXSNO-UHFFFAOYSA-N 0.000 claims description 2
- KYVBNYUBXIEUFW-UHFFFAOYSA-N 1,1,3,3-tetramethylguanidine Chemical compound CN(C)C(=N)N(C)C KYVBNYUBXIEUFW-UHFFFAOYSA-N 0.000 claims description 2
- LTMRRSWNXVJMBA-UHFFFAOYSA-L 2,2-diethylpropanedioate Chemical compound CCC(CC)(C([O-])=O)C([O-])=O LTMRRSWNXVJMBA-UHFFFAOYSA-L 0.000 claims description 2
- SDXAWLJRERMRKF-UHFFFAOYSA-N 3,5-dimethyl-1h-pyrazole Chemical compound CC=1C=C(C)NN=1 SDXAWLJRERMRKF-UHFFFAOYSA-N 0.000 claims description 2
- NSPMIYGKQJPBQR-UHFFFAOYSA-N 4H-1,2,4-triazole Chemical compound C=1N=CNN=1 NSPMIYGKQJPBQR-UHFFFAOYSA-N 0.000 claims description 2
- CMNQIVHHHBBVSC-UHFFFAOYSA-N 5-hydroxy-3,4-dihydro-2h-isoquinolin-1-one Chemical compound O=C1NCCC2=C1C=CC=C2O CMNQIVHHHBBVSC-UHFFFAOYSA-N 0.000 claims description 2
- UZGARMTXYXKNQR-UHFFFAOYSA-K 7,7-dimethyloctanoate;neodymium(3+) Chemical compound [Nd+3].CC(C)(C)CCCCCC([O-])=O.CC(C)(C)CCCCCC([O-])=O.CC(C)(C)CCCCCC([O-])=O UZGARMTXYXKNQR-UHFFFAOYSA-K 0.000 claims description 2
- 229920002748 Basalt fiber Polymers 0.000 claims description 2
- BTJSEUZLCUZXEE-UHFFFAOYSA-N C(C)O.C[N+](C)(C)C Chemical compound C(C)O.C[N+](C)(C)C BTJSEUZLCUZXEE-UHFFFAOYSA-N 0.000 claims description 2
- UBTZPBFNZVZBSV-UHFFFAOYSA-N C(CC(=O)C)(=O)O.C(C1=CC=CC=C1)N(N(CC)CC)CC Chemical compound C(CC(=O)C)(=O)O.C(C1=CC=CC=C1)N(N(CC)CC)CC UBTZPBFNZVZBSV-UHFFFAOYSA-N 0.000 claims description 2
- XXFXYMOTLATVSM-UHFFFAOYSA-N C(CC)[N+](CCC)(CCC)CCC.CO Chemical compound C(CC)[N+](CCC)(CCC)CCC.CO XXFXYMOTLATVSM-UHFFFAOYSA-N 0.000 claims description 2
- HAQVNYPYRSKTRK-UHFFFAOYSA-N C(CCCC)[N+](CCCCC)(CCCCC)CCCCC.C(C)O Chemical compound C(CCCC)[N+](CCCCC)(CCCCC)CCCCC.C(C)O HAQVNYPYRSKTRK-UHFFFAOYSA-N 0.000 claims description 2
- LGFGKDOKPLVTAU-UHFFFAOYSA-N C(CCCCCCC)[N+](CCCCCCCC)(CCCCCCCC)CCCCCCCC.C(C)O Chemical compound C(CCCCCCC)[N+](CCCCCCCC)(CCCCCCCC)CCCCCCCC.C(C)O LGFGKDOKPLVTAU-UHFFFAOYSA-N 0.000 claims description 2
- ZVMVQBODFWIGRN-UHFFFAOYSA-N C(CCCCCCCCCCCCC)[N+](CCCCCC)(CCCCCC)CCCCCC.C(C)O Chemical compound C(CCCCCCCCCCCCC)[N+](CCCCCC)(CCCCCC)CCCCCC.C(C)O ZVMVQBODFWIGRN-UHFFFAOYSA-N 0.000 claims description 2
- SXTLJZDPHFWQKF-UHFFFAOYSA-N C(CCCCCCCCCCCCCCCCC)[N+](CCCCCCCCCCCCCCCCCC)(CCCCCCCCCCCCCCCCCC)CCCCCCCCCCCCCCCCCC.C(C)O Chemical compound C(CCCCCCCCCCCCCCCCC)[N+](CCCCCCCCCCCCCCCCCC)(CCCCCCCCCCCCCCCCCC)CCCCCCCCCCCCCCCCCC.C(C)O SXTLJZDPHFWQKF-UHFFFAOYSA-N 0.000 claims description 2
- DOZZUJWJSHISQF-UHFFFAOYSA-N CCCCCCCCCCCCCCN.CO Chemical compound CCCCCCCCCCCCCCN.CO DOZZUJWJSHISQF-UHFFFAOYSA-N 0.000 claims description 2
- VVYLVMMPXXZWFQ-UHFFFAOYSA-N CO.C[N+](C1=CC=CC=C1)(C)C Chemical compound CO.C[N+](C1=CC=CC=C1)(C)C VVYLVMMPXXZWFQ-UHFFFAOYSA-N 0.000 claims description 2
- AWLLEQMPAZXSJL-UHFFFAOYSA-N C[N+](C1=CC=CC=C1)(C)C.C(C)O Chemical compound C[N+](C1=CC=CC=C1)(C)C.C(C)O AWLLEQMPAZXSJL-UHFFFAOYSA-N 0.000 claims description 2
- SDBFAOLKCDCBHG-UHFFFAOYSA-N C[N+](CCCC)(CCCC)CCCC.C(C)O Chemical compound C[N+](CCCC)(CCCC)CCCC.C(C)O SDBFAOLKCDCBHG-UHFFFAOYSA-N 0.000 claims description 2
- GSDIGAFFRSTBAX-UHFFFAOYSA-N C[N+](CCCC)(CCCC)CCCC.CO Chemical compound C[N+](CCCC)(CCCC)CCCC.CO GSDIGAFFRSTBAX-UHFFFAOYSA-N 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- 229920002292 Nylon 6 Polymers 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims description 2
- UDYGXWPMSJPFDG-UHFFFAOYSA-M benzyl(tributyl)azanium;bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CC1=CC=CC=C1 UDYGXWPMSJPFDG-UHFFFAOYSA-M 0.000 claims description 2
- VJGNLOIQCWLBJR-UHFFFAOYSA-M benzyl(tributyl)azanium;chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CC1=CC=CC=C1 VJGNLOIQCWLBJR-UHFFFAOYSA-M 0.000 claims description 2
- QVGHRPSUYBFXLH-UHFFFAOYSA-M benzyl(tributyl)azanium;iodide Chemical compound [I-].CCCC[N+](CCCC)(CCCC)CC1=CC=CC=C1 QVGHRPSUYBFXLH-UHFFFAOYSA-M 0.000 claims description 2
- YWQWUCTYYCXUMJ-UHFFFAOYSA-N benzyl(triethyl)azanium methanol Chemical compound CO.C(C1=CC=CC=C1)[N+](CC)(CC)CC YWQWUCTYYCXUMJ-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
本發明係關於由具有液態樹脂組份(較佳為液態多元醇)之聚胺甲酸酯組成物構成之貯存安定性聚胺甲酸酯預浸體,及由彼製成之模製品。
Description
本發明係關於由具有液態樹脂組份(較佳為液態多元醇)之聚胺甲酸酯組成物構成之貯存安定性聚胺甲酸酯預浸體,及由彼製成之模製品。
具有液態樹脂組份(較佳為液態多元醇)之聚胺甲酸酯組成物特別適於製造貯存安定性聚胺甲酸酯預浸體及由彼製成之模製品(複合材料組份)。貯存安定性聚胺甲酸酯預浸體係藉使用將織物及不織布使用該反應性聚胺甲酸酯組成物浸漬之方法而得。
各種模製方法,諸如反應轉注成形(RTM)法,包含將強化纖維置入模具中,將模具關閉,將可交聯樹脂調合物置入模具中,繼而將樹脂交聯(通常藉熱供應)。
此方法之其中一限制為將強化纖維放置於模具中較為困難。布料或不織布之個別層必需切割以適合廣大多樣化之模具幾何形狀。這可既耗時且亦複雜,尤其是當模具亦欲含有泡沫或其他核心時。具簡易操作及已存在重塑可能性之可模製性纖維強化品在此處亦合乎需要。
預浸體形式之纖維強化材料已用於許多工業應用中,因為其易於操作且與其他濕式積層技術相比之下,於製程期間之效能增加。
此系統(以及較快循環時間及較高貯存安定性(甚至
於室溫下))之工業用戶亦要求將預浸體切割而不會使切割工具於自動化切割及個別預浸體層之積層期間被經常黏滯之基質材料污染之可能性。
如同聚酯、乙烯酯及環氧系統一樣,交聯基質系統領域中有一系列之專門的樹脂。這些亦包括聚胺甲酸酯樹脂,其因為具有韌性、損傷容限性及強度,故尤其用於藉拉擠法以製造複合材料廓線。所用異氰酸酯的毒性則經常被提及為其缺點。
與乙烯酯、不飽和聚酯樹脂(UPR)或UPR-聚胺甲酸酯混成樹脂相比之下,聚胺甲酸酯複合材料亦顯現較優良之韌性。
以環氧系統為基底,預浸體及由彼製成之複合材料乃例如述於WO 98/50211,US 4,992,228,US 5,080,857,US 5,427,725,GB 2007676,GB 2182074,EP 309 221,EP 297 674,WO 89/04335,US 5,532,296及US 4,377,657,US 4,757,120中。
WO 2006/043019中說明以環氧樹脂聚胺甲酸酯粉末為基底之預浸體的製法。
此外,以作為基質之粉末形式之熱塑性塑料為基底的預浸體係已知。
US 2004/0231598中說明一種其中令微粒通過具有靜電之特殊加速室中的方法。此裝置係用於玻璃、芳綸或碳纖維基質之塗覆以供製造熱塑性塑料預浸體。在樹脂方面,被提及的有聚乙烯(PE)、聚丙烯(PP)、聚醚醚酮(
PEEK)、聚醚碸(PES)、聚苯碸(PPS)、聚醯亞胺(PI)、聚醯胺(PA)、聚碳酸酯(PC)、聚對苯二甲酸乙二酯(PET)、聚胺甲酸酯(PU)、聚酯及氟基聚合物。由彼製成之熱塑性塑料預浸體結構顯現固有之韌性、良好之黏彈性阻尼性能、無限貯存期、及良好之化學品抗性及可回收性。
WO 98/31535中說明一種粉末浸漬法,其係將待浸漬之玻璃或碳纖維股以微粒/液體或微粒/氣體以明確之速度廓線撞擊。其中,粉末係由陶瓷或熱塑性材料,尤其是熱塑性聚胺甲酸酯所組成。
WO 99/64216中說明預浸體及複合材料及其製法,其中所用乳膠所含聚合物微粒如此之小以至於能進行個別之纖維塗覆。該微粒聚合物具有至少5000厘泊之黏度且為熱塑性或為交聯性聚胺甲酸酯聚合物。
EP 0590702中說明供製造預浸體之粉末浸漬法,其中該粉末係由熱塑性塑料及反應性單體或預聚合物之混合物所組成。WO 2005/091715同樣地說明使用熱塑性塑料於製造預浸體之用途。
Michaeli等人於Coatings & Composite Materials,No.19,p.37-39,1997中說明以熱塑性聚胺甲酸酯(稱為TPU)進行拉擠法之粉末技術之發展。
此外,於文獻Processing and properties of thermoplastic polyurethane prepreg.(Ma,C.C.M.;Chiang,C.L.Annual Technical Conference -Society of
Plastics Engineers(1991),49th 2065-9)中揭露以含有溶劑及水之TPU系統為基底之熱塑性聚胺甲酸酯(TPU)預浸體。
具有以2-組份聚胺甲酸酯(2-C PUR)為基底之基質的預浸體係已知。2-C PUR之類目實質上包含標準反應性聚胺甲酸酯樹脂系統。原則上,此為由兩個個別組份所組成之系統。一個組份中之重要成分永遠是聚異氰酸酯,至於第二個組份則為多元醇,或者最近之發展則亦為胺基-或胺-多元醇混合物。這兩個部分僅在製程之前不久混合在一起。其後,藉由加聚作用發生化學熟化,同時形成聚胺甲酸酯或聚脲之網狀系統。將兩種組份混合後,2-組份系統具有有限之製程時間(靜置時間,可使用時間),因反應開始而導致黏度逐漸增加且最終導致系統之凝膠化。然而,有許多因素決定其加工性的有效期限:反應參與者之反應性、催化反應、濃度、溶解度、濕量、NCO/OH比及環境溫度為最重要[Lackharze,Stoye/Freitag,Hauser-Verlag 1996,pages 210/212]。以此2-C PUR系統為基底之預浸體的缺點在於僅有短時間可利用以供將預浸體製成複合材料。結果是,此預浸體不能安定數小時,更遑論天數了。
下列者係說明以2-C PUR系統為基底之聚胺甲酸酯預浸體或複合材料。在K.Recker之文獻中報告特別參照SMC組份之加工性質所進行之2-C聚胺甲酸酯系統之樹脂mat法之發展。(Baypreg-a novel POLYURETHANE
material for the resin mat process,Recker,Klaus,Kunststoffe-Plastics 8,1981)。
WO 2005/049301揭露催化性活化之2-C PUR系統,其係將聚異氰酸酯組份與多元醇混合,再藉拉擠法製成複合材料。
WO 2005/106155揭露供營建業用之纖維強化複合材料,其係藉以2-C聚胺甲酸酯系統進行長纖維注射技術(LFI)而製得。
JP 2004196851中說明經由使用以聚合亞甲基二苯基二異氰酸酯(MDI)及具體含OH基之化合物為基底之2-C PUR基質而由碳纖維及有機纖維(諸如麻)中所製成之複合材料。
EP 1 319 503說明聚胺甲酸酯複合材料,其乃使用供纖維層壓板用之浸漬有2-C PUR樹脂之特殊聚胺甲酸酯覆蓋層(其係覆蓋核心層,例如蜂窩紙芯)。此2-C PUR樹脂係由(例如)MDI與得自氧化乙烯氧化丙烯共聚物之聚丙三醇類及二醇類的混合物所組成。
WO 2003/101719中說明聚胺甲酸酯為基底之複合材料及其製法。其為具有明確黏度及具體凝膠化時間之2-C聚胺甲酸酯樹脂。
2-C PUR系統亦於“Fiber reinforced polyurethane composites:shock tolerant components with particular emphasis on armor plating”(Ratcliffe,Colin P.;Crane,RogerM.;Santiago,Armando L.,AMD(1995),211
(Innovative Processing and Characterization of Composite Materials),29-37.)and in Fiber-reinforced polyurethane composites.I.Process feasibility and morphology.(Ma,Chen Chi M.;Chen,Chin Hsing.International SAMPE Symposium and Exhibition(1992),37(Mater.Work.You 21st Century),1062-74)中討論。
除了不同之黏結劑基礎外,濕熟化漆在其組成以及其性質方面均大幅相當於類似之2-C系統。原則上,係使用相同的溶劑、色素、填料及輔助物質。不像2-C漆,基於安定性的因素,這些系統在其應用之前無論如何要容忍無濕氣之狀態。
亦已知者為以無反應性PUR彈性體為基底之物理乾燥系統。這些為得自二醇類及二異氰酸酯類(較佳為MDI、TDI、HDI及IPDI)之高分子量、直鏈、熱塑性胺甲酸酯。此熱塑性系統通常顯現極高黏度且因此亦顯現極高之製程溫度。此嚴苛地阻礙其供預浸體之用途。在以纖維複合材料製造預浸體中,於反應系統中使用粉末較不常見且至今已限制在為數不多的使用領域上。最常見之將粉末塗佈至纖維表面上的方法可能為流體床法(流體床浸漬法)。經由向上導向之流動,將粉末微粒轉化成顯現流體狀性質的狀態。此方法於EP 590 702中使用。其中,乃將個別纖維束之股分開地漂浮,再於流體床中塗覆上粉末。此處之粉末係由反應性及熱塑性粉末之混合物所組成,因而可使基質之性質最理想化。最後,將個別粗紗(纖維束)鋪
在一起,再將數層於16巴之壓力下壓縮約20分鐘。溫度在250至350℃間變化。然而,流體床法中,經常發生不規則的塗覆,尤其是如果纖維股未分開拉時。
有關於US 20040231598,其提出具有類似於流體床法功能之方法。其中,氣流將微粒運送至基質中,再經由具體配置而完成粉末之均勻沈積。
另一方法述於US 20050215148中。粉末於纖維上之均勻分佈係使用剛才說明之裝置達成。其中,粒徑在1至2000微米之範圍內。一些實例中,塗覆係由一側或兩側完成。經由粉末之均勻塗佈,則可於接續之預浸體壓縮後,得到無氣泡之層壓板。
另一申請案WO 2006/043019說明粉末形式之帶有環氧及胺基終端之樹脂。其中,乃將粉末混合,再塗佈至纖維上。其後,將微粒燒結。粒徑落在1至3000微米間,但較佳介於1至150微米間。
此粒徑要求到相當小直徑之限制亦為密西根州立大學之研究中所推薦。此處之理論為小直徑之微粒似乎比大直徑之微粒更能穿透至個別纖維間的洞中。(S.Padaki,L.T.Drzal:a simulation study on the effects of particle size on the consolidation of polymer powder impregnated tapes,Department of Chemical Engineering,Michigan State University,Composites:Part A(1999),pp.325-337)。
除了預浸體技術外,反應性粉末系統亦用於其他標準
方法中,例如於纏繞技術中[M.N.Ghasemi Nejhad,K.M.Ikeda:Design,manufacture and characterization of composites using on-line recycled thermoplastic powder impregnation of fibres and in-situ filament winding,Department of Mechanical Engineering,University of Hawaii at Manoa,Journal of Thermoplastic Composite Materials,Vol 11,pp.533-572,November 1998]或於拉擠法中。供拉擠法方面,乃例如將纖維股(絲束預浸體)塗覆上粉末並首度纏繞,再以所謂絲束預浸體形式貯存。供此製造之一種可能性乃述於SAMPLE期刊之文獻中[R.E.Allred,S.P.Wesson,D.A.Babow:powder impregnation studies for high temperature towpregs,Adherent Technologies,SAMPE Journal,Vol.40,No.6,pp.40-48,November/December 2004]。另一研究中,乃藉拉擠法將這些絲束預浸體一起壓擠,再熟化以得材料組份[N.C.Parasnis,K.Ramani,H.M.Borgaonkar:Ribbonizing of electrostatic powder spray impregnated thermoplastic tows by pultrusion,School of Mechanical Engineering,Purdue University,Composites,Part A,Applied science and manufacturing,Vol.27,pp.567-574,1996]。雖然絲束預浸體之製造及接續於拉擠法中之壓縮已經以脲醛系統進行,但迄今在很大程度上僅有熱塑性系統用於此法中。
DE 102009001793.3及DE 102009001806.9中乃說明製造貯存安定性預浸體之方法,該預浸體實質上由下列者
所組成:A)至少一種纖維支架及B)至少一種作為基質材料之粉末形式的反應性聚胺甲酸酯組成物。
本目的係欲發現易於操作、亦即無毒性、以聚胺甲酸酯為基底之預浸體系統(以聚胺甲酸酯組成物為基底)之製法。本發明之進一步目的係欲發現可藉由簡單方法製得之具聚胺甲酸酯基質材料之預浸體,其中主要強調點必需放在預浸體之處理及貯存期限上。
供製造預浸體方面,如果非交聯性基質材料製備之黏度夠低以確保具有足夠纖維體積含量之纖維支架在複合材料組份的製造期間濕化,則將有利,此期間有搖溶現象亦有利,故可避免垂直組份片段中樹脂之流失。
經由選擇供製備基質材料之適當原材料,必需保證未完全反應之基質材料之熔化與反應之完成間要有夠長的製程時間(依複合材料之製造中的特定應用而定)。
貯存安定性聚胺甲酸酯預浸體,及由彼製成之模製品已由
DE 102009001793及DE 102009001806中得知。
DE 102010029355.5係關於供聚胺甲酸酯預浸體用之熔融應用法。
DE 102010030233.3說明具有複曲率之聚胺甲酸酯預浸體系統。
DE 102010030234.1呈現含溶劑之聚胺甲酸酯預浸體系統。
DE 102010041239.2申請彩色聚胺甲酸酯預浸體系統
之專利。DE 102010041256.2接著關於於固定箔上之聚胺甲酸酯預浸體系統,而DE 102010041243.0說明具有小於50%纖維體積含量之聚胺甲酸酯預浸體系統。所有上述文件之常見特徵為其中所述之樹脂組份(聚合物b)必需具有固態樹脂之特質,亦即至少40℃之玻璃轉化溫度(Tg)。此高Tg迄今被視為是確保預浸體之貯存安定性所必需。
意外地,如今發現,在已浸漬、反應性及貯存安定性聚胺甲酸酯預浸體部分中所說明之這些應用中,如果彼等使用液態樹脂組份(較佳為多元醇)作為樹脂組份,則可實現特別的優點。有關製程技術之顯而易見的優點不僅在於預浸體之製造,亦在於接續之壓擠以得具較佳加工性之複合材料組份,而不會導致犠牲預浸體之貯存安定性。尤其,預浸體之製造是在無不期望的起泡或其他表面破裂之情況下進行。在接續之壓擠以得複合材料期間,液態樹脂組份導致層內之流動改善,因此得到優良性質的材料。
此外,由於通常基質材料於較高溫度下之較低黏度,故壓擠以得複合材料組份之作用可於較低壓力下進行,且此為有利的。
故所得預浸體具有與DE 102009001793或DE 102009001806中所述者至少相同或甚至改善之製程性質,其可用於製造高效能之複合材料以供營建、汽車、航太工
業、能源技術(風力發電廠)及於船及造船業部門之各種應用。根據本發明可用之反應性聚胺甲酸酯組成物為對環境無害、低成本、顯現良好機械性質,可輕易進行製程且於熟化後具有良好耐天氣性且在剛性與撓性之間取得平衡關聯之特徵。
本發明之主題為一種預浸體,實質上由下列者所組成A)至少一種纖維支架及B)至少一種作為基質材料之反應性聚胺甲酸酯組成物,其中該聚胺甲酸酯組成物實質上含有下列者之混合物:液態樹脂組份b),其具有對異氰酸酯具反應性之官能基且具有低於25℃之Tg或熔點,且具有50至2000毫克氫氧化鉀/克之OH數,及作為熟化劑a)之內部阻斷及/或被阻斷劑所阻斷之二-或聚異氰酸酯。
玻璃轉化溫度Tg及熔點係根據DIN EN ISO 11357-1及DIN 53765測定。
冷卻至室溫後,根據本發明所製之根據本發明預浸體於室溫下顯現極高之貯存安定性,但前提是基質材料具有至少40℃之Tg。依所含反應性聚胺甲酸酯組成物及催化反應而定,其於室溫下至少數天,但通常預浸體於40℃或更低之溫度下可安定貯存數星期或甚至數個月。所製得之
預浸體通常不黏滯,故極易於操作及進一步進行製程。因此,根據本發明所用之反應性或高度反應性聚胺甲酸酯組成物於纖維支架上顯現極良好之黏著及分佈。在將預浸體進一步製成複合材料期間(例如藉於增溫下壓縮),則纖維支架可發生極良好之浸漬,這是由於在交聯反應之前、凝膠化發生之前或整個聚胺甲酸酸酯完全熟化(由於反應性或高度反應性聚胺甲酸酯組成物於增溫下之交聯反應)之前,液態低黏度反應性或高度反應性聚胺甲酸酯聚合物可將支架之纖維濕化得非常好的緣故。
依所用之反應性或高度反應性聚胺甲酸酯組成物之組成及已加入之催化劑而定,複合材料組份製造中之交聯反應速率以及基質之性質可在廣泛範圍間變化。
本發明文中,供製造預浸體所用之反應性或高度反應性聚胺甲酸酯組成物乃定義為基質材料,而在預浸體之說明中,該仍具反應性或具高度反應性聚胺甲酸酯組成物乃藉由根據本發明之方法塗佈至纖維上。
基質乃定義為來自複合材料中交聯之反應性或高度反應性聚胺甲酸酯組成物的基質材料。
本發明之纖維支架係由纖維材料(通常亦稱為強化纖維)所組成。通常任何纖維材料均適當,然而較佳係使用玻璃、碳、塑膠諸如聚醯胺(芳綸)或聚酯、天然纖維或礦物纖維材料諸如玄武岩纖維或陶瓷纖維(以氧化鋁及/
或二氧化矽為基底之氧化物纖維)。纖維型式之混合物,諸如芳綸與玻璃纖維之纖維組合,或碳與玻璃纖維之組合亦可使用。同樣地,混雜複合材料組份可使用得自不同纖維支架的預浸體所製成。
玻璃纖維為最常使用的纖維型式,主要由於其價位較低。此處原則上,所有型式之以玻璃為基底之強化纖維均適當(E玻璃、S玻璃、R玻璃、M玻璃、C玻璃、ECR玻璃、D玻璃、AR玻璃、或空心玻璃纖維)。
碳纖維通常用於高效能複合材料中,因其比起玻璃纖維具較低密度且同時具較高強度為重要因素。碳纖維為工業製造的纖維,其係由含碳之原材料藉裂解反應轉化成石墨狀配置結構之碳而得。其可區分成各向同性及各向異性型式:各向同性纖維僅具有低強度值及較低工業意義,而各向異性纖維則顯現高強度及剛度值且同時具有低斷裂伸長率。
此處,所有得自植物及動物材料(例如木、纖維素、棉、麻、黃麻、亞麻、劍麻或竹纖維)之紡織纖維及纖維材料均稱為天然纖維。
芳綸纖維(亦類似於碳纖維)具有負熱膨脹係數,亦即加熱後變較短。其具體強度及其彈性模數顯著低於碳纖維者。與基質樹脂之正膨脹係數結合,可以製造高度尺寸安定性組份。與碳纖維強化塑膠相比之下,芳綸纖維複合材料之壓力抗性顯著較低。芳綸纖維之己詳知品牌名為Dupont之Nomex®及Kevlar®,或Teijin之Teijinconex®
、Twaron®及Technora®。由玻璃纖維、碳纖維、芳綸纖維或陶瓷纖維所製得之支架特別適當。纖維材料為平面結構體。不織布材料之平面結構體、同樣地所謂的針織物品、諸如編織及針織物、以及非針織束諸如布料、不織布或網布均適當。此外,作為支架之長纖維及短纖維有所區分。根據本發明之亦適當者為粗紗及紗線。所有之上述材料在本發明中均適於作為纖維支架。
強化纖維之概述乃含於“Composites Technologien,Paolo Ermanni(Version 4),Script for Lecture ETH Zürich,August 2007,Chapter 7”中。
原則上,所有反應性聚胺甲酸酯組成物(包括於室溫下具貯存安定性之其他組成物)均適於作為基質材料。根據本發明,適當之聚胺甲酸酯組成物由下列者之混合物所組成:液態樹脂組份b),其具有對NCO基具反應性之官能基且具有低於25℃之Tg或熔點;及暫時去活化(換言之為內部阻斷及/或被阻斷劑所阻斷)之二-或聚異氰酸酯,亦稱作為熟化劑a)(組份a)。樹脂組份b)於室溫下為液態,因此無固態樹脂之特質。樹脂組份b)較佳地於20至23℃下為液態,且較佳地於低於20℃下為液態。
樹脂組份b)之適當官能基為羥基、胺基及硫醇基,其中彼等係與游離異氰酸酯基於加成反應中起反應,因而使聚胺甲酸酯組成物交聯及硬化。以多元醇較佳。樹脂組
份於室溫下必需為液態。其意指樹脂組份必需具有低於25℃之Tg或熔點。樹脂組份b)較佳地於20至23℃下為液態,且特佳地於低於20℃下為液態。
可用作為樹脂組份b)之材料為單體多元醇、聚酯、聚己內酯、聚醚、聚丙烯酸酯、聚碳酸酯及聚胺甲酸酯,其具有50至2000毫克氫氧化鉀/克之OH數及62至3000克/莫耳之平均莫耳質量。
具官能基之樹脂組份b)之量乃予選擇以使得組份b)之每一個官能基中較佳有0.6至2個之NCO當量或0.3至1個組份a)之脲二酮基存在。
較佳係使用具有200至1500毫克氫氧化鉀/克之OH數,特佳具有501至1000毫克氫氧化鉀/克之OH數的多元醇。且極特佳係使用具有600至800毫克氫氧化鉀/克之OH數的多元醇。
較佳之多元醇具有100至1000克/莫耳之平均分子量,特佳具有100至500克/莫耳之平均分子量。
極特佳之多元醇具有501至1000毫克氫氧化鉀/克之OH數,其於20至23℃下為液態,且較佳地於低於20℃下為液態。
甚至更佳之多元醇具有600至800毫克氫氧化鉀/克之OH數,其於20至23℃下為液態,且較佳地於低於20℃下為液態。
當然亦可能使用這些樹脂組份b)之混合物。
適當多元醇之實例為:
當然亦可能使用這些多元醇b)之混合物。
熟化組份a)方面,係使用被阻斷劑所阻斷或內部阻斷(脲二酮)之二-及聚異氰酸酯。
根據本發明所用之二-及聚異氰酸酯可由芳族、脂族、環脂族及/或(環)脂族二-及聚異氰酸酯所組成。
芳族二-及聚異氰酸酯方面,原則上所有已知之芳族化合物均適當,以1,3-及1,4-苯二異氰酸酯、1,5-萘二異氰酸酯、甲苯胺二異氰酸酯、2,6-甲苯二異氰酸酯、2,4-甲苯二異氰酸酯(2,4-TDI)、2,4’-二苯基甲烷二異氰酸酯(2,4’-MDI)、4,4’-二苯基甲烷二異氰酸酯、單體二苯基甲烷二異氰酸酯(MDI)與寡聚二苯基甲烷二異氰酸酯(聚合物MDI)之混合物、苯二亞甲基二異氰酸酯、四甲基苯二亞甲基二異氰酸酯及三異氰酸酯基甲苯特別適當。
適當之脂族二-或聚異氰酸酯有利地於直鏈或支鏈亞烷基殘基中具有3至16個碳原子、較佳4至12個碳原子,且適當之環脂族或(環)脂族二異氰酸酯有利地於環亞烷基殘基中具有4至18個碳原子、較佳6至15個碳原子。熟諳此藝者理解,(環)脂族二異氰酸酯同時意指環或脂族結合之NCO基,諸如二異氰酸異佛爾酮。與此對比之下,環脂族二異氰酸酯當然意指彼些僅具有直接結合至環脂族環上之NCO基者,例如H12MDI。實例為環己烷二異氰酸酯、甲基環己烷二異氰酸酯、乙基環己烷二異氰酸酯、丙基環己烷二異氰酸酯、甲基二乙基環己烷二異氰酸
酯、丙烷二異氰酸酯、丁烷二異氰酸酯、戊烷二異氰酸酯、己烷二異氰酸酯、庚烷二異氰酸酯、辛烷二異氰酸酯、壬烷二異氰酸酯、壬烷三異氰酸酯、諸如4-異氰酸酯基甲基-1,8-辛烷二異氰酸酯(TIN)、癸烷二-及三異氰酸酯、十一烷二-及三異氰酸酯及十二烷二-及三異氰酸酯。
以異氰酸異佛爾酮(IPDI)、六亞甲基二異氰酸酯(HDI)、二異氰酸酯二環己基甲烷(H12MDI)、二異氰酸2-甲基戊烷(MPDI)、2,2,4-三甲基六亞甲基二異氰酸酯/2,4,4-三甲基六亞甲基二異氰酸酯(TMDI)及降冰片烷二異氰酸酯(NBDI)較佳,特佳使用者為IPDI、HDI、TMDI及/或H12MDI,異氰尿酸酯亦可使用。
亦適當者為4-甲基-環己烷1,3-二異氰酸酯、2-丁基-2-乙基五亞甲基二異氰酸酯、3(4)-異氰酸酯基甲基-1-甲基環己基異氰酸酯、2-異氰酸酯基丙基環己基異氰酸酯、2,4'-亞甲基雙(環己基)二異氰酸酯及1,4-二異氰酸酯基-4-甲基-戊烷。
當然亦可能使用二-及聚異氰酸酯之混合物。
此外,較佳地可使用寡-或聚異氰酸酯,其係由上述二-或聚異氰酸酯或其混合物中藉鍵結法經由胺甲酸酯、脲基甲酸酯、脲、縮二脲、脲二酮、醯胺、異氰尿酸酯、碳化二亞胺、脲酮亞胺、噁二嗪三酮或亞胺基噁二嗪二酮結構而製得。以異氰尿酸酯,尤其得自IPDI及/或HDI者,特別適當。
根據本發明所用之聚異氰酸酯被阻斷。可能供其使用
之外部阻斷劑諸如為乙醯乙酸乙酯、二異丙胺、甲乙酮肟、丙二酸二乙酯、ε-己內醯胺、1,2,4-三唑、酚或經取代酚及3,5-二甲基吡唑。
較佳使用之熟化組份為IPDI加合物,其含有異氰尿酸酯基團及ε-己內醯胺阻斷之異氰酸酯結構。
內部阻斷亦可能且此為較佳使用方式。內部阻斷係經由二聚物之形成經由脲二酮結構而完成,其於增溫下再度裂解回原始存在之異氰酸酯結構且因此使交聯作用隨著黏結劑運動。
隨意地,反應性聚胺甲酸酯組成物可含有其他催化劑。這些為有機金屬催化劑,諸如二月桂酸二丁基錫(DBTL)、辛酸鋅、新十二酸鉍、或另為三級胺,較佳為1,4-二氮雜二環[2.2.2]辛烷,量為0.001-1重量%。根據本發明所用之這些反應性聚胺甲酸酯組成物係於正常條件下,例如使用DBTL催化反應,從160℃、通常從約180℃開始及依所示熟化。
供製造反應性聚胺甲酸酯組成物方面,於塗覆粉末技術中常見的添加劑,諸如平整劑,例如聚矽氧烷或丙烯酸酯;光屏蔽劑,例如位阻胺;或其他輔助物質諸如述於EP 669 353中者;可以0.05至5重量%之總量加入。填料及色素諸如二氧化鈦;或染料可以至多可達總組成物50重量%之量加入。
本發明文中,反應性(改良I)意指根據本發明所用之反應性聚胺甲酸酯組成物係如上所述地,從160℃之溫
度開始熟化(其依支架之特性而定)。
根據本發明所用之反應性聚胺甲酸酯組成物係於正常條件下,例如使用DBTL催化反應,從160℃、通常從約180℃開始熟化。根據本發明所用之反應性聚胺甲酸酯組成物之熟化時間通常在5至60分鐘內。
本發明中較佳使用者為基質材料B),來自含有反應性脲二酮基之聚胺甲酸酯組成物B),實質上含有a)至少一種含有脲二酮基之熟化劑,以來自含有脂族、(環)脂族或環脂族脲二酮基之聚異氰酸酯的聚加成化合物以及含羥基之化合物為基底,其中該熟化劑低於40℃時以固體形式存在且高於110℃時以液體形式存在,且具有小於5重量%之游離NCO含量及3-25重量%之脲二酮含量,b)至少一種含羥基之液態樹脂組份b),其具有低於25℃之Tg或熔點以及介於50至2000間之OH數。
c)隨意地至少一種催化劑,d)隨意地聚胺甲酸酯化學中已知之輔助物質及添加劑,以便使兩種組份a)及b)以組份b)之每個羥基中有0.3至1個組份a)之脲二酮基之比率存在,較佳為0.45至0.55。後者相當於0.9至1.1:1之NCO/OH比。
含脲二酮之聚異氰酸酯已詳知且例如述於US 4,476,054、US 4,912,210、US 4,929,724及EP 417 603中
。工業有關之供將異氰酸酯二聚化成脲二酮之方法的綜合概述則由J.Prakt.Chem.336(1994)185-200提供。通常,異氰酸酯轉化成脲二酮係於適當二聚反應催化劑諸如二烷胺基吡啶、三烷膦、磷酸三醯胺或咪唑之存在下完成。該反應(隨意地於溶劑中進行,但較佳於溶劑缺乏下進行)係於達到期望轉化程度後藉加入催化劑毒物而停止。然後將過量之單體異氰酸酯藉急驟蒸發法移除。如果催化劑具足夠揮發性,則反應混合物可在單體分離過程中揮發地移除催化劑。催化劑毒藥的添加在此狀況下可以省略。實質上,廣泛之異氰酸酯適用於製造含有脲二酮基之聚異氰酸酯。上述二-及聚異氰酸酯可予使用。然而,以來自任何脂族、環脂族及/或(環)脂族二-及/或聚異氰酸酯之二-及聚異氰酸酯較佳。根據本發明,使用的為異氰酸異佛爾酮(IPDI)、六亞甲基二異氰酸酯(HDI)、二異氰酸酯二環己基甲烷(H12MDI)、二異氰酸2-甲基戊烷(MPDI)、2,2,4-三甲基六亞甲基二異氰酸酯/2,4,4-三甲基六亞甲基二異氰酸酯(TMDI)或降冰片烷二異氰酸酯(NBDI)。相當特佳者為單獨或以混合物形式使用之IPDI、HDI、TMDI及H12MDI,異氰尿酸酯亦可使用。
相當特佳地,IPDI及/或HDI乃用於供基質材料用。將這些含脲二酮基之聚異氰酸酯轉化成含脲二酮基之熟化劑a)之作用包含令游離NCO基與作為鏈增長劑之含羥基的單體或聚合物,諸如聚酯、聚硫醚、聚醚、聚己內醯胺、聚環氧化物、聚酯醯胺、聚胺甲酸酯或低分子量二、
三-及/或四元醇,及隨意之作為鏈終止劑之單胺及/或單元醇起反應,且己經常被述及(EP 669 353、EP 669 354、DE 30 30 572、EP 639 598或EP 803 524)。
較佳之具有脲二酮基的熟化劑a)具有小於5重量%之游離NCO含量及3至25重量%、較佳6至18重量%之脲二酮基含量(以C2N2O2計算,分子量84)。以聚酯及單體二元醇較佳。除了脲二酮基之外,熟化劑亦可顯現異氰尿酸酯、縮二脲、脲基甲酸酯、胺甲酸酯及/或脲之結構。
至於在含羥基之液態樹脂組份b)方面,較佳係使用單體多元醇、聚酯、聚己內酯、聚醚、聚丙烯酸酯、聚碳酸酯及聚胺甲酸酯,其具有50至2000毫克氫氧化鉀/克之OH數及62至3000克/莫耳之平均莫耳質量,且這些具有低於25℃之Tg或熔點。
較佳係使用具有200至1500毫克氫氧化鉀/克之OH數,特佳具有501至1000毫克氫氧化鉀/克之OH數的多元醇。極特佳係使用具有600至800毫克氫氧化鉀/克之OH數的多元醇。
較佳之多元醇具有100至1000克/莫耳之平均分子量,特佳具有100至500克/莫耳之平均分子量。
極特佳之多元醇具有501至1000毫克氫氧化鉀/克之OH數,其於20至23℃下為液態,且較佳地於低於20℃下為液態。甚至更佳之多元醇具有600至800毫克氫氧化鉀/克之OH數,其於20至23℃下為液態,且較佳地於低
於20℃下為液態。
當然,亦可能使用這些樹脂組份之混合物。含羥基之樹脂組份b)的使用量乃予選擇以便使組份b)之每個羥基中有0.3至1個組份a)之脲二酮基存在,較佳為0.45至0.55。
隨意地,額外催化劑c)亦可含於根據本發明之反應性聚胺甲酸酯B)中。這些為有機金屬催化劑,諸如二月桂酸二丁基錫、辛酸鋅、新十二酸鉍、或另為三級胺,諸如1,4-二氮雜二環[2.2.2]辛烷,量為0.001-1重量%。根據本發明所用之這些反應性聚胺甲酸酯組成物係於正常條件下,例如使用DBTL催化反應,從160℃、通常從約180℃開始熟化,且稱之為改良I。
供製造反應性聚胺甲酸酯組成物方面,於漆、黏著劑及密封劑技術中常見的添加劑d),諸如平整劑,例如聚矽氧烷或丙烯酸酯;光屏蔽劑,例如位阻胺;或其他添加劑諸如述於EP 669 353中者;可以0.05至5重量%之總量加入。填料及色素諸如二氧化鈦可以至多可達總組成物30重量%之量加入。
根據本發明所用之反應性聚胺甲酸酯組成物係於正常條件下,例如使用DBTL催化反應,從160℃、通常從約180℃開始熟化。根據本發明所用之反應性聚胺甲酸酯組成物可提供極良好之流動且因此提供良好之浸漬性能及於熟化狀態中優良之化學品抗性。此外,隨著脂族交聯劑(例如IPDI或H12MDI)之使用,亦可得到良好之耐天氣性
。
特佳地,本發明使用之基質材料係由B)至少一種含高度反應性脲二酮基之聚胺甲酸酯組成物所組成,實質上含有a)至少一種含有脲二酮基之熟化劑,及b)隨意地至少一種液態樹脂組份b),其具有低於25℃之Tg或熔點以及介於50至2000毫克氫氧化鉀/克間之OH數,且具有對NCO基團具反應性之官能基;c)0.1至5重量%之至少一種催化劑,其選自具有鹵素、氫氧化物、醇化物或有機或無機酸陰離子作為抗衡離子之四級銨鹽及/或四級鏻鹽;及d)0.1至5重量%之至少一種輔催化劑,其選自d1)至少一種環氧化物及/或d2)至少一種金屬乙醯丙酮酸鹽及/或乙醯丙酮酸四級銨及/或乙醯丙酮酸四級鏻;e)隨意地於聚胺甲酸酯化學中已知之輔助物質及添加劑。
相當特佳地,基質材料B)係由B)至少一種作為基質材料之含脲二酮基之高度反應性聚胺甲酸酯組成物所組成,實質上含有
a)至少一種含有脲二酮基之熟化劑,以來自含有脲二酮基之脂族、(環)脂族或環脂族聚異氰酸酯的聚加成化合物以及含羥基之化合物為基底,其中該熟化劑低於40℃時以固體形式存在且高於110℃時以液體形式存在,且具有小於5重量%之游離NCO含量及3-25重量%之脲二酮含量,b)至少一種液態多元醇,其具有低於25℃之Tg或熔點以及介於50至2000毫克氫氧化鉀/克間之OH數。
c)0.1至5重量%之至少一種催化劑,其選自具有鹵素、氫氧化物、醇化物或有機或無機酸陰離子作為抗衡離子之四級銨鹽及/或四級鏻鹽;及d)0.1至5重量%之至少一種輔催化劑,其選自d1)至少一種環氧化物及/或d2)至少一種金屬乙醯丙酮酸鹽及/或乙醯丙酮酸四級銨及/或乙醯丙酮酸四級鏻;e)隨意地於聚胺甲酸酯化學中已知之輔助物質及添加劑,以便使兩種組份a)及b)以組份b)之每個羥基中有0.3至1個組份a)之脲二酮基之比率存在,較佳為0.6至0.9。後者相當於0.6至2:1之NCO/OH比且較佳1.2至1.8:1。根據本發明所用之這些高度反應性聚胺甲酸酯組
成物係於100至160℃下熟化且稱之為改良II。
適當之根據本發明之含高度反應性脲二酮基的聚胺甲酸酯組成物含有下列者之混合物:暫時去活化,亦即含脲二酮基(內部阻斷)之二-或聚胺甲酸酯,亦稱為熟化劑a)及根據本發明所含之催化劑c)及d),以及此外,隨意地,具有官能基(對NCO基具反應性)且具有低於25℃之Tg或熔點及具有50至2000毫克氫氧化鉀/克之OH數的液態樹脂組份,亦稱為樹脂b)。催化劑可確保含脲二酮基之聚胺甲酸酯組成物於低溫下熟化。故該含脲二酮基之聚胺甲酸酯組成物具高度反應性。
如上所述之材料係用作為含脲二酮基之熟化組份a)。
可用作為液態樹脂組份b)之材料為單體多元醇、聚酯、聚己內酯、聚醚、聚丙烯酸酯、聚碳酸酯及聚胺甲酸酯,其具有50至2000毫克氫氧化鉀/克之OH數及62至3000克/莫耳之平均莫耳質量。
較佳係使用具有200至1500毫克氫氧化鉀/克之OH數,特佳具有501至1000毫克氫氧化鉀/克之OH數的多元醇。較佳之多元醇具有100至1000克/莫耳之平均分子量,特佳具有100至500克/莫耳之平均分子量。
極特佳之多元醇具有501至1000毫克氫氧化鉀/克之OH數,其於20至23℃下為液態,且較佳地於低於20℃下為液態。
催化劑c)方面,較佳係使用具有鹵素、氫氧化物、
醇化物或有機或無機酸陰離子作為抗衡離子之四級銨鹽及/或四級鏻鹽。這些之實例為:甲酸四甲基銨、乙酸四甲基銨、丙酸四甲基銨、丁酸四甲基銨、苯甲酸四甲基銨、甲酸四乙基銨、乙酸四乙基銨、丙酸四乙基銨、丁酸四乙基銨、苯甲酸四乙基銨、甲酸四丙基銨、乙酸四丙基銨、丙酸四丙基銨、丁酸四丙基銨、苯甲酸四丙基銨、甲酸四丁基銨、乙酸四丁基銨、丙酸四丁基銨、丁酸四丁基銨及苯甲酸四甲基銨及乙酸四丁基鏻、甲酸四丁基鏻及乙酸乙基三苯基鏻、苯並三唑四丁基鏻、酚四苯基鏻及癸酸三己基十四烷基鏻、氫氧化甲基三丁基銨、氫氧化甲基三乙基銨、氫氧化四甲基銨、氫氧化四乙基銨、氫氧化四丙基銨、氫氧化四丁基銨、氫氧化四戊基銨、氫氧化四己基銨、氫氧化四辛基銨、氫氧化四癸基銨、氫氧化十四烷基三己基銨、氫氧化四(十八烷基)銨、氫氧化苄基三甲基銨、氫氧化苄基三乙基銨、氫氧化三甲基苯基銨、氫氧化三乙基甲基銨、氫氧化三甲基乙烯基銨、甲醇甲基三丁基銨、甲醇甲基三乙基銨、甲醇四甲基銨、甲醇四乙基銨、甲醇四丙基銨、甲醇四丁基銨、甲醇四戊基銨、甲醇四己基銨、甲醇四辛基銨、甲醇四癸基銨、甲醇十四烷基三已基銨、甲醇四(十八烷基)銨、甲醇苄基三甲基銨、甲醇苄基三乙基銨、甲醇三甲基苯基銨、甲醇三乙基甲基銨、甲醇三甲基乙烯基銨、乙醇甲基三丁基銨、乙醇甲基三乙基銨、乙醇四甲基銨、乙醇四乙基銨、乙醇四丙基銨、乙醇四丁基銨、乙醇四戊基銨、乙醇四己基銨、乙醇四辛基銨、
乙醇四癸基銨、乙醇十四烷基三己基銨、乙醇四(十八烷基)銨、乙醇苄基三甲基銨、乙醇苄基三乙基銨、乙醇三甲基苯基銨、乙醇三乙基甲基銨、乙醇三甲基乙烯基銨、苄化甲基三丁基銨、苄化甲基三乙基銨、苄化四甲基銨、苄化四乙基銨、苄化四丙基銨、苄化四丁基銨、苄化四戊基銨、苄化四己基銨、苄化四辛基銨、苄化四癸基銨、苄化十四烷基三已基銨、苄化四(十八烷基)銨、苄化苄基三甲基銨、苄化苄基三乙基銨、苄化三甲基苯基銨、苄化三乙基甲基銨、苄化三甲基乙烯基銨、氟化四甲基銨、氟化四乙基銨、氟化四丁基銨、氟化四辛基銨、氟化苄基三甲基銨、氫氧化四丁基鏻、氟化四丁基鏻、氯化四丁基銨、溴化四丁基銨、碘化四丁基銨、氯化四乙基銨、溴化四乙基銨、碘化四乙基銨、氯化四甲基銨、溴化四甲基銨、碘化四甲基銨、氯化苄基三甲基銨、氯化苄基三乙基銨、氯化苄基三丙基銨、氯化苄基三丁基銨、氯化甲基三丁基銨、氯化甲基三丙基銨、氯化甲基三乙基銨、氯化甲基三苯基銨、氯化苯基三甲基銨、溴化苄基三甲基銨、溴化苄基三乙基銨、溴化苄基三丙基銨、溴化苄基三丁基銨、溴化甲基三丁基銨、溴化甲基三丙基銨、溴化甲基三乙基銨、溴化甲基三苯基銨、溴化苯基三甲基銨、碘化苄基三甲基銨、碘化苄基三乙基銨、碘化苄基三丙基銨、碘化苄基三丁基銨、碘化甲基三丁基銨、碘化甲基三丙基銨、碘化甲基三乙基銨、碘化甲基三苯基銨及碘化苯基三甲基銨、氫氧化甲基三丁基銨、氫氧化甲基三乙基銨、氫氧化四甲
基銨、氫氧化四乙基銨、氫氧化四丙基銨、氫氧化四丁基銨、氫氧化四戊基銨、氫氧化四己基銨、氫氧化四辛基銨、氫氧化四癸基銨、氫氧化十四烷基三己基銨、氫氧化四(十八烷基)銨、氫氧化苄基三甲基銨、氫氧化苄基三乙基銨、氫氧化三甲基苯基銨、氫氧化三乙基甲基銨、氫氧化三甲基乙烯基銨、氟化四甲基銨、氟化四乙基銨、氟化四丁基銨、氟化四辛基銨及氟化苄基三甲基銨。這些催化劑可單獨地或以任何期望之混合物形式存在。較佳係使用苯甲酸四乙基銨及/或氫氧化四丁基銨。
以基質材料之全體調合物為基準,催化劑c)的含量可為0.1至5重量%,較佳為0.3至2重量%。
根據本發明之一改良,改良亦包括將此催化劑c)結合至聚合物b)之官能基上。此外,這些催化劑可被惰性殼所環繞,故可封入膠囊內。
當使用輔催化劑d1)環氧化物時。此處可能之實例為縮水甘油醚、縮水甘油酯、脂族環氧化物、以雙酚A為基底之二縮水甘油醚、及/或甲基丙烯酸縮水甘油酯。此環氧化物之實例為異氰尿酸三縮水甘油酯(TGIC,商標名ARALDIT 810,Huntsman)、對苯二甲酸二縮水甘油酯與偏苯三甲酸三縮水甘油酯之混合物(商標名ARALDIT PT 910及912,Huntsman)、叔碳酸縮水甘油酯(商標名KARDURA E10,Shell)、3’,4’-環氧基環己烷羧酸3,4-環氧基環己基甲酯(ECC)、以雙酚A為基底之二縮水甘油醚(商標名EPIKOTE 828,Shell)、乙基己基縮水甘油醚
、丁基縮水甘油醚、異戊四醇四縮水甘油醚,(商標名POLYPOX R 16,UPPC AG)及其他含游離環氧基之Polypox型式。混合物亦可使用。較佳係使用對苯二甲酸二縮水甘油酯與偏苯三甲酸三縮水甘油酯之混合物(商標名ARALDIT PT 910及/或912)。
當輔催化劑d2)金屬乙醯丙酮酸鹽可行時。其實例為乙醯丙酮酸鋅、乙醯丙酮酸鋰及乙醯丙酮酸錫,以單獨或混合物形式使用。較佳係使用乙醯丙酮酸鋅。
輔催化劑d2)方面,乙醯丙酮酸四級銨或乙醯丙酮酸四級鏻亦可行。
此催化劑之實例為乙醯丙酮酸四甲基銨、乙醯丙酮酸四乙基銨、乙醯丙酮酸四丙基銨、乙醯丙酮酸四丁基銨、乙醯丙酮酸苄基三甲基銨、乙醯丙酮酸苄基三乙基銨、乙醯丙酮酸四甲基鏻、乙醯丙酮酸四乙基鏻、乙醯丙酮酸四丙基鏻、乙醯丙酮酸四丁基鏻、乙醯丙酮酸苄基三甲基鏻、乙醯丙酮酸苄基三乙基鏻。特佳係使用乙醯丙酮酸四乙基銨及/或乙醯丙酮酸四丁基銨。此催化劑之混合物當然亦可使用。
以基質材料之全體調合物為基準,輔催化劑d1)及/或d2)之含量可為0.1至5重量%,較佳為0.3至2重量%。
藉由根據本發明使用之高反應性且因而低溫熟化之聚胺甲酸酯組成物B),於100至160℃之熟化溫度不僅可節省能源及熟化時間,亦可使用許多溫度敏感性支架。
本發明文中,高度反應性(改良II)意指根據本發明之含脲二酮基之聚胺甲酸酯組成物係依支架之特性而於100至160℃下熟化。此熟化溫度較佳為120至150℃,特佳為130至140℃。根據本發明所用之聚胺甲酸酯組成物之熟化時間通常在1至60分鐘內。
根據本發明所用之反應性或高度反應性聚胺甲酸酯組成物可提供極良好之流動且因此提供良好之浸漬性能及於熟化狀態中優良之化學品抗性。此外,隨著脂族交聯劑(例如IPDI或H12MDI)之使用,亦可得到良好之耐天氣性。
根據本發明之預浸體,以及複合材料組份,乃具有大於10%,較佳50至70%,特佳50至65%之纖維體積含量。
基質材料B)可為高黏度材料,或為液體或固體。基質材料B)通常具有至少30℃之Tg或熔點。
根據本發明所用之反應性或高度反應性聚胺甲酸酯組成物實質上係由反應性樹脂與熟化劑之混合物所組成。如為反應性聚胺甲酸酯組成物,此混合物通常僅於超過160℃之溫度反應,或者如為高度反應性聚胺甲酸酯組成物,則於超過100℃之溫度反應,以得交聯性聚胺甲酸酯且因而形成複合材料之基質。此意指根據本發明之預浸體在其製造之後係由支架及所塗佈之作為基質材料的反應性聚胺甲酸酯組成物(其以未交聯但具反應性之形式存在)所組成。
故該預浸體具貯存安定性,通常為數天且甚至數星期及數月,因此可於任何時間進一步進行製程以得複合材料。此乃實質不同於己上述之2-組份系統(此2-組份系統具反應性但不具貯存安定性,從塗佈後這些立即開始反應及交聯以得聚胺甲酸酯)。
本發明之主題亦為一種製造預浸體的方法,該預浸體實質上由下列者所組成A)至少一種纖維支架及B)至少一種作為基質材料之反應性聚胺甲酸酯組成物,其中該聚胺甲酸酯組成物實質上含有下列者之混合物:液態樹脂組份b),其具有對異氰酸酯具反應性之官能基且具有低於25℃之Tg或熔點,且具有介於50至2000毫克氫氧化鉀/克間之OH數;及作為熟化劑a)之內部阻斷及/或被阻斷劑所阻斷之二-或聚異氰酸酯,該方法為I.藉製造反應性聚胺甲酸酯組成物B),及II.將纖維支架A)以聚胺甲酸酯組成物B)(其已隨意地溶於溶劑中)浸漬,III.再隨意地將溶劑移除。
基質材料B)可為高黏度材料,或為液體或固體。基質材料B)通常具有至少30℃之Tg或熔點。
預浸體之製造方法的原理為,首先反應性聚胺甲酸酯組成物B)係由其個別之組份中製得(隨意地於適當之共用溶劑中)。然後將反應性聚胺甲酸酯組成物B)與隨意溶劑之此組合塗佈至纖維支架A)上,較佳地於製得反應性聚胺甲酸酯組成物B)後直接塗佈,且將纖維支架浸漬。然後將該隨意溶劑隨意地移除。較佳地係將溶劑於低溫下,較佳<160℃下,特佳<100℃下,藉(例如)加熱處理或施予真空而完全移除。
然後將可貯存之預浸體於接續時刻進行進一步製程以得複合材料。根據本發明之方法可使纖維支架得到極良好之浸漬,此乃因液態樹脂組份b)可使反應性聚胺甲酸酯組成物得到極良好之支架纖維之濕化。當使用液態樹脂組份b)時,亦可明顯更輕易地移除所用之溶劑。再接續之壓擠以得複合材料期間,液態樹脂組份導致層內之較佳流動,因此得到優良性質的材料。
供製造預浸體之聚胺甲酸酯組成物B)之製造可於適當組裝中,例如於可加熱攪拌槽、捏合機、或另於擠壓機中進行,但此處不應超過100℃之上限溫度。
可供本發明方法使用之適當溶劑為任何不與反應聚胺甲酸酯組成物起反應之質子惰性溶劑,其具有足夠能力以令反應性聚胺甲酸酯組成物中所用之個別組份溶解,及供在製程之溶劑移除步驟中可被撤除之目的(惟微量(小於
0.5重量%)之來自被反應性聚胺甲酸酯組成物浸漬之預浸體者除外),且此處有利地可將移除之溶劑再循環。此處可提及之實例為:酮類(丙酮、甲基乙基酮、甲基異丁基酮、環己酮),醚類(四氫呋喃),酯類(乙酸正丙酯、乙酸正丁酯、乙酸異丁酯、1,2-碳酸丙烯酯、丙二醇甲基醚乙酸酯)。
藉上述浸漬法(隨意地與溶劑)之預浸體之製造原則上可根據本發明,藉任何期望方法及經由已知機器設備及儀器進行。
溶液浸漬法尤其用於供製造環氧基複合材料[“Composites Technologien(Technologies of composites),Paolo Ermanni(Version 4),script for paper to be given at ETH Zürich,August 2007,Chapter 4.2.2”]。然而,彼發表並未述及於溶液中之反應性聚胺甲酸酯組成物。
纖維之浸漬亦可另於無溶劑之情況下以直接熔融法進行。
本發明之主題為一種製造預浸體之直接熔融浸漬方法,該預浸體實質上由下列者所組成A)至少一種纖維支架及B)至少一種作為基質材料之反應性聚胺甲酸酯組成物,其中該聚胺甲酸酯組成物實質上含有下列者之混
合物:液態樹脂組份b),其具有對異氰酸酯具反應性之官能基且具有低於25℃之Tg或熔點,且具有介於50至2000毫克氫氧化鉀/克間之OH數;及作為熟化劑a)之內部阻斷及/或被阻斷劑所阻斷之二-或聚異氰酸酯該方法為I.藉製造反應性聚胺甲酸酯組成物B)於熔融物中,及II.將纖維支架A)直接以B)之熔融物浸漬。
預浸體之直接熔融浸漬法包含首先由個別組份中製得反應性聚胺甲酸酯組成物B)。然後將此反應性聚胺甲酸酯組成物B)之熔融物直接塗佈至纖維支架A)上,亦即將纖維支架A)以B)之熔融物浸漬。然後將已冷卻可貯存之預浸體於接續時刻進行進一步製程以得複合材料。根據本發明之直接熔融浸漬法可得到極良好之纖維支架之浸漬,此乃因低黏度液態反應性聚胺甲酸酯組成物在此可將支架極之纖維極有效地濕化,而先前之熔融物均化作用在此可避免聚胺甲酸酯組成物之熱應力而可導致交聯反應開始,再者如今並無供碾磨及篩選出個別粒徑級之製程步驟,因此所浸漬纖維支架所得之產率較高。
傳統熔融浸漬法中或粉末形式反應性聚胺甲酸酯組成物之起始燒結中所需之至少短時間之高溫在根據本發明之方法中則無需到此程度,因為液態樹脂組份導致熔融物黏
度之顯著降低。僅有在浸漬法後移除隨意所用溶劑期間會發生反應性聚胺甲酸酯組成物之熱應力,此處溫度不應超過80至100℃,以避免或使反應基質材料之起始反應降至最小。
如有需要,可將預浸體組合成各種形狀並切割。
供預浸體之固結以得單一複合材料及供基質材料之交聯以得基質方面,乃將預浸體切割,隨意地縫在一起或以任何其他方式固定,再於適當模具中、於壓力下及隨意地施予真空予以壓擠。供本發明之目的方面,此由預浸體中製造複合材料之步驟係於依硬化時間所決定之溫度下進行,當使用反應性基質材料(變體I)時,溫度超過約160℃,當使用備有適當催化劑之高度反應性基質材料(變體II)時,則溫度超過100℃。
本發明之主題亦為於複合材料表面上具有固定箔C)之預浸體。
可予使用之(多層)箔為以衍生自由熱塑性聚胺甲酸酯(TPU)、熱塑性聚烯烴(TPO)、(甲基)丙烯酸聚合物、聚碳酸酯箔(例如得自Sabic Innovative Plastics之Lexan SLX)、聚醯胺、聚醚酯醯胺、聚醚醯胺、或聚二氟乙烯(例如得自SOLIANT之SOLIANT FLUOREX,AkzoNobel,或得自Avery之AVLOY)或金屬化或金屬箔例如鋁、銅或其他材料所製之熱塑性塑料或混合物或(分別地)化合材料為基底之層壓箔,其中黏合至含脲二酮基之仍具反應性或高度反應性之基質系統上之作用係於預浸
體製造完成之前進行。而且,箔之進一步固定亦於預浸體之進一步製程以得複合材料之硬化聚胺甲酸酯層壓表面期間進行。以熱塑性材料為基底之層壓箔可以色素及/或染料進行箔之主體著色或另為印花箔或為於外表上漆之箔。
層壓箔具有0.2至10毫米間之厚度,較佳介於0.5至4毫米間。供貯存安定性高高度反應性聚胺甲酸酯用之軟化點介於80至260℃間,較佳介於110至180℃間,特佳介於130至180℃間,供反應性聚胺甲酸酯用之軟化點介於130至220℃間,且特佳介於160至220℃間。
適當箔之實例亦述於WO 2004/067246中。
根據本發明,層壓箔於預浸體上之固定係於預浸體之製造期間直接進行。此處箔之固定係經由經過基質進行黏著(經由圖1之實例所述),藉將預浸體就地於預浸體乾燥溫度(亞交聯溫度,意指此溫度低於基質材料交聯開始之溫度)下層壓而達成。該固定通常於50至110℃之溫度下進行。
另一種將層壓箔固定於預浸體上之方法係先於第一步驟製得預浸體,再於第二步驟將箔塗佈並固定至已稍後分別製得之預浸體上。此處箔之固定係藉經由基質黏著,藉將預浸體於乾燥溫度(亞交聯溫度)下層壓而達成。該固定通常於50至110℃之溫度下進行。
所製得之備有層壓箔之貯存安定性預浸體亦可與其他預浸體(未層壓)經由適當方法例如壓熱法或壓模法進行製程以得層壓物或,分別地,三明治組份。
層壓箔之另一用途為由以反應性或高度反應性聚胺甲酸酯組成物B)為基底(且其具有與製造根據本發明貯存安定性預浸體相同或使用類似之調合物)之材料所製之裝飾性塗覆層或箔之分別製造。
根據本發明預浸體之另一方面(及本發明實施例)係經由顯著增加之基質:纖維比而顯現特殊之表面品質。因此其具有極小之纖維體積含量。此實施例中供特別平滑及/或彩色複合材料表面所設定之纖維體積含量<50%,較佳<40%,特佳<35%。
根據本發明之層壓預浸體或雙層預浸體之製造可經由已知之機器設備及裝備藉反應注射成形法(RIM)、強化反應注射成形法(RRIM)、或拉擠法,藉將溶液施至輥軋機中或經由熱刮刀,或其他方法進行。
本發明之主題亦為預浸體,尤其是含玻璃、碳或芳綸纖維之纖維支架的預浸體之用途。
本發明之主題亦為使用根據本發明之預浸體於製造於船及造船業、於航太技術、於汽車製造、及於腳踏車、較佳為摩托車及自行車,及於汽車部門、運輸、營建、醫學工程、運動、電力及電子工業、及發電廠中之複合材料(例如製造風力發電廠中之轉動葉片)的用途。
本發明之主題亦為藉根據本發明之方法製得之預浸體。
本發明之主題亦為由根據本發明之預浸體製成之複合材料。
以下,本發明藉由實例說明。
所用之玻璃纖維不織布/布料:下列之玻璃纖維不織布/布料係用於實例中:玻璃長纖布,296克/平方公尺-Atlas,Finish FK 144(Interglas 92626)
含脲二酮之熟化劑H之製造:令119.1克IPDI脲二酮(Evonik Degussa GmbH)溶於100毫升乙酸丁酯中,再將27.5克甲基戊二醇及3.5克三甲醇基丙烷與其混合。將0.01克二月桂酸二丁錫加入後,將混合物加熱至80℃ 4小時,同時攪拌。然後藉滴定法測得無殘留之游離NCO基可檢出。熟化劑H具有12.8重量%之有效潛NCO含量(以固狀物為基準)。
反應性聚胺甲酸酯組成物係用於製造預浸體及複合材料。
將表中之原材料於預先混合器中密切混合,然後溶於已述之溶劑中。
欲製造預浸體,乃將玻璃纖維布料以基質材料溶液浸漬。將預浸體於烘箱中、於50至70℃之溫度下、且施予真空予以乾燥成恆定重量。經測得之纖維質量含量於比較實例1中為49%(10次測試)。發明實例2中為55%(10次測試),發明實例3中為48%(10次測試)且發明實例4中為52%(10次測試)。
比較實例1之預浸體在移除溶劑期間顯現嚴重之起泡現象,可能因為高黏度之故,而由此得到極不規則之表面。因此此預浸體不能進行進一步之製程。
相比之下,根據本發明之發明實例2的預浸體在移除
溶劑後得到無起泡現象之一致性表面。此預浸體可成功地進行進一步之製程。根據本發明之發明實例3的預浸體在移除溶劑後得到含少許起泡現象之一致性表面。雖然不像發明實例2那麼成功,但此預浸體仍可成功地進行進一步之製程。根據本發明之發明實例4的預浸體在移除溶劑後得到無起泡現象之一致性表面。此預浸體可成功地進行進一步之製程。
DSC試驗(玻璃轉化溫度測定及反應測量之焓)係根據DIN 53765標準,使用Mettler Toledo DSC 821e進行。
實例1及2預浸體之DSC研究得到下列之結果:
於第二次加熱步驟中所測量之玻璃轉化溫度為完全交聯/反應之基質材料的玻璃轉化溫度。
實例1、2、3及4預浸體於貯存之前及之後的DSC
研究可見於表1中。根據本發明之發明實例2、3及4預浸體所測量之反應焓在貯存期間並不會顯著降低,此為該基質材料具貯存安定性的證據。
複合材料組份係於複合材料壓機上藉熟諳此藝者已知之壓縮技術製得。將藉由浸漬法所製得之均質預浸體於台面式壓機上壓縮成複合材料。此台面式壓機為Schwabenthan公司之Polystat 200T,經由此壓機將預浸體於120至200℃間壓縮成相對應之複合材料板。壓力在正常壓力與450巴之間變化。
發明實例2及3中,壓機之溫度設定在150℃且在壓擠過程期間增至180℃,而壓力則在3分鐘之短暫熔融相之後增至5巴,再保持此壓力直至最高達30分鐘之後由壓機中移除複合材料組份為止。然後測試此硬性、剛性、化學品抗性及衝擊抗性複合材料組份(板狀產物)之熟化程度(藉DSC測定)。隨著聚胺甲酸酯組成物之使用,交聯作用於約20分鐘後完成,其後亦無殘留之交聯反應之反應焓可檢出。
發明實例4中(催化版),壓機之溫度設定在150℃且在壓擠過程期間增至180℃,而壓力則在3分鐘之短暫熔融相之後增至5巴,再保持此壓力直至最高達10分鐘之後由壓機中移除複合材料組份為止。然後測試此硬性、剛性、化學品抗性及衝擊抗性複合材料組份(板狀產物)
之熟化程度(藉DSC測定)。隨著聚胺甲酸酯組成物之使用,交聯作用於約20分鐘後完成,其後亦無殘留之交聯反應之反應焓可檢出。
起泡現象阻礙了比較實例1預浸體(其非根據本發明)之壓擠。
Claims (30)
- 一種預浸體,實質上由下列者所組成A)至少一種纖維支架及B)至少一種作為基質材料之反應性聚胺甲酸酯組成物,其中該聚胺甲酸酯組成物實質上含有下列者之混合物:液態樹脂組份b),其具有對異氰酸酯具反應性之官能基且具有低於25℃之Tg或熔點,且具有50至2000毫克氫氧化鉀/克之OH數,及作為熟化劑a)之內部阻斷及/或被阻斷劑所阻斷之二-或聚異氰酸酯。
- 根據申請專利範圍第1項之預浸體,其中該基質材料B)為高黏度材料或為液體或固體。
- 根據申請專利範圍第1項之預浸體,其中該基質材料具有至少30℃之Tg。
- 根據申請專利範圍第1項之預浸體,其中含有玻璃、碳、塑膠諸如聚醯胺(芳綸)或聚酯、天然纖維或礦物纖維材料諸如玄武岩纖維或陶瓷纖維之纖維材料。
- 根據申請專利範圍第1項之預浸體, 其中包含作為纖維支架之不織布材料之平面結構體、針織物品、諸如編織及針織物、非針織束諸如布料、不織布或網布、其呈現為長纖維及短纖維材料。
- 根據申請專利範圍第1項之預浸體,其中存在二-或聚異氰酸酯,其選自二異氰酸異佛爾酮(IPDI)、六亞甲基二異氰酸酯(HDI)、二異氰酸酯二環己基甲烷(H12MDI)、二異氰酸2-甲基戊烷(MPDI)、2,2,4-三甲基六亞甲基二異氰酸酯/2,4,4-三甲基六亞甲基二異氰酸酯(TMDI)及/或降冰片烷二異氰酸酯(NBDI)、特佳為IPDI、HDI、TMDI及/或H12MDI,其中該異氰酸酯亦可用。
- 根據申請專利範圍第1項之預浸體,其中存在外部阻斷劑,其選自乙醯乙酸乙酯、二異丙胺、甲乙酮肟、丙二酸二乙酯、ε-己內醯胺、1,2,4-三唑、酚或經取代酚及/或3,5-二甲基吡唑。
- 根據申請專利範圍第1項之預浸體,其中存在IPDI加合物,其含有異氰尿酸酯基團及ε-己內醯胺阻斷之異氰酸酯結構。
- 根據申請專利範圍第1項之預浸體,其中 反應性聚胺甲酸酯組成物B)含有0.001至1重量%之量的額外催化劑,較佳為二月桂酸二丁基錫、辛酸鋅、新十二酸鉍、及/或三級胺,較佳為1,4-二氮雜二環[2.2.2]辛烷。
- 根據申請專利範圍第1項之預浸體,其具有具至少一種反應性聚胺甲酸酯組成物B)(含脲二酮基)之基質材料,實質上含有a)至少一種含有脲二酮基之熟化劑,以來自含有脲二酮基之脂族、(環)脂族或環脂族聚異氰酸酯的聚加成化合物以及含羥基之化合物為基底,其中該熟化劑低於40℃時以固體形式存在且高於110℃時以液體形式存在,且具有小於5重量%之游離NCO含量及3-25重量%之脲二酮含量,b)至少一種含羥基之液態樹脂組份b),其具有低於25℃之Tg或熔點以及介於50至2000毫克氫氧化鉀/克間之OH數,c)隨意地至少一種催化劑,d)隨意地聚胺甲酸酯化學中已知之輔助物質及添加劑,以便使兩種組份a)及b)以組份b)之每個羥基中有0.3至1個組份a)之脲二酮基之比率存在,較佳為0.45至0.55。
- 根據申請專利範圍第1項之預浸體,其具有至少一種作為基質材料之含高度反應性脲二酮基之聚胺甲酸酯組成物B),實質上含有 a)至少一種含有脲二酮基之熟化劑,及b)隨意地至少一種液態樹脂組份b),其具有低於25℃之Tg或熔點以及介於50至2000毫克氫氧化鉀/克間之OH數,且具有對NCO基團具反應性之官能基;c)0.1至5重量%之至少一種催化劑,其選自具有鹵素、氫氧化物、醇化物或有機或無機酸陰離子作為抗衡離子之四級銨鹽及/或四級鏻鹽;及d)0.1至5重量%之至少一種輔催化劑,其選自d1)至少一種環氧化物及/或d2)至少一種金屬乙醯丙酮酸鹽及/或乙醯丙酮酸四級銨及/或乙醯丙酮酸四級鏻;e)隨意地於聚胺甲酸酯化學中已知之輔助物質及添加劑。
- 根據前述申請專利範圍第1至6項或11項中至少一項之預浸體,其具有至少一種作為基質材料之含脲二酮基之高度反應性聚胺甲酸酯組成物B),實質上含有a)至少一種含有脲二酮基之熟化劑,以來自含有脲二酮基之脂族、(環)脂族或環脂族聚異氰酸酯的聚加成化合物以及含羥基之化合物為基底,其中該熟化劑低於40℃時以固體形式存在且高於 110℃時以液體形式存在,且具有小於5重量%之游離NCO含量及3-25重量%之脲二酮含量,b)至少一種液態多元醇,其具有低於25℃之Tg或熔點以及介於50至2000毫克氫氧化鉀/克間之OH數,c)0.1至5重量%之至少一種催化劑,其選自具有鹵素、氫氧化物、醇化物或有機或無機酸陰離子作為抗衡離子之四級銨鹽及/或四級鏻鹽;及d)0.1至5重量%之至少一種輔催化劑,其選自d1)至少一種環氧化物及/或d2)至少一種金屬乙醯丙酮酸鹽及/或乙醯丙酮酸四級銨及/或乙醯丙酮酸四級鏻;e)隨意地於聚胺甲酸酯化學中已知之輔助物質及添加劑,以便使兩種組份a)及b)以組份b)之每個羥基中有0.3至1個組份a)之脲二酮基之比率存在,較佳為0.6至0.9。
- 根據前述申請專利範圍第1至6項或11項中至少一項之預浸體,其中存在作為c)催化劑之甲酸四甲基銨、乙酸四甲基銨、丙酸四甲基銨、丁酸四甲基銨、苯甲酸四甲基銨、甲酸 四乙基銨、乙酸四乙基銨、丙酸四乙基銨、丁酸四乙基銨、苯甲酸四乙基銨、甲酸四丙基銨、乙酸四丙基銨、丙酸四丙基銨、丁酸四丙基銨、苯甲酸四丙基銨、甲酸四丁基銨、乙酸四丁基銨、丙酸四丁基銨、丁酸四丁基銨及苯甲酸四甲基銨及乙酸四丁基鏻、甲酸四丁基鏻及乙酸乙基三苯基鏻、苯並三唑四丁基鏻、酚四苯基鏻及癸酸三己基十四烷基鏻、氫氧化甲基三丁基銨、氫氧化甲基三乙基銨、氫氧化四甲基銨、氫氧化四乙基銨、氫氧化四丙基銨、氫氧化四丁基銨、氫氧化四戊基銨、氫氧化四己基銨、氫氧化四辛基銨、氫氧化四癸基銨、氫氧化十四烷基三己基銨、氫氧化四(十八烷基)銨、氫氧化苄基三甲基銨、氫氧化苄基三乙基銨、氫氧化三甲基苯基銨、氫氧化三乙基甲基銨、氫氧化三甲基乙烯基銨、甲醇甲基三丁基銨、甲醇甲基三乙基銨、甲醇四甲基銨、甲醇四乙基銨、甲醇四丙基銨、甲醇四丁基銨、甲醇四戊基銨、甲醇四己基銨、甲醇四辛基銨、甲醇四癸基銨、甲醇十四烷基三已基銨、甲醇四(十八烷基)銨、甲醇苄基三甲基銨、甲醇苄基三乙基銨、甲醇三甲基苯基銨、甲醇三乙基甲基銨、甲醇三甲基乙烯基銨、乙醇甲基三丁基銨、乙醇甲基三乙基銨、乙醇四甲基銨、乙醇四乙基銨、乙醇四丙基銨、乙醇四丁基銨、乙醇四戊基銨、乙醇四己基銨、乙醇四辛基銨、乙醇四癸基銨、乙醇十四烷基三己基銨、乙醇四(十八烷基)銨、乙醇苄基三甲基銨、乙醇苄基三乙基銨、乙醇三甲基苯基銨、乙醇三乙基甲基銨、乙醇三甲基乙烯基銨、苄化 甲基三丁基銨、苄化甲基三乙基銨、苄化四甲基銨、苄化四乙基銨、苄化四丙基銨、苄化四丁基銨、苄化四戊基銨、苄化四己基銨、苄化四辛基銨、苄化四癸基銨、苄化十四烷基三已基銨、苄化四(十八烷基)銨、苄化苄基三甲基銨、苄化苄基三乙基銨、苄化三甲基苯基銨、苄化三乙基甲基銨、苄化三甲基乙烯基銨、氟化四甲基銨、氟化四乙基銨、氟化四丁基銨、氟化四辛基銨、氟化苄基三甲基銨、氫氧化四丁基鏻、氟化四丁基鏻、氯化四丁基銨、溴化四丁基銨、碘化四丁基銨、氯化四乙基銨、溴化四乙基銨、碘化四乙基銨、氯化四甲基銨、溴化四甲基銨、碘化四甲基銨、氯化苄基三甲基銨、氯化苄基三乙基銨、氯化苄基三丙基銨、氯化苄基三丁基銨、氯化甲基三丁基銨、氯化甲基三丙基銨、氯化甲基三乙基銨、氯化甲基三苯基銨、氯化苯基三甲基銨、溴化苄基三甲基銨、溴化苄基三乙基銨、溴化苄基三丙基銨、溴化苄基三丁基銨、溴化甲基三丁基銨、溴化甲基三丙基銨、溴化甲基三乙基銨、溴化甲基三苯基銨、溴化苯基三甲基銨、碘化苄基三甲基銨、碘化苄基三乙基銨、碘化苄基三丙基銨、碘化苄基三丁基銨、碘化甲基三丁基銨、碘化甲基三丙基銨、碘化甲基三乙基銨、碘化甲基三苯基銨及碘化苯基三甲基銨、氫氧化甲基三丁基銨、氫氧化甲基三乙基銨、氫氧化四甲基銨、氫氧化四乙基銨、氫氧化四丙基銨、氫氧化四丁基銨、氫氧化四戊基銨、氫氧化四己基銨、氫氧化四辛基銨、氫氧化四癸基銨、氫氧化十四烷基三己基銨、氫氧化四(十 八烷基)銨、氫氧化苄基三甲基銨、氫氧化苄基三乙基銨、氫氧化三甲基苯基銨、氫氧化三乙基甲基銨、氫氧化三甲基乙烯基銨、氟化四甲基銨、氟化四乙基銨、氟化四丁基銨、氟化四辛基銨及氟化苄基三甲基銨,單獨地或以任何期望之混合物形式存在,較佳為苯甲酸四乙基銨及/或氫氧化四銨。
- 根據前述申請專利範圍第1至6項或11項中至少一項之預浸體,其中存在作為輔催化劑d1)之縮水甘油醚、脂族環氧化物、以雙酚A為基底之二縮水甘油醚、及甲基丙烯酸縮水甘油酯,單獨地或以任何期望之混合物形式存在。
- 根據前述申請專利範圍第1至6項或11項中至少一項之預浸體,其中存在作為輔催化劑d2)之乙醯丙酮酸鋅、乙醯丙酮酸鋰及乙醯丙酮酸錫,較佳是乙醯丙酮酸鋅,單獨地或以任何期望之混合物形式存在。
- 根據前述申請專利範圍第1至6項或11項中至少一項之預浸體,其中存在作為輔催化劑d2)之乙醯丙酮酸四甲基銨、乙醯丙酮酸四乙基銨、乙醯丙酮酸四丙基銨、乙醯丙酮酸四丁基銨、乙醯丙酮酸苄基三甲基銨、乙醯丙酮酸苄基三乙基銨、乙醯丙酮酸四甲基鏻、乙醯丙酮酸四乙基鏻、乙醯丙酮酸四丙基鏻、乙醯丙酮酸四丁基鏻、乙醯丙酮酸苄基三甲基鏻、乙醯丙酮酸苄基三乙基鏻,單獨地或以任何期望 之混合物形式存在,較佳為乙醯丙酮酸四乙基銨及/或乙醯丙酮酸四丁基銨。
- 根據申請專利範圍第1項之預浸體,其中該樹脂組份b)於20至23℃下為液態,且以低於20℃下為液態特佳。
- 根據申請專利範圍第1項之預浸體,其中存在作為液態樹脂組份b)之單體多元醇、聚酯、聚己內醯胺、聚醚、聚丙烯酸酯、聚碳酸酯及聚胺甲酸酯,其具有50至2000毫克氫氧化鉀/克之OH數及62至3000克/莫耳之平均莫耳質量。
- 根據申請專利範圍第1項之預浸體,其中存在作為液態樹脂組份b)之多元醇,其具有200至1500毫克氫氧化鉀/克之OH數,特佳具有501至1000毫克氫氧化鉀/克之OH數,且極特佳具有600至800毫克氫氧化鉀/克之OH數。
- 根據申請專利範圍第1項之預浸體,其中存在作為液態樹脂組份b)之多元醇,其具有100至1000克/莫耳之平均分子量,特佳具有100至500克/莫耳之平均分子量。
- 根據申請專利範圍第1項之預浸體, 其中存在作為液態樹脂組份b)之多元醇,其具有501至1000毫克氫氧化鉀/克之OH數,且其於20至23℃下為液態,以低於20℃下為液態特佳。
- 根據申請專利範圍第1項之預浸體,其具有大於10%之纖維體積含量,較佳為50-70%,特佳為50至65%。
- 一種預浸體,實質上由下列者所組成A)及B)及C)至少一種箔,其經由聚胺甲酸酯組成物B)而固定於該預浸體上。
- 一種製造根據申請專利範圍第1至23項中至少一項之預浸體的方法,該預浸體實質上由下列者所組成A)至少一種纖維支架及B)至少一種作為基質材料之反應性聚胺甲酸酯組成物,其中該聚胺甲酸酯組成物實質上含有下列者之混合物:液態樹脂組份b),其具有對異氰酸酯具反應性之官能基且具有低於25℃之Tg或熔點,且具有 介於50至2000毫克氫氧化鉀/克間之OH數;及作為熟化劑a)之內部阻斷及/或被阻斷劑所阻斷之二-或聚異氰酸酯,該方法為I.藉製造反應性聚胺甲酸酯組成物B),及II.將纖維支架A)以聚胺甲酸酯組成物B)(其已隨意地溶於溶劑中)浸漬,III.再隨意地將溶劑移除。
- 根據申請專利範圍第24項之製造方法,其中該基質材料B)係以高黏度材料、液體或固體形式使用。
- 一種製造根據申請專利範圍第1至23項中至少一項之預浸體的直接熔融浸漬方法,該預浸體實質上由下列者所組成A)至少一種纖維支架及B)至少一種作為基質材料之反應性聚胺甲酸酯組成物,其中該聚胺甲酸酯組成物實質上含有下列者之混合物:液態樹脂組份b),其具有對異氰酸酯具反應性之官能基且具有低於25℃之Tg或熔點,且具有介於50至2000毫克氫氧化鉀/克間之OH數;該方法為 I.藉製造反應性聚胺甲酸酯組成物B)於熔融物中,及II.將纖維支架A)直接以B)之熔融物浸漬。
- 一種根據前述申請專利範圍第1至23項中至少一項之預浸體的用途,特別是具有玻璃、碳或芳綸纖維之纖維支架者。
- 一種使用根據申請專利範圍第27項所製之預浸體於製造於船及造船業、於航太技術、於汽車製造、及於腳踏車、較佳為摩托車及自行車,及於汽車部門、運輸、營建、醫學工程、運動、電力及電子工業、及發電廠中之複合材料(例如製造風力發電廠中之轉動葉片)的用途。
- 一種複合材料組份,其係由根據申請專利範圍第1至23項中至少一項之預浸體所製。
- 一種由根據申請專利範圍第1至23項中至少一項之預浸體所製的複合材料組份,該預浸體係由下列者所組成:A)至少一種纖維支架及B)至少一種交聯聚胺甲酸酯組成物,較佳為含有脲二酮基之交聯聚胺甲酸酯組成物。
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DE102012219324A1 (de) | 2012-10-23 | 2014-04-24 | Evonik Industries Ag | Zusammensetzungen umfassend alkoxysilanhaltige Isocyanateund saure Stabilisatoren |
DE102013204124A1 (de) | 2013-03-11 | 2014-09-11 | Evonik Industries Ag | Composite-Halbzeuge und daraus hergestellte Formteile sowie direkt hergestellte Formteile auf Basis von hydroxyfunktionalisierten (Meth)Acrylaten und Uretdionen die mittels Strahlung duroplastisch vernetzt werden |
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2011
- 2011-03-25 DE DE201110006163 patent/DE102011006163A1/de not_active Withdrawn
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2012
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- 2012-03-21 US US14/007,585 patent/US10633519B2/en active Active
- 2012-03-21 KR KR1020137027734A patent/KR101879900B1/ko active IP Right Grant
- 2012-03-21 ES ES12710498T patent/ES2764524T3/es active Active
- 2012-03-21 CA CA2830456A patent/CA2830456A1/en not_active Abandoned
- 2012-03-21 MY MYPI2013003402A patent/MY167878A/en unknown
- 2012-03-21 WO PCT/EP2012/054938 patent/WO2012130672A1/de active Application Filing
- 2012-03-21 RU RU2013147458/04A patent/RU2013147458A/ru not_active Application Discontinuation
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- 2012-03-21 AU AU2012234522A patent/AU2012234522B2/en not_active Ceased
- 2012-03-23 TW TW101110159A patent/TWI597310B/zh not_active IP Right Cessation
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2013
- 2013-10-22 ZA ZA2013/07861A patent/ZA201307861B/en unknown
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---|---|
AU2012234522A1 (en) | 2013-10-10 |
CN103459452A (zh) | 2013-12-18 |
KR20140024333A (ko) | 2014-02-28 |
JP2014510813A (ja) | 2014-05-01 |
KR101879900B1 (ko) | 2018-07-18 |
TWI597310B (zh) | 2017-09-01 |
ZA201307861B (en) | 2014-07-30 |
MX354837B (es) | 2018-03-21 |
AU2012234522B2 (en) | 2015-04-16 |
DE102011006163A1 (de) | 2012-09-27 |
US10633519B2 (en) | 2020-04-28 |
CA2830456A1 (en) | 2012-10-04 |
MY167878A (en) | 2018-09-26 |
EP2688934B1 (de) | 2019-10-02 |
MX2013010790A (es) | 2013-10-30 |
JP5955376B2 (ja) | 2016-07-20 |
ES2764524T3 (es) | 2020-06-03 |
US20140087613A1 (en) | 2014-03-27 |
RU2013147458A (ru) | 2015-04-27 |
EP2688934A1 (de) | 2014-01-29 |
WO2012130672A1 (de) | 2012-10-04 |
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