CN106947061A - 用于制备纤维复合材料的液体浸渍工艺用潜伏性环氧树脂组合物 - Google Patents
用于制备纤维复合材料的液体浸渍工艺用潜伏性环氧树脂组合物 Download PDFInfo
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- CN106947061A CN106947061A CN201611128605.4A CN201611128605A CN106947061A CN 106947061 A CN106947061 A CN 106947061A CN 201611128605 A CN201611128605 A CN 201611128605A CN 106947061 A CN106947061 A CN 106947061A
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- Prior art keywords
- epoxide
- polyamines
- epoxy resin
- amino
- diamines
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- 239000002131 composite material Substances 0.000 title claims abstract description 41
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 36
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000007788 liquid Substances 0.000 title claims abstract description 10
- 230000008595 infiltration Effects 0.000 title abstract description 4
- 238000001764 infiltration Methods 0.000 title abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 84
- 150000002118 epoxides Chemical class 0.000 claims abstract description 26
- 239000004848 polyfunctional curative Substances 0.000 claims abstract description 12
- -1 epoxide compound Chemical class 0.000 claims description 58
- 229920000768 polyamine Polymers 0.000 claims description 45
- 150000004985 diamines Chemical class 0.000 claims description 29
- 150000001412 amines Chemical class 0.000 claims description 28
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 23
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 20
- 229920005989 resin Polymers 0.000 claims description 18
- 239000011347 resin Substances 0.000 claims description 18
- FTVFPPFZRRKJIH-UHFFFAOYSA-N 2,2,6,6-tetramethylpiperidin-4-amine Chemical compound CC1(C)CC(N)CC(C)(C)N1 FTVFPPFZRRKJIH-UHFFFAOYSA-N 0.000 claims description 16
- 239000000654 additive Substances 0.000 claims description 16
- 230000000996 additive effect Effects 0.000 claims description 15
- 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 15
- PXKLMJQFEQBVLD-UHFFFAOYSA-N Bisphenol F Natural products C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 150000002148 esters Chemical class 0.000 claims description 12
- 238000005516 engineering process Methods 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 10
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 9
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 8
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 8
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 8
- 239000007795 chemical reaction product Substances 0.000 claims description 8
- 239000011162 core material Substances 0.000 claims description 8
- 125000000524 functional group Chemical group 0.000 claims description 8
- LCFVJGUPQDGYKZ-UHFFFAOYSA-N Bisphenol A diglycidyl ether Chemical compound C=1C=C(OCC2OC2)C=CC=1C(C)(C)C(C=C1)=CC=C1OCC1CO1 LCFVJGUPQDGYKZ-UHFFFAOYSA-N 0.000 claims description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 7
- 150000002989 phenols Chemical class 0.000 claims description 7
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims description 6
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 6
- 239000005977 Ethylene Substances 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerol Natural products OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- IMUDHTPIFIBORV-UHFFFAOYSA-N aminoethylpiperazine Chemical class NCCN1CCNCC1 IMUDHTPIFIBORV-UHFFFAOYSA-N 0.000 claims description 6
- 229940106691 bisphenol a Drugs 0.000 claims description 6
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 6
- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical compound NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 claims description 6
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 5
- 125000001931 aliphatic group Chemical group 0.000 claims description 5
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 5
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- QWNVAOLTCRRZGS-UHFFFAOYSA-N 3-n,1,5,5-tetramethylcyclohexane-1,3-diamine Chemical compound CNC1CC(C)(C)CC(C)(N)C1 QWNVAOLTCRRZGS-UHFFFAOYSA-N 0.000 claims description 4
- 239000001361 adipic acid Substances 0.000 claims description 4
- 235000011037 adipic acid Nutrition 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 125000003118 aryl group Chemical group 0.000 claims description 4
- GGBJHURWWWLEQH-UHFFFAOYSA-N butylcyclohexane Chemical compound CCCCC1CCCCC1 GGBJHURWWWLEQH-UHFFFAOYSA-N 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims description 4
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 claims description 4
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 4
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 4
- ITZPOSYADVYECJ-UHFFFAOYSA-N n'-cyclohexylpropane-1,3-diamine Chemical compound NCCCNC1CCCCC1 ITZPOSYADVYECJ-UHFFFAOYSA-N 0.000 claims description 4
- SYSQUGFVNFXIIT-UHFFFAOYSA-N n-[4-(1,3-benzoxazol-2-yl)phenyl]-4-nitrobenzenesulfonamide Chemical class C1=CC([N+](=O)[O-])=CC=C1S(=O)(=O)NC1=CC=C(C=2OC3=CC=CC=C3N=2)C=C1 SYSQUGFVNFXIIT-UHFFFAOYSA-N 0.000 claims description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 4
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 claims description 4
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 claims description 3
- OOCWELITDFHVKI-UHFFFAOYSA-N 3-ethyl-1-methoxy-2,2,6,6-tetramethylpiperidin-4-amine Chemical class CON1C(C(C(CC1(C)C)N)CC)(C)C OOCWELITDFHVKI-UHFFFAOYSA-N 0.000 claims description 3
- FDLQZKYLHJJBHD-UHFFFAOYSA-N [3-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC(CN)=C1 FDLQZKYLHJJBHD-UHFFFAOYSA-N 0.000 claims description 3
- 125000002723 alicyclic group Chemical group 0.000 claims description 3
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 150000003512 tertiary amines Chemical class 0.000 claims description 3
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 claims description 2
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical class NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 2
- NNKQRURNVUHWKB-UHFFFAOYSA-N 1-butyl-2,2,6,6-tetramethylpiperidin-4-amine Chemical class CCCCN1C(C)(C)CC(N)CC1(C)C NNKQRURNVUHWKB-UHFFFAOYSA-N 0.000 claims description 2
- CTKXYQMUGQCAQH-UHFFFAOYSA-N 1-ethyl-2,2,6,6-tetramethylpiperidin-4-amine Chemical class CCN1C(C)(C)CC(N)CC1(C)C CTKXYQMUGQCAQH-UHFFFAOYSA-N 0.000 claims description 2
- JCUZDQXWVYNXHD-UHFFFAOYSA-N 2,2,4-trimethylhexane-1,6-diamine Chemical class NCCC(C)CC(C)(C)CN JCUZDQXWVYNXHD-UHFFFAOYSA-N 0.000 claims description 2
- MPNQOTJXVYHXNQ-UHFFFAOYSA-N 2,2,6,6-tetramethyl-1-(2-morpholin-4-ylethyl)piperidin-4-amine Chemical class O1CCN(CC1)CCN1C(CC(CC1(C)C)N)(C)C MPNQOTJXVYHXNQ-UHFFFAOYSA-N 0.000 claims description 2
- VMPDMPSCHGFNHB-UHFFFAOYSA-N 2,2,6,6-tetramethyl-1-propan-2-ylpiperidin-4-amine Chemical class C(C)(C)N1C(CC(CC1(C)C)N)(C)C VMPDMPSCHGFNHB-UHFFFAOYSA-N 0.000 claims description 2
- DPQHRXRAZHNGRU-UHFFFAOYSA-N 2,4,4-trimethylhexane-1,6-diamine Chemical compound NCC(C)CC(C)(C)CCN DPQHRXRAZHNGRU-UHFFFAOYSA-N 0.000 claims description 2
- WTYYGFLRBWMFRY-UHFFFAOYSA-N 2-[6-(oxiran-2-ylmethoxy)hexoxymethyl]oxirane Chemical compound C1OC1COCCCCCCOCC1CO1 WTYYGFLRBWMFRY-UHFFFAOYSA-N 0.000 claims description 2
- IHHPUXJKPWXNQZ-UHFFFAOYSA-N 2-ethylpiperazin-1-amine Chemical class CCC1CNCCN1N IHHPUXJKPWXNQZ-UHFFFAOYSA-N 0.000 claims description 2
- JZUHIOJYCPIVLQ-UHFFFAOYSA-N 2-methylpentane-1,5-diamine Chemical compound NCC(C)CCCN JZUHIOJYCPIVLQ-UHFFFAOYSA-N 0.000 claims description 2
- POTQBGGWSWSMCX-UHFFFAOYSA-N 3-[2-(3-aminopropoxy)ethoxy]propan-1-amine Chemical class NCCCOCCOCCCN POTQBGGWSWSMCX-UHFFFAOYSA-N 0.000 claims description 2
- FWJOQNJBRSHMEO-UHFFFAOYSA-N 4-(2,2,6,6-tetramethylpiperidin-4-yl)morpholine Chemical class C1C(C)(C)NC(C)(C)CC1N1CCOCC1 FWJOQNJBRSHMEO-UHFFFAOYSA-N 0.000 claims description 2
- 244000226021 Anacardium occidentale Species 0.000 claims description 2
- 229930185605 Bisphenol Natural products 0.000 claims description 2
- 239000009261 D 400 Substances 0.000 claims description 2
- 229920003656 Daiamid® Polymers 0.000 claims description 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical class NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical class NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 claims description 2
- 125000002252 acyl group Chemical group 0.000 claims description 2
- 150000004982 aromatic amines Chemical class 0.000 claims description 2
- XUCHXOAWJMEFLF-UHFFFAOYSA-N bisphenol F diglycidyl ether Chemical compound C1OC1COC(C=C1)=CC=C1CC(C=C1)=CC=C1OCC1CO1 XUCHXOAWJMEFLF-UHFFFAOYSA-N 0.000 claims description 2
- RGTXVXDNHPWPHH-UHFFFAOYSA-N butane-1,3-diamine Chemical compound CC(N)CCN RGTXVXDNHPWPHH-UHFFFAOYSA-N 0.000 claims description 2
- 235000020226 cashew nut Nutrition 0.000 claims description 2
- 239000000539 dimer Substances 0.000 claims description 2
- 125000000031 ethylamino group Chemical group [H]C([H])([H])C([H])([H])N([H])[*] 0.000 claims description 2
- 125000000623 heterocyclic group Chemical group 0.000 claims description 2
- 238000001802 infusion Methods 0.000 claims description 2
- GKQPCPXONLDCMU-CCEZHUSRSA-N lacidipine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C1=CC=CC=C1\C=C\C(=O)OC(C)(C)C GKQPCPXONLDCMU-CCEZHUSRSA-N 0.000 claims description 2
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 claims description 2
- 150000002762 monocarboxylic acid derivatives Chemical class 0.000 claims description 2
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- ZETYUTMSJWMKNQ-UHFFFAOYSA-N n,n',n'-trimethylhexane-1,6-diamine Chemical compound CNCCCCCCN(C)C ZETYUTMSJWMKNQ-UHFFFAOYSA-N 0.000 claims description 2
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 claims description 2
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- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 2
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- ZECYMOKSTOKOIF-UHFFFAOYSA-N 2-(4-amino-2,2,6,6-tetramethylpiperidin-1-yl)ethanol Chemical class CC1(C)CC(N)CC(C)(C)N1CCO ZECYMOKSTOKOIF-UHFFFAOYSA-N 0.000 claims 1
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- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 claims 1
- DJOWTWWHMWQATC-KYHIUUMWSA-N Karpoxanthin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1(O)C(C)(C)CC(O)CC1(C)O)C=CC=C(/C)C=CC2=C(C)CC(O)CC2(C)C DJOWTWWHMWQATC-KYHIUUMWSA-N 0.000 claims 1
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Abstract
本发明涉及用于制备纤维复合材料的液体浸渍工艺用潜伏性环氧树脂组合物。本发明提供由至少一种树脂组分和至少一种硬化剂组分构成的环氧化物组合物，该组合物适合作为用于制备纤维‑基质‑半成品和硬化的纤维‑基质‑层压物的热固性基质。
Description
技术领域
本发明提供由至少一种树脂组分和至少一种硬化剂组分构成的环氧化物组合物，该组合物适合作为用于制备纤维-基质-半成品和硬化的纤维-基质-层压物，所谓的复合材料的热固性基质。
背景技术
由至少一种环氧树脂和至少一种硬化剂，例如胺、醛、双氰胺，构成的环氧化物组合物长期以来是已知的，并用于例如涂料、复合材料或地板应用领域中。在此上下文中，将复合材料理解为是指纤维和塑料基质的复合材料。
在日益增长的有效利用稀缺资源的要求的范围内，轻质结构解决方案在各种行业中越来越受到关注。在必须移动大量/物料（Massen）的所有地方，纤维复合材料/复合材料都是令人感兴趣的选择，因为其在提供低重量的同时提供了高的比刚度和强度。由于这个原因，复合材料在航空领域已投入使用了几十年，而且如果没有纤维复合材料技术，例如用于风能源设备的转子叶片也是不可想象的。由于其优异的性能特征，这些材料在汽车制造中也越来越受到关注。在所提及的所有3个细分市场中均需要高机械强度的部件，如这可通过连续纤维增强的聚合物材料来实现。然而，对这些部件的几何形状的要求变得越来越高（例如，风能源设备的转子叶片的长度不断增加，以便能够尽可能多地“收获”风能），同时需要越来越高的生产率。
在本发明范围内，将术语复合材料（Composites）尤其与术语复合材料（Verbundstoff）、复合部件、复合材料（Verbundwerkstoff）、纤维复合材料、复合-模制品、纤维增强塑料或纤维增强部件、预浸料、纤维-基质-半成品、SMC(片状模塑料(SheetMoulding Compound))、SMC-复合材料(SMC-纤维-基质-半成品)、CFK、GFK和FVK同义使用。
制备复合材料的方法可分为单级法，例如RTM(树脂转换模塑法(Resin TransferMoulding))、VARTM(真空辅助树脂转换模塑法(Vacuum Assisted Resin TransferMoulding))，以及多级法，例如预浸料技术、SMC(片状模塑料(Sheet MouldingCompound))。
在多级法中经由纤维半成品（例如用预聚物浸渍的基于玻璃纤维或碳纤维的纺织平面构型物品，预浸料）的路线具有优点。特别是在连续纤维增强的结构部件的范围内，由于树脂基质对纤维的优异润湿性能，预浸料技术提供了获得极高机械品质的部件的途径，因此，在航空领域中，预浸料技术多年来已作为生产复合材料部件的最重要的加工方法。然而，纤维半成品由于它们的性质是二维平面构型物品，因此其应用可能性局限于生产具有有限几何复杂性的平的基本为二维或三维部件，例如翼或尾翼部件。预浸料技术在风能源设备用的转子叶片的制造中也是已采用的方法。
与此相比，具有高复杂度的三维几何形状的连续纤维增强的复合材料部件以RTM方法来制备。该方法的特征在于，首先由纺织平面构型物品制备所谓的近净形预成型件。在这种情况中，将未用树脂浸渍的纤维产品（即，织物、稀松布、无纺织物等以交付状态）近净形预成型为三维构型物品，并且同时粘合各层以固定，或者在特别复杂的部件的情况下，缝合。然后，将这种纯纤维预成型件引入腔中，并且在封闭腔，例如加热的钢模具中，用不含溶剂的液体树脂组合物浸渍，并且在该封闭的腔中立即完全硬化直至最终状态（单级法）。在此出现的部分具有高复杂度的流动几何（Fließgeometrien）需要具有长适用期的低粘度树脂，以便有效地润湿所有纤维长丝。因此，用于此的树脂体系具有低反应性，并且需要在高温下长的硬化时间。硬化后，将制成的部件脱模，并任选还进一步处理，例如去毛刺。
然而，如上所述的单级RTM法在生产具有非常大的尺寸的部件，诸如例如风能源设备的转子叶片时，或在以小的件数制造原型时在技术上或经济上是不可行的（钢模具过高的重量和/或过高的成本）。在此，在开放-模具-制造方式中使用不同的液体浸渍方法（真空灌注方法，压力最大1巴），例如记载在F. Henning/E. Moeller „Handbuch Leichtbau“,Carl-Hanser-verlag, 第641页及以后几页中。 该模具仅由下半部组成，并且除了金属材料而外也可以由复合材料制成; 在这些方法中，由待浸渍的增强纤维和任选的其它预制部件或芯材料构成的结构从顶部用真空薄膜密封。施加真空产生最大1巴的压力差，因此，在灌注法中使用的树脂体系必须具有非常低的粘度并且必须具有长的加工时间。 通常，在制造大部件时流动路径长，并且由于小的压力差，流速小。
适合于此目的的低反应性的无溶剂环氧树脂组合物是已知的，例如树脂体系EPIKOTE™ Resin MGS™ RIMR235，其具有来自Hexion的EPIKURE™固化剂MGS™ RIMH233,RIMH235-237。
在文献DE 2640408、DE 2640409、DE 2540410、DE 2950067和DE 3328134中记载了2,2,6,6-四甲基-4-哌啶胺(简称为三丙酮二胺或缩写为TAD)作为用于硬化环氧树脂的潜伏性胺。作为应用，在这些文献中合适的是重点为粉末漆的表面涂料和任选可用纤维或其它物质增强的模塑料。作为实例列举了纯TAD和环氧树脂的组合。然而，这些体系仅热硬化，并且通常不能如在以开放模具制造方法制造大部件，例如风能源设备用的转子叶片时那样，在70至80℃的硬化温度下使用。
发明内容
发明目的
复合材料的性能除了由所选择的树脂基质和增强纤维的性能特征决定而外，还非常特别地为纤维基质复合材料的品质所决定。复合材料的高品质以树脂基质无缺陷地润湿所有增强纤维为先决条件。在制造非常大的部件如风能源设备的转子叶片时，树脂组合物必须在真空灌注法中在最大1巴的压力下流过长的流动路径。此外，待浸渍的由增强纤维、预制部件和芯材料构成的结构经常除了其复杂性而外也具有高的壁厚。这些层必须被液体树脂组合物完全地并且没有缺陷地渗透和润湿。
鉴于对生产越来越高比例的再生能源的需求，风能源设备的转子叶片的尺寸变得越来越大。 因此，如上所述的传统的环氧化物树脂组合物接近其加工性的极限，并且存在对具有明显更长时间“开放”，即具有明显更长时间的低粘度并且在该低粘度下可自由流动的环氧化物树脂组合物的需求，以使以所需的品质润湿所有纤维，但是由于生产率的原因，周期时间不允许有显著的上升，并且在灌注持续期间，在树脂容器（树脂储罐）中不允许产生高的放热温度峰。
解决方案
已经令人惊讶地发现，根据本发明的环氧树脂组合物可以在宽范围内调节，以使得其满足对较长加工时间的要求，由此可以使例如树脂储罐中直至达到临界温度的时间增加40％和将直至达到1000mPas的粘度极限的时间增加12％。在70℃下的硬化提供了≥70℃的玻璃化转变温度，转化率≥95％，这符合了例如根据GL（Germanischer Lloyd）的用于转子叶片的要求。
用于制备三维部件的有效的液体浸渍法用的本发明的环氧树脂组合物具有下列有利性能：
- 低粘度
- 相应于所需流动路径的时间长度的低粘度，直至没有缺陷地浸渍所有纤维
- 浸渍所有纤维后在所选择的条件下硬化，以确保所需要的生产率
- 没有产生放热温度峰，其可能导致树脂体系开始分解和/或由于复合材料中的应力累积而形成裂纹
- 其满足所有对机械、热和介质稳定性的所有要求并具有好的表面性能。
本发明提供环氧树脂组合物，其包含：
A) 至少一种环氧化物化合物
和
B) 硬化剂组合物，其由下列组分构成：
B1) 5-65重量%至少一种基于三丙酮二胺的多胺
和
B2) 35-95重量%至少一种另外的二胺和/或多胺，
其中，A)的环氧基团与B)的官能团的活性氢原子的数量的化学计量比在1:0.5-1:1之间变动，优选1:0.6-1:1.05，特别优选1:0.95-1:1.05；
C) 任选至少一种硬化加速剂，
其中A)-C)的量合计为100重量%，
D) 任选另外的添加剂。
组分A)
作为组分A)合适的是环氧化物化合物。合适的环氧化物化合物记载在例如EP 675 185中。
大量为此目的已知的化合物被考虑在内，其每分子包含多于一个环氧基团，优选两个环氧基团。这些环氧化物化合物可以是饱和或不饱和的以及脂族、脂环族、芳族或杂环的，并且也可以具有羟基。它们可另外含有在混合条件或反应条件下不引起干扰性副反应的取代基，例如烷基取代基或芳基取代基、醚基团等。优选地，它们是衍生自多元酚，特别是双酚和酚醛清漆的缩水甘油基醚，其基于环氧基团的数量计的摩尔质量ME（“环氧当量”、“EV值”）为100-1500，但是尤其为150-250 g /当量。
作为多元酚例如可提及：间苯二酚、氢醌、2,2-双-(4-羟基苯基)丙烷(双酚A)、二羟基二苯基甲烷的异构体混合物(双酚F)、4,4'-二羟基二苯基环己烷、4,4'-二羟基-3,3'-二甲基二苯基丙烷、4,4'-二羟基二苯基、4,4'-二羟基二苯甲酮、双-(4-羟基苯基)-1,1-乙烷、双-(4-羟基苯基)-1,1-异丁烷、2,2-双-(4-羟基-叔丁基苯基)丙烷、双-(2-羟基萘基)甲烷、1,5-二羟基萘、三-(4-羟基苯基)甲烷、双-(4-羟基苯基)醚、双-(4-羟基苯基)砜以及其它，以及上述化合物的氯化产物和溴化产物，例如四溴双酚A。特别优选地，使用基于双酚A和双酚F的液体二缩水甘油基醚，其具有150-200 g/当量的环氧当量。
也可以使用多元醇的多缩水甘油基醚，例如乙二醇-1,2-二缩水甘油基醚、丙二醇-1,2-二缩水甘油基醚、丙二醇-1,3-二缩水甘油基醚、丁二醇二缩水甘油基醚、戊二醇二缩水甘油基醚(包括新戊二醇二缩水甘油基醚)、己二醇二缩水甘油基醚、二乙二醇二缩水甘油基醚、二丙二醇二缩水甘油基醚，更高级的多氧基亚烷基二醇二缩水甘油基醚（Polyoxyalkylenglykoldiglycidylether），例如更高级的多氧基乙二醇二缩水甘油基醚（Polyoxyäthylenglykoldiglycidylether）和多氧基丙二醇二缩水甘油基醚（Polyoxypropylenglykoldiglycidylether）、混合多氧基亚乙基-亚丙基二醇二缩水甘油基醚（Mischpolyoxyäthylen-propylenglykoldiglycidylether）、多氧基四亚甲基二醇二缩水甘油基醚，下述物质的多缩水甘油基醚：丙三醇、己烷-1,2,6-三醇、三羟甲基丙烷、三羟甲基乙烷、季戊四醇、山梨醇，烷氧基化多元醇(例如丙三醇、三羟甲基丙烷、季戊四醇以及其它)的多缩水甘油基醚、环己烷二甲醇的二缩水甘油基醚、双-(4-羟基环己基)甲烷的二缩水甘油基醚和2,2-双-(4-羟基环己基)丙烷的二缩水甘油基醚、蓖麻油的多缩水甘油基醚、三缩水甘油基三-(2-羟基乙基)异氰脲酸酯。
作为组分A)此外可以考虑：可通过表氯醇和胺的反应产物的脱氢卤化获得的多(N-缩水甘油基)化合物，所述胺如苯胺、正丁基胺、双-(4-氨基苯基)甲烷、间二甲苯二胺或双-(4-甲基氨基苯基)甲烷。但是，所述多(N-缩水甘油基)化合物也包括三缩水甘油基异氰脲酸酯、三缩水甘油基脲唑及其低聚物、环亚烷基脲的N,N'-二缩水甘油基衍生物和乙内酰脲的二缩水甘油基衍生物以及其它。
此外，也可以使用多元羧酸的多缩水甘油基酯，其通过表氯醇或类似的环氧化物化合物与脂族、脂环族或芳族多元羧酸的反应得到，所述多元羧酸如草酸、琥珀酸、己二酸、戊二酸、邻苯二甲酸、对苯二甲酸、四氢邻苯二甲酸、六氢邻苯二甲酸、2,6-萘二甲酸和更高级的二缩水甘油基二羧酸酯，例如二聚或三聚的亚麻酸。实例是己二酸二缩水甘油基酯、邻苯二甲酸二缩水甘油基酯和六氢邻苯二甲酸二缩水甘油基酯。
此外可提及不饱和羧酸的缩水甘油酯和不饱和醇或不饱和羧酸的环氧化的酯。除了多缩水甘油基醚之外，可以共同使用少量的单环氧化物，例如甲基缩水甘油基醚、丁基缩水甘油基醚、烯丙基缩水甘油基醚、乙基己基缩水甘油基醚，长链脂族缩水甘油基醚，例如鲸蜡基缩水甘油基醚和硬脂基缩水甘油基醚，高级异构醇混合物的单缩水甘油基醚、C12至C13醇的混合物的缩水甘油基醚、苯基缩水甘油基醚、甲苯基缩水甘油基醚、对叔丁基苯基缩水甘油基醚、对辛基苯基缩水甘油基醚、对苯基-苯基缩水甘油基醚、烷氧基化月桂醇的缩水甘油基醚以及单环氧化物例如环氧化单不饱和烃（环氧丁烷、环氧环己烷、氧化苯乙烯），其质量比例为至多30重量％，优选10至20重量％，基于多缩水甘油基醚的质量计。
合适的环氧化物化合物的详细列举可见于A. M. Paquin的手册"Epoxidverbindungen und Epoxidharze" 中，Springer Verlag, Berlin 1958, 第IV章,和Lee Neville "Handbook of Epoxy Resins"中, 1967, 第2章。
作为环氧化物化合物在此优选考虑缩水甘油基醚和缩水甘油酯，脂族环氧化物，基于双酚A和/或双酚F的二缩水甘油醚，和缩水甘油基甲基丙烯酸酯。这种环氧化物的实例还包括三缩水甘油基异氰脲酸酯(TGIC, 商品名: ARALDIT 810, Huntsman)、对苯二甲酸二缩水甘油酯和偏苯三酸三缩水甘油酯的混合物(商品名: ARALDIT PT 910和912,Huntsman)、叔碳酸（Versaticsäure）的缩水甘油酯(商品名: CARDURA E10, Shell)、3,4-环氧基环己基甲基-3',4'-环氧环己烷甲酸酯 (ECC)、乙基己基缩水甘油基醚、丁基缩水甘油基醚、季戊四醇四缩水甘油基醚 (商品名: POLYPOX R 16, UPPC AG)和其它具有游离环氧基团的Polypox类型。
也可以使用所述环氧化物化合物的混合物。
作为环氧组分，特别优选基于双酚A-二缩水甘油醚、双酚F-二缩水甘油醚、4,4'-亚甲基双[N,N-双(2,3-环氧丙基)苯胺]、己二醇二缩水甘油醚、丁二醇二缩水甘油醚、三羟甲基丙烷缩水甘油基醚、1,2,3-丙三醇三缩水甘油基醚、季戊四醇四缩水甘油基醚和六氢邻苯二甲酸二缩水甘油基酯的多环氧化物。根据本发明，这些环氧化物化合物的混合物也可优选作为组分A）来使用。
组分A）的量视组分B）的组成而定，并且如此计算，以使A）的环氧基团与B）的官能团的活性氢原子的数量的化学计量比在1:0.5至1:1的范围内变动，优选1:0.6-1:1.05，特别优选1:0.95-1:1.05。这意味着来自B）的氨基中的每一个氢原子与一个来自A）的环氧基团反应。
组分B1）
基于三丙酮二胺的多胺B1）从文献中通常已知。作为组分B1）优选使用基于三丙酮二胺的以下胺：2,2,6,6-四甲基-4-氨基哌啶(TAD)、六亚甲基双-(4-氨基-2,2,6,6-四甲基哌啶)、N-丁基-4-氨基-2,2,6,6-四甲基哌啶、N,N-二甲基氨基丙基-4-氨基-2,2,6,6-四甲基哌啶、N-丙基-4-氨基-2,2,6,6-四甲基哌啶、N-异丙基-4-氨基-2,2,6,6-四甲基哌啶、N-羟基乙基-4-氨基-2,2,6,6-四甲基哌啶、N-甲氧基乙基-4-氨基-2,2,6,6-四甲基哌啶、N-甲氧基乙基-4-氨基-2,2,6,6-四甲基哌啶、N',N'-二甲基氨基乙基-4-氨基-2,2,6,6-四甲基哌啶、N-吗啉代乙基-4-氨基-2,2,6,6-四甲基哌啶、N-哌嗪子基乙基-4-氨基-2,2,6,6-四甲基哌啶、4-吗啉代-2,2,6,6-四甲基哌啶。
也可以使用上述基于三丙酮二胺的胺B1)的混合物。
优选使用2,2,6,6-四甲基-4-氨基哌啶(TAD)和/或六亚甲基双-(4-氨基-2,2,6,6-四甲基哌啶)。
组分B1)的使用量通常为5-65重量%，优选25-55重量%，特别优选35-45重量%，基于B1)和B2)的总量计。
组分B2)
作为化合物B2）原则上合适的是包含至少2个氨基的二胺和多胺。二胺和多胺也可以以与氨基醇或多硫醇的混合物的形式来使用。
二胺或多胺B2）在文献中是已知的。这些可以是单体、低聚和/或聚合的化合物。单体和低聚的化合物优选选自二胺、三胺、四胺。二胺或多胺B2）的胺基团可以连接到伯、仲或叔碳原子上，优选连接到伯或仲碳原子上。
以下胺可用作组分B2），单独地或以混合物形式：
● 脂族胺，如多亚烷基多胺，优选选自1,2-乙二胺、1,2-丙二胺、1,3-丙二胺、1,2-丁二胺、1,3-丁二胺、1,4-丁二胺、2-(乙基氨基)乙胺、3-(甲基氨基)丙胺、二亚乙基三胺、三亚乙基四胺、五亚乙基六胺、三甲基六亚甲基二胺、2,2,4-三甲基六亚甲基二胺、2,4,4-三甲基六亚甲基二胺、2-甲基戊二胺、六亚甲基二胺、N-(2-氨基乙基)-1,2-乙二胺、N-(3-氨基丙基)-1,3-丙二胺、N,N''-1,2-乙烷二基双-(1,3-丙二胺)、二亚丙基三胺、己二酸二酰肼，肼;
● 氧基亚烷基多胺，选自多氧基亚丙基二胺和多氧基亚丙基三胺(例如Jeffamine®D-230, Jeffamine® D-400, Jeffamine® T-403, Jeffamine® T-5000)，1,13-二氨基-4,7,10-三氧杂十三烷、4,7-二氧杂癸烷-1,10-二胺;
● 脂环族胺，选自异佛尔酮二胺(3,5,5-三甲基-3-氨基甲基环己胺)、4,4'-二氨基二环己基甲烷、2,4'-二氨基二环己基甲烷和2,2'-二氨基二环己基甲烷，单独地或以异构体的混合物形式，3,3'-二甲基-4,4'-二氨基二环己基甲烷、N-环己基-1,3-丙二胺、1,2-二氨基环己烷、3-(环己基氨基)丙胺、哌嗪、N-氨基乙基哌嗪、TCD-二胺(3(4),8(9)-双(氨基甲基)三环[5.2.1.02,6]癸烷)、4-甲基环己烷-1,3-二胺
● 芳脂族胺，如二甲苯二胺;
● 芳族胺，选自苯二胺、1,3-苯二胺、1,4-苯二胺、4,4'-二氨基二苯基甲烷、2,4'-二氨基二苯基甲烷、2,2'-二氨基二苯基甲烷，单独地或以异构体的混合物形式；
● 加合物硬化剂，其是环氧化物化合物，特别是双酚A和F的缩水甘油基醚与过量胺的反应产物；
● 聚酰胺胺硬化剂，其通过单羧酸和多羧酸与多胺的缩合，特别是通过二聚脂肪酸与多亚烷基多胺的缩合获得;
● 曼尼希碱硬化剂，其通过一元或多元酚与醛，特别是甲醛和多胺的反应获得;
● 曼尼希碱，例如基于苯酚和/或间苯二酚、甲醛和间二甲苯二胺以及N-氨基乙基哌嗪和由N-氨基乙基哌嗪与壬基苯酚和/或苄醇构成的混合物，在从腰果酚类、醛和胺的曼尼希反应中获得的酚醛胺（Phenalkamine）。
也可以使用上述二胺或多胺的混合物作为组分B2)。
优选使用二胺作为组分B2)，其选自异佛尔酮二胺(3,5,5-三甲基-3-氨基甲基环己胺, IPD)、4,4'-二氨基二环己基甲烷、2,4'-二氨基二环己基甲烷、2,2'-二氨基二环己基甲烷(也称为PACM)，单独地或以异构体的混合物形式，选自多氧基亚丙基二胺和多氧基亚丙基三胺的氧基亚烷基多胺，基于环氧化物化合物和前述胺B2)或前述胺B2)的组合的反应产物的加合物硬化剂。也可以使用这些化合物的混合物。
作为组分B2)特别优选使用异佛尔酮二胺（3,5,5-三甲基-3-氨基甲基环己胺，IPD），
和/或由异佛尔酮二胺和/或PACM（4,4'-、2,4'-和2,2'-二氨基二环己基甲烷的异构体混合物）和多氧基亚丙基二胺和/或多氧基亚丙基三胺构成的组合，
和/或基于环氧化物化合物与上述胺B2)或上述胺B2)的组合的反应产物的加合物硬化剂。
作为组分B2)，非常特别优选使用
a) 异佛尔酮二胺(3,5,5-三甲基-3-氨基甲基环己胺, IPD),
b) 和/或异佛尔酮二胺与多氧基亚丙基二胺和/或多氧基亚丙基三胺的组合，
c) 和/或基于环氧化物化合物与上述胺B2)或上述胺B2)的组合的反应产物的加合物硬化剂。
在b）中的组分的量比，异佛尔酮二胺：多氧基亚丙基多胺和/或多氧基亚丙基三胺通常为10:90-90:10重量％，优选20:80-40:60重量％。
根据本发明，氨基醇可以用作组分B2）中的与二胺和多胺混合的另外的组分。作为氨基醇例如可提及单乙醇胺、3-氨基-1-丙醇、异丙醇胺、氨基乙氧基乙醇、N-(2-氨基乙基)乙醇胺、N-乙基乙醇胺、N-丁基乙醇胺、二乙醇胺、3-(羟基乙基氨基)-1-丙醇、异佛尔酮氨基醇和二异丙醇胺。氨基醇可以单独地或作为多种氨基醇的混合物与二胺和多胺一起作为组分B2)来使用。
根据本发明，多硫醇也可以用作组分B2）中的与二胺和多胺混合的另外的组分。作为硫醇（Mercaptane），也称为硫醇（Thiole）例如可提及乙硫醇、二硫苏糖醇、二硫赤藓糖醇、二硫代甘醇酸甘油酯、二巯基乙酸乙二醇酯、三羟甲基丙烷三巯基乙酸酯、季戊四醇四巯基乙酸酯、乙二醇二-(3-巯基丙酸酯)、三羟甲基丙烷三-(3-巯基丙酸酯)、季戊四醇四-(3-巯基丙酸酯)、二季戊四醇六-(3-巯基丙酸酯)、乙氧基化的三羟甲基丙烷三-(3-巯基丙酸酯)（商品名：Thiocure ETTMP 1300），三-[2-(3-巯基丙酰氧基)乙基]异氰脲酸酯。其它的硫醇描述于例如EP394495A1、US4775733A1和WO2007096425A2中。硫醇可以单独地或作为多种硫醇的混合物与二胺和多胺一起作为组分B2)来使用。
除了所提到的二胺和多胺之外，可以将二胺和多胺与多酚一起作为组分B2)来使用。对此的实例在“Epoxy Resins-Chemistry and Technology; Curing Agents andModifiers;第481-482页，第2版1988”中提到。多酚可以单独地或作为多种多酚的混合物与二胺和多胺一起作为组分B2)来使用。
组分B2）的用量通常为35-95重量％，优选45-75重量％，特别优选55-65重量％，基于B1)和B2)的总量计。
组分C）硬化加速剂
此外，任选添加用于环氧-胺反应的催化剂。合适的加速剂描述于：H.Lee和K.Neville，Handbook of Epoxy Resins，McGraw-Hill，New York，1967。根据本发明，使用0.1至10重量％，优选0.1至5重量％，特别优选0.5至2.0重量％的至少一种硬化加速剂。
合适的加速剂的实例是有机酸如水杨酸、二羟基苯甲酸、三羟基苯甲酸、甲基水杨酸、2-羟基-3-异丙基苯甲酸或羟基萘甲酸、乳酸和乙醇酸，叔胺如苄基二甲基胺(BDMA)、1,4-二氮杂双环[2.2.2]辛烷(DABCO)、三乙胺、N,N'-二甲基哌嗪或氨基乙基哌嗪(AEP)，羟胺如二甲基氨基甲基苯酚、双-(二甲基氨基甲基)苯酚、2,4,6-三-(二甲基氨基甲基)苯酚(Ancamine K54)，Urone如3-(4-氯苯基)-1,1-二甲基脲(灭草隆(Monuron))、3-(3,4-二氯苯基)-1,1-二甲基脲(敌草隆(Diuron))、3-苯基-1,1-二甲基脲(非草隆(Fenuron))、3-(3-氯-4-甲基苯基)-1,1-二甲基脲(绿麦隆(Chlortoluron))，四烷基胍如N,N,N',N'-四甲基胍(TMG)，咪唑和咪唑衍生物如1H-咪唑、1-甲基咪唑、2-甲基咪唑、1-苄基-2-甲基咪唑、2-乙基-4-甲基咪唑、2-苯基咪唑、2-苯基-4-甲基咪唑、1-乙烯基咪唑、1-(2-羟基乙基)咪唑、1,2-二甲基咪唑、1-氰基乙基咪唑及其合适的盐，苯酚和苯酚衍生物如叔丁基苯酚、壬基苯酚、双酚A或双酚F，以及有机或无机盐和配合物化合物如溴化甲基三苯基鏻、硝酸钙（Accelerator 3130），或Mg、Ca、Zn和Sn的羧酸盐、磺酸盐、膦酸盐、硫酸盐、四氟硼酸盐或硝酸盐。特别优选的是叔胺的基团。
组分D）添加剂
本发明的组合物可任选包含添加剂。将添加剂理解为是指通常添加以便在所希望的方向改变环氧化物组合物的性质，例如粘度、润湿特性、稳定性、反应速度、气泡形成、储存性或粘附性，以及使用性能，以匹配使用目的的物质。合适的添加剂描述于例如WO 99/55772，第15-25页中，以及在“Plastics Additives，R.Gächter和H.Müller，Hanser Publishers1983”中。这些可以加入到组分A)或B)中。
因此，可以以0.05至5重量％的总量加入例如光保护剂，例如位阻胺，或者其它助剂，其例如描述在EP 669 353中的。
为了制备本发明的反应性组合物，还可以添加添加剂如流平剂，例如有机硅（Polysilicone）或增粘剂，例如基于丙烯酸酯的那些。此外，还可以任选包含其它组分。
作为助剂和添加剂另外可以使用调节剂、增塑剂、稳定剂和/或抑制剂。
此外，可以添加染料、纳米级填料、增韧剂（韧性改进剂）、脱模剂、阻燃剂、颜料、干燥剂、润湿助剂、分散助剂和流平助剂、增粘剂、UV稳定剂、消泡剂和流变添加剂。
本发明还提供环氧树脂组合物用于制备复合材料的用途，所述环氧树脂组合物包含：
A) 至少一种环氧化物化合物
和
B) 硬化剂组合物，其由下列组分构成：
B1) 5-65重量%至少一种基于三丙酮二胺的多胺
和
B2) 35-95重量%至少一种另外的二胺和/或多胺，
其中A)的环氧基团与B)的官能团的活性氢原子的数量的化学计量比在1:0.5至1:1范围内变化，优选1:0.6-1:1.05，特别优选1:0.95-1:1.05，
C) 任选至少一种硬化加速剂，
其中A)-C)的量合计为100重量%，
D) 任选另外的添加剂。
本发明还提供复合材料部件，
其基本上由下述构成
1) 至少一种纤维状载体和任选的芯材料
和
2) 环氧树脂组合物，其包含：
A) 至少一种环氧化物化合物
和
B) 硬化剂组合物，其由下列组分构成：
B1) 5-65重量%至少一种基于三丙酮二胺的多胺
和
B2) 35-95重量%至少一种另外的二胺和/或多胺，
其中A)的环氧基团与B)的官能团的活性氢原子的数量的化学计量比在1:0.5至1:1范围内变化，优选1:0.6-1:1.05，特别优选1:0.95-1:1.05，
C) 任选至少一种硬化加速剂，
其中A)-C)的量合计为100重量%，
D) 任选另外的添加剂。
纤维状载体
根据本发明优选使用的纤维状载体材料的特征在于，该纤维状载体主要由玻璃、碳、塑料如聚酰胺（芳族聚酰胺）或聚酯、天然纤维或矿物纤维材料如玄武岩纤维或陶瓷纤维构成，单独地或由混合物，或由不同纤维类型的多个层构成。
所述纤维状载体作为由非织造织物、针织物/毛圈织物（Maschenwaren）、针织物（Gewirke）或纬编织物（Gestricke）、非针织构型物品（nicht maschige Gebinde）如织物(Gewebe)、稀松布或编织物（Geflechte）制成的纺织平面构型物品，作为长纤维材料或短纤维材料存在，单独地或由不同类型的多个层构成。
详述如下：本发明中的纤维状载体由纤维状材料（也常称为增强纤维）构成。通常，构成纤维的任何材料均是合适的，但是优选使用由玻璃、碳、塑料例如聚酰胺（芳族聚酰胺）或聚酯、天然纤维或矿物纤维材料如玄武岩纤维或陶瓷纤维（基于铝氧化物和/或硅氧化物的氧化纤维）。也可以使用纤维类型的混合物，例如芳族聚酰胺纤维和玻璃纤维，或碳和玻璃纤维的织物组合。
主要是因为它们相对低的价格，玻璃纤维是最常用的纤维类型。原则上，所有类型的玻璃基增强纤维（E-玻璃纤维、S-玻璃纤维、R-玻璃纤维、M-玻璃纤维、C-玻璃纤维、ECR-玻璃纤维、D-玻璃纤维、AR-玻璃纤维或中空玻璃纤维）在此都是合适的。
碳纤维通常用于高性能复合材料中，在那里，在同时具有高强度的情况下与玻璃纤维相比较低的密度也是一个重要因素。碳纤维是由含碳起始原料工业生产的纤维，其被热解转化为石墨状排列的碳。其被分为各向同性和各向异性类型：各向同性纤维仅具有低强度和较低的工业意义;各向异性纤维表现出高强度和刚性，同时具有低断裂伸长率。作为天然纤维在这里是指从植物和动物材料（例如木纤维、纤维素纤维、棉纤维、大麻纤维、黄麻纤维、亚麻纤维、剑麻纤维和竹纤维）获得的所有纺织纤维和纤维材料。与碳纤维类似，芳族聚酰胺纤维具有负的热膨胀系数，即在加热时变短。它们的比强度及其弹性模量明显低于碳纤维。与基质树脂的正膨胀系数相结合，可以生产高尺寸稳定性的部件。与碳纤维增强塑料相比，芳族聚酰胺纤维复合材料的抗压强度明显较低。芳族聚酰胺纤维的已知商品名为DuPont的Nomex®和Kevlar®，或Teijin的Teijinconex®、Twaron®和Technora®。特别合适和优选的是由玻璃纤维、碳纤维、芳族聚酰胺纤维或陶瓷纤维制成的载体。纤维状材料是纺织平面构型物品。合适的是由非织造织物、以及所谓的针织物/毛圈织物（Maschenwaren），如针织物（Gewirke）和纬编织物（Gestricke），以及非针织构型物品（nicht maschige Gebinde）如织物(Gewebe)、稀松布或编织物（Geflechte）制成的纺织平面构型物品。此外，对作为载体的长纤维材料和短纤维材料进行区分。根据本发明同样适合的是粗纱（Rovings）和纱线（Garne）。在本发明范围内，所提及的所有材料均适合作为纤维状载体。增强纤维的概述包含在“Composites Technologien”，Paolo Ermanni（第4版），ETHZürich讲座讲义，2007年8月，第7章中。
芯材料
合适的芯材料例如是：基于浸渍的纸、芳族聚酰胺纤维或轻质金属例如铝的蜂窝结构，基于轻质金属或热塑性或热固性聚合物材料如聚氨酯、聚烯烃、聚苯乙烯、聚甲基丙烯酰亚胺（PMI）的泡沫，例如Rohacell®，酚醛树脂或氰酸酯树脂以及木质材料，例如，轻木（Balsa-Holz）。
本发明也提供通过下述方法步骤制备复合材料的方法：
I. 提供反应性组合物，其包含
A) 至少一种环氧化物化合物
和
B) 硬化剂组合物，其由下列组分构成：
B1) 5-65重量%至少一种基于三丙酮二胺的多胺
和
B2) 35-95重量%至少一种另外的二胺和/或多胺，
其中A)的环氧基团与B)的官能团的活性氢原子的数量的化学计量比在1:0.5至1:1范围内变化，优选1:0.6-1:1.05，特别优选1:0.95-1:1.05，
C) 任选至少一种硬化加速剂，
其中A)-C)的量合计为100重量%，
D) 任选另外的添加剂;
II. 根据液体树脂浸渍法在模型(Form)中或模具（Werkzeug）中用得自I的组合物浸渍由纤维状载体和任选的其它芯材料构成的结构，或者浸渍纤维状载体并缠绕在芯轴（Dorn）上，
III. 使所述反应性组合物硬化成复合材料部件和
IV. 将制成的部件从模型中脱模。
本发明的主题特别还是根据本发明制备的复合材料在船舶制造中、航空航天技术中、汽车制造中，用于两轮车辆，优选摩托车和自行车，在汽车工业、建筑结构(Construction)（例如管道）、容器结构（Behälterbau）、医疗技术、运动、电气和电子工业、和尤其是能量产生装置，例如用于风力涡轮机领域中的用途。
本发明的环氧化物组合物特别适合用于制造风力涡轮机的转子叶片。
具体实施方式
实施例
在表1中解释在下面的实施例中使用的原料。
表1:原料
| 商品名 | 供应商 | 化学名称 | 缩写 |
| 三丙酮二胺 | Evonik Industries | 2,2,6,6-四甲基-4-氨基哌啶 | TAD |
| Vestamin® IPD | Evonik Industries | 3-氨基甲基-3,5,5-三甲基环己胺 | IPD |
| Jeffamine® D230 | Huntsman | 多氧基亚丙基二胺 | D230 |
| D.E.R. ® 351 | Dow Chemical | 由双酚A/双酚F和表氯醇制成的环氧基树脂 | - |
| D.E.R. ® 731 | Dow Chemical | 丁二醇二缩水甘油醚 | - |
在下面的实施例中使用的分析方法的描述：
粘度升高，等温
仪器:Rheotec Rheometer RC 30
测量体系:EWS30-CC25 DIN/FTK
带有 MB30-CC25 DIN/FTK 杯
用量:16 g
温控:Julabo F33-ME制冷循环恒温器（Kälte-Umwälzthermostat）
树脂/硬化剂组合物的温度升高
仪器:Yokogawa 4153 3-channel µP recorder
热电偶:NiCr-Ni -200℃至1370℃
用量:900 g
温控:Julabo F33-ME 制冷循环恒温器
过程:热电偶位于批料中间距离基底约1.5cm处。温度曲线记录为温度 - 时间曲线。
DSC
仪器:Mettler DSC 1
参数:温度 -30℃至+250℃，加热速率10 K/ min
玻璃化转变温度的确定(Tg):
半步高法，中点DIN 51007
转化率的确定:。
实施例 1:
在合适的搅拌容器中，配制由50 g Vestamin® IPD、100 g三丙酮二胺、100 gJeffamine® D230、730 g D.E.R. 351和80 g D.E.R. 731组成的批料，并在Hauschild的Speedmixer型号DAC 600.1 VAC-P中在1200-1800转/min下密切混合。随后，在30℃下用Rheotec的RC30流变仪等温测定该环氧树脂组合物的粘度升高。
此外，在23℃下测量温度升高。
此外，进行硬化筛选。为此，将5g环氧树脂组合物称入小铝盘（直径50mm）中，使样品在空气循环干燥箱中在70℃下硬化6h。然后通过DSC（机器Mettler DSC 1）测定转化率和Tg。加热速率为10K/min，从-30℃至250℃。所有结果示于表2中。
实施例 2(非本发明的)
以与实施例1中相同的方式，在合适的搅拌容器中，配制由75 g Vestamin® IPD、175g Jeffamine® D230、718 g D.E.R. 351和80 g D.E.R. 731组成的批料，并在Hauschild的Speedmixer型号DAC 600.1 VAC-P中在1200-1800转/min下密切混合。用该环氧树脂组合物以与实施例1中相同的方式进行实验以测定在30℃的粘度升高、在23℃的温度升高并进行硬化筛选。尽管该组合物显示出好的Tg发展，但是在30℃下较快达到1000毫帕·秒的粘度并因此具有较小的工艺时间窗口。也明显更快达到树脂储罐中的临界温度，这将导致浸渍工艺的过早终止。这些结果也示于表2中。
实施例3（非本发明的） 以与实施例1中相同的方式，在合适的搅拌容器中，配制由250克三丙酮二胺、720克D.E.R. 351和80g的D.E.R.731组成的批料，并在Hauschild的Speedmixer型号DAC 600.1 VAC-P中在1200-1800转/min下密切混合。用该环氧树脂组合物以与实施例1中相同的方式进行实验以测定在30℃的粘度升高、在23℃的温度升高并进行硬化筛选。尽管该组合物显示出非常宽的工艺时间窗口（在30℃下4小时后才达到1000毫帕·秒）和在树脂储罐中根本没有出现较高的温度，但是，在70℃下的固化条件下的Tg-发展是完全不令人满意的，因此，基于纯TAD的硬化剂组合物未提供符合要求的成品部件。这些结果也示于下表2中。
表 2:
Claims (16)
1.环氧树脂组合物，其包含：
A) 至少一种环氧化物化合物
和
B) 硬化剂组合物，其由下列组分构成：
B1) 5-65重量%的至少一种基于三丙酮二胺的多胺
和
B2) 35-95重量%的至少一种另外的二胺和/或多胺，
其中A)的环氧基团与B)的官能团的活性氢原子的数量的化学计量比在1:0.5至1:1范围内变化，优选1:0.6-1:1.05，特别优选1:0.95-1:1.05，
C) 任选至少一种硬化加速剂，
其中A)-C)的量合计为100重量%，
D) 任选另外的添加剂。
2.根据权利要求1的环氧树脂组合物，其特征在于，包含环氧化合物A)，所述环氧化合物A)选自饱和的、不饱和的、脂族、脂环族、芳族或杂环的环氧化合物，并且其也可具有羟基。
3.根据前述权利要求中至少一项的环氧树脂组合物，其特征在于，包含环氧化合物A)，所述环氧化合物A)选自缩水甘油基醚、缩水甘油酯、脂族环氧化物、基于双酚A和/或双酚F的二缩水甘油基醚、甲基丙烯酸缩水甘油酯。
4.根据前述权利要求中至少一项的环氧树脂组合物，其特征在于，包含环氧化合物A)，所述环氧化合物A)选自基于双酚A-二缩水甘油基醚的环氧树脂、基于双酚F-二缩水甘油基醚的环氧树脂、4,4'-亚甲基双[N,N-双(2,3-环氧丙基)苯胺]、己二醇二缩水甘油基醚、丁二醇二缩水甘油基醚、三羟甲基丙烷三缩水甘油基醚、1,2,3-丙三醇三缩水甘油基醚、季戊四醇四缩水甘油基醚、六氢邻苯二甲酸二缩水甘油酯、脂族或脂环族环氧树脂类型。
5.根据前述权利要求中至少一项的环氧树脂组合物，其特征在于，包含基于三丙酮二胺的多胺B1)，所述多胺B1)选自2,2,6,6-四甲基-4-氨基哌啶（TAD）、六亚甲基双-(4-氨基-2,2,6,6-四甲基哌啶)、N-丁基-4-氨基-2,2,6,6-四甲基哌啶、N,N-二甲基氨基丙基-4-氨基-2,2,6,6-四甲基哌啶、N-丙基-4-氨基-2,2,6,6-四甲基哌啶、N-异丙基-4-氨基-2,2,6,6-四甲基哌啶、N-羟基乙基-4-氨基-2,2,6,6-四甲基哌啶、N-甲氧基乙基-4-氨基-2,2,6,6-四甲基哌啶、N-甲氧基乙基-4-氨基-2,2,6,6-四甲基哌啶、N',N'-二甲基氨基乙基-4-氨基-2,2,6,6-四甲基哌啶、N-吗啉代乙基-4-氨基-2,2,6,6-四甲基哌啶、N-哌嗪子基乙基-4-氨基-2,2,6,6-四甲基哌啶、4-吗啉代-2,2,6,6-四甲基哌啶。
6.根据前述权利要求中至少一项的环氧树脂组合物，其特征在于，包含二胺和/或多胺B2)，所述二胺和/或多胺B2)选自伯和/或仲二胺和/或多胺。
7.根据前述权利要求中至少一项的环氧树脂组合物，其特征在于，单独地或以混合物形式使用以下胺作为组分B2)：
● 脂族胺，如多亚烷基多胺，优选选自1,2-乙二胺、1,2-丙二胺、1,3-丙二胺、1,2-丁二胺、1,3-丁二胺、1,4-丁二胺、2-(乙基氨基)乙胺、3-(甲基氨基)丙胺、二亚乙基三胺、三亚乙基四胺、五亚乙基六胺、三甲基六亚甲基二胺、2,2,4-三甲基六亚甲基二胺、2,4,4-三甲基六亚甲基二胺、2-甲基戊二胺、六亚甲基二胺、N-(2-氨基乙基)-1,2-乙二胺、N-(3-氨基丙基)-1,3-丙二胺、N,N''-1,2-乙烷二基双-(1,3-丙二胺)、二亚丙基三胺、己二酸二酰肼，肼;
● 氧基亚烷基多胺，选自多氧基亚丙基二胺和多氧基亚丙基三胺(例如Jeffamine®D-230，Jeffamine® D-400、Jeffamine® T-403、Jeffamine® T-5000)，1,13-二氨基-4,7,10-三氧杂十三烷、4,7-二氧杂癸烷-1,10-二胺;
● 脂环族胺，选自异佛尔酮二胺(3,5,5-三甲基-3-氨基甲基环己胺)、4,4'-二氨基二环己基甲烷、2,4'-二氨基二环己基甲烷和2,2'-二氨基二环己基甲烷，单独地或以异构体的混合物形式，3,3'-二甲基-4,4'-二氨基二环己基甲烷、N-环己基-1,3-丙二胺、1,2-二氨基环己烷、3-(环己基氨基)丙胺、哌嗪、N-氨基乙基哌嗪、TCD-二胺(3(4),8(9)-双(氨基甲基)三环[5.2.1.02,6]癸烷)、4-甲基环己烷-1,3-二胺
● 芳脂族胺，如二甲苯二胺;
● 芳族胺，选自苯二胺、1,3-苯二胺、1,4-苯二胺、4,4'-二氨基二苯基甲烷、2,4'-二氨基二苯基甲烷、2,2'-二氨基二苯基甲烷，单独地或以异构体的混合物形式；
● 加合物硬化剂，其是环氧化物化合物，特别是双酚A和F的缩水甘油基醚与过量胺的反应产物；
● 聚酰胺胺硬化剂，其通过单羧酸和多羧酸与多胺的缩合获得，特别是通过二聚脂肪酸与多亚烷基多胺的缩合获得;
● 曼尼希碱硬化剂，其通过一元或多元酚与醛，特别是甲醛，和多胺的反应获得;
● 曼尼希碱，例如基于苯酚和/或间苯二酚，甲醛和间二甲苯二胺以及N-氨基乙基哌嗪，和由N-氨基乙基哌嗪与壬基苯酚和/或苄醇构成的混合物，在由腰果酚类、醛和胺的曼尼希反应中获得的酚醛胺。
8.根据前述权利要求中至少一项的环氧树脂组合物，其特征在于，包含二胺和/或多胺B2)，所述二胺和/或多胺B2)选自异佛尔酮二胺、4,4'-二氨基二环己基甲烷、2,4'-二氨基二环己基甲烷、2,2'-二氨基二环己基甲烷(PACM)，单独地或以异构体的混合物形式，选自多氧基亚丙基二胺和多氧基亚丙基三胺的氧基亚烷基多胺，基于环氧化物化合物和前述胺B2)或前述胺B2)的组合的反应产物的加合物硬化剂。
9.根据前述权利要求中至少一项的环氧树脂组合物，其特征在于，
作为组分B2)，使用
异佛尔酮二胺（3,5,5-三甲基-3-氨基甲基环己胺，IPD）， 和/或由异佛尔酮二胺和/或PACM和多氧基亚丙基二胺和/或多氧基亚丙基三胺构成的组合， 和/或基于环氧化物化合物与上述胺B2)或上述胺B2)的组合的反应产物的加合物硬化剂。
10.根据前述权利要求中至少一项的环氧树脂组合物，其特征在于，
作为组分B2)，使用
a) 异佛尔酮二胺，
b) 和/或异佛尔酮二胺与多氧基亚丙基二胺和/或多氧基亚丙基三胺的组合，
c) 和/或基于环氧化物化合物与上述胺B2)或上述胺B2)的组合的反应产物的加合物硬化剂。
11.根据前述权利要求中至少一项的环氧树脂组合物，其特征在于，包含叔胺作为硬化加速剂C)。
12.根据前述权利要求中至少一项的环氧树脂组合物用于制造复合材料的用途，所述组合物包含：
A) 至少一种环氧化物化合物
和
B) 硬化剂组合物，其由下列组分构成：
B1) 5-65重量%的至少一种基于三丙酮二胺的多胺
和
B2) 35-95重量%的至少一种另外的二胺和/或多胺，
其中A)的环氧基团与B)的官能团的活性氢原子的数量的化学计量比在1:0.5至1:1范围内变化，优选1:0.6-1:1.05，特别优选1:0.95-1:1.05，
C) 任选至少一种硬化加速剂，
其中A)-C)的量合计为100重量%，
D) 任选另外的添加剂。
13.复合材料部件，
其基本上由下述构成
1) 至少一种纤维状载体和任选的芯材料
和
2) 根据前述权利要求1-10中至少一项的环氧树脂组合物，其包含：
A) 至少一种环氧化物化合物
和
B) 硬化剂组合物，其由下列组分构成：
B1) 5-65重量%至少一种基于三丙酮二胺的多胺
和
B2) 35-95重量%至少一种另外的二胺和/或多胺，
其中A)的环氧基团与B)的官能团的活性氢原子的数量的化学计量比在1:0.5至1:1范围内变化，优选1:0.6-1:1.05，特别优选1:0.95-1:1.05，
C) 任选至少一种硬化加速剂，
其中A)-C)的量合计为100重量%，
D) 任选另外的添加剂。
14.通过下述方法步骤制造根据权利要求13中所述的复合材料的方法：
I. 提供反应性组合物，其包含
A) 至少一种环氧化物化合物
和
B) 硬化剂组合物，其由下列组分构成：
B1) 5-65重量%的至少一种基于三丙酮二胺的多胺
和
B2) 35-95重量%的至少一种另外的二胺和/或多胺，
其中A)的环氧基团与B)的官能团的活性氢原子的数量的化学计量比在1:0.5至1:1范围内变化，优选1:0.6-1:1.05，特别优选1:0.95-1:1.05，
C) 任选至少一种硬化加速剂，
其中A)-C)的量合计为100重量%，
D) 任选另外的添加剂；
II. 根据液体树脂浸渍法在模型中或模具中用得自I的组合物浸渍由纤维状载体和任选的其它芯材料构成的结构，或者浸渍纤维状载体并缠绕在芯轴上，
III. 使所述反应性组合物硬化成复合材料部件和
IV. 将制成的部件从模型中脱模。
15.根据权利要求13-14的复合材料在船舶制造中、航空航天技术中、汽车制造中，用于两轮车辆，优选摩托车和自行车，在汽车工业、建筑结构、医疗技术、运动、电气和电子工业、发电设备的领域中的用途。
16.根据权利要求13-14的复合材料在制造风力涡轮机的转子叶片中的用途。
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| PL3178862T3 (pl) * | 2015-12-11 | 2020-04-30 | Evonik Degussa Gmbh | Utajone formulacje żywic epoksydowych do ciekłego impregnowania kompozytów wzmocnionych włóknami |
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- 2016-12-09 JP JP2016239397A patent/JP2017115134A/ja active Pending
- 2016-12-09 CN CN201611128605.4A patent/CN106947061A/zh active Pending
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| CN108239507A (zh) * | 2016-12-23 | 2018-07-03 | 赢创德固赛有限公司 | 用于结构粘合剂的固化剂制剂中作为构成单元的apcha |
| CN108239507B (zh) * | 2016-12-23 | 2021-11-02 | 赢创运营有限公司 | 用于结构粘合剂的固化剂制剂中作为构成单元的apcha |
| CN109467942A (zh) * | 2017-09-07 | 2019-03-15 | 信越化学工业株式会社 | 树脂组合物、树脂膜、半导体层叠体、半导体层叠体的制造方法及半导体装置的制造方法 |
| CN109467942B (zh) * | 2017-09-07 | 2022-02-11 | 信越化学工业株式会社 | 树脂组合物、树脂膜、半导体层叠体、半导体层叠体的制造方法及半导体装置的制造方法 |
| CN114990925A (zh) * | 2021-03-02 | 2022-09-02 | 中国制浆造纸研究院有限公司 | 一种耐热助剂的制备方法 |
| CN114990925B (zh) * | 2021-03-02 | 2023-06-16 | 中国制浆造纸研究院有限公司 | 一种耐热助剂的制备方法 |
| CN114150534A (zh) * | 2021-12-14 | 2022-03-08 | 湖南红四方新材料有限公司 | 一种用于胶粘作用胶膜纸的生产制备方法 |
| CN114150528A (zh) * | 2021-12-14 | 2022-03-08 | 湖南红四方新材料有限公司 | 一种集装箱地板高耐磨表面覆膜纸的制备方法 |
| CN115181521A (zh) * | 2022-07-19 | 2022-10-14 | 山东省公路桥梁建设集团有限公司 | 体外预应力钢结构注胶粘贴工艺 |
Also Published As
| Publication number | Publication date |
|---|---|
| TW201734081A (zh) | 2017-10-01 |
| BR102016028902A2 (pt) | 2017-06-20 |
| US20180162991A1 (en) | 2018-06-14 |
| US10280252B2 (en) | 2019-05-07 |
| MX2016015904A (es) | 2017-06-12 |
| CA2951253A1 (en) | 2017-06-11 |
| KR20170069948A (ko) | 2017-06-21 |
| ES2750306T3 (es) | 2020-03-25 |
| EP3178861B1 (de) | 2019-08-28 |
| EP3178861A1 (de) | 2017-06-14 |
| JP2017115134A (ja) | 2017-06-29 |
| ES2750306T8 (es) | 2020-06-24 |
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