CN107109063A - 包含聚酰胺和聚硅氧烷的热塑性组合物 - Google Patents
包含聚酰胺和聚硅氧烷的热塑性组合物 Download PDFInfo
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- CN107109063A CN107109063A CN201580069438.8A CN201580069438A CN107109063A CN 107109063 A CN107109063 A CN 107109063A CN 201580069438 A CN201580069438 A CN 201580069438A CN 107109063 A CN107109063 A CN 107109063A
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- Prior art keywords
- hotmelt
- thermoplastic compounds
- polyamide
- weight
- silane
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- -1 polysiloxanes Polymers 0.000 title claims abstract description 109
- 150000001875 compounds Chemical class 0.000 title claims abstract description 68
- 229920001169 thermoplastic Polymers 0.000 title claims abstract description 49
- 229920002647 polyamide Polymers 0.000 title claims abstract description 47
- 239000004952 Polyamide Substances 0.000 title claims abstract description 45
- 239000004416 thermosoftening plastic Substances 0.000 title claims abstract description 43
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 32
- 239000000203 mixture Substances 0.000 claims abstract description 42
- 239000012943 hotmelt Substances 0.000 claims abstract description 40
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000000853 adhesive Substances 0.000 claims abstract description 8
- 230000001070 adhesive effect Effects 0.000 claims abstract description 8
- 241001074085 Scophthalmus aquosus Species 0.000 claims abstract description 4
- 239000008393 encapsulating agent Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000013019 agitation Methods 0.000 claims abstract description 3
- 239000003607 modifier Substances 0.000 claims abstract description 3
- 229910000077 silane Inorganic materials 0.000 claims description 52
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 51
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 20
- 239000003381 stabilizer Substances 0.000 claims description 18
- 239000000945 filler Substances 0.000 claims description 14
- 239000004014 plasticizer Substances 0.000 claims description 11
- 239000000654 additive Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 230000000996 additive effect Effects 0.000 claims description 9
- 229920002554 vinyl polymer Polymers 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 8
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 8
- 239000003431 cross linking reagent Substances 0.000 claims description 7
- WHIVNJATOVLWBW-UHFFFAOYSA-N n-butan-2-ylidenehydroxylamine Chemical compound CCC(C)=NO WHIVNJATOVLWBW-UHFFFAOYSA-N 0.000 claims description 6
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical group [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 abstract description 13
- 239000006254 rheological additive Substances 0.000 abstract description 4
- 239000002585 base Substances 0.000 description 28
- 239000002253 acid Substances 0.000 description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 21
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- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 17
- 239000004831 Hot glue Substances 0.000 description 16
- 150000001412 amines Chemical class 0.000 description 15
- 235000014113 dietary fatty acids Nutrition 0.000 description 15
- 239000000194 fatty acid Substances 0.000 description 15
- 229930195729 fatty acid Natural products 0.000 description 15
- 150000004665 fatty acids Chemical class 0.000 description 15
- 229920005573 silicon-containing polymer Polymers 0.000 description 14
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- 125000003118 aryl group Chemical group 0.000 description 9
- 125000000217 alkyl group Chemical group 0.000 description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 8
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 8
- 150000001991 dicarboxylic acids Chemical class 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 125000004169 (C1-C6) alkyl group Chemical group 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 6
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 5
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical group OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 4
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 description 4
- 125000001931 aliphatic group Chemical group 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- 125000001891 dimethoxy group Chemical group [H]C([H])([H])O* 0.000 description 4
- 238000005227 gel permeation chromatography Methods 0.000 description 4
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- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 4
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- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 3
- SJRJJKPEHAURKC-UHFFFAOYSA-N N-Methylmorpholine Chemical compound CN1CCOCC1 SJRJJKPEHAURKC-UHFFFAOYSA-N 0.000 description 3
- NEAPKZHDYMQZCB-UHFFFAOYSA-N N-[2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]ethyl]-2-oxo-3H-1,3-benzoxazole-6-carboxamide Chemical compound C1CN(CCN1CCNC(=O)C2=CC3=C(C=C2)NC(=O)O3)C4=CN=C(N=C4)NC5CC6=CC=CC=C6C5 NEAPKZHDYMQZCB-UHFFFAOYSA-N 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- 125000004103 aminoalkyl group Chemical group 0.000 description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 230000000977 initiatory effect Effects 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
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- 239000000047 product Substances 0.000 description 3
- IVHXEBVFCNBWED-UHFFFAOYSA-N prop-1-en-2-yloxysilane Chemical compound CC(=C)O[SiH3] IVHXEBVFCNBWED-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 description 2
- YBYIRNPNPLQARY-UHFFFAOYSA-N 1H-indene Chemical compound C1=CC=C2CC=CC2=C1 YBYIRNPNPLQARY-UHFFFAOYSA-N 0.000 description 2
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 description 2
- IMSODMZESSGVBE-UHFFFAOYSA-N 2-Oxazoline Chemical compound C1CN=CO1 IMSODMZESSGVBE-UHFFFAOYSA-N 0.000 description 2
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
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- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 2
- PWLXTFFHCFWCGG-UHFFFAOYSA-N Heneicosanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCCCCCCCCC(O)=O PWLXTFFHCFWCGG-UHFFFAOYSA-N 0.000 description 2
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- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 2
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- IHEDBVUTTQXGSJ-UHFFFAOYSA-M 2-[bis(2-oxidoethyl)amino]ethanolate;titanium(4+);hydroxide Chemical class [OH-].[Ti+4].[O-]CCN(CC[O-])CC[O-] IHEDBVUTTQXGSJ-UHFFFAOYSA-M 0.000 description 1
- GOJUJUVQIVIZAV-UHFFFAOYSA-N 2-amino-4,6-dichloropyrimidine-5-carbaldehyde Chemical group NC1=NC(Cl)=C(C=O)C(Cl)=N1 GOJUJUVQIVIZAV-UHFFFAOYSA-N 0.000 description 1
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 1
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- IRTCJFCIQKNFPP-UHFFFAOYSA-N 2-methyl-1,4-dioxane Chemical compound CC1COCCO1 IRTCJFCIQKNFPP-UHFFFAOYSA-N 0.000 description 1
- 125000004493 2-methylbut-1-yl group Chemical group CC(C*)CC 0.000 description 1
- JZUHIOJYCPIVLQ-UHFFFAOYSA-N 2-methylpentane-1,5-diamine Chemical compound NCC(C)CCCN JZUHIOJYCPIVLQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种热塑性组合物,其包含至少一种优选具有小于185℃的熔点的聚酰胺和至少一种在25℃下优选具有750‑100,000mPas的粘度并且是OH封端的液体聚硅氧烷化合物,其中所述热塑性组合物可通过包括以下步骤的方法得到:1a)加热所述至少一种聚酰胺至高于该至少一种聚酰胺的熔点并且优选低于185℃的温度;2a)在搅拌下向步骤1a)的加热的化合物中加入所述至少一种液体聚硅氧烷化合物,其中所述温度保持在高于所述至少一种聚酰胺的熔点并且优选低于185℃;以及3a)优选在80‑180℃下,更优选在110‑140℃下将步骤2a)得到的混合物混合。根据本发明所述的热塑性组合物在密封剂中,在粘合剂中或作为流变改性剂或表面改性剂中的用途。此外,本发明涉及包含根据本发明所述的热塑性组合物的热熔粘合剂。以及这种热熔体在车辆部件、结构、窗户、玻璃窗、卫生应用、配件、屋顶、管道、设备应用和窗格粘合中的用途。
Description
本发明涉及包含至少一种聚酰胺和至少一种液体聚硅氧烷化合物的热塑性组合物,其可以通过如下定义的具体方法得到。此外,本发明涉及这种热塑性组合物在密封剂、粘合剂或流变改性剂或表面改性剂中的用途。此外,包括特定热塑性组合物的热熔粘合剂以及这种热熔粘合剂在车辆部件、结构、窗户、玻璃窗、卫生应用、配件、屋顶、管道、设备应用和窗格粘合中的用途也是本发明的一部分。
普通有机硅密封剂在有机硅密封剂固化之前无法将基底保持密封在一起。为了确保使用有机硅密封剂的更精确的密封,本发明的目的是提供一种粘合剂,其具有普通有机硅密封剂的特性,但是另外具有在固化前能够保持基底粘合在一起的能力。
本发明人出人意料地发现,通过本发明的特定热塑性组合物,可以获得热熔粘合剂,其显示出标准有机硅密封剂的特性,并具有标准热熔体的高初始强度。
特别地,本发明涉及:
一种热塑性组合物,其包含至少一种优选具有小于185℃的熔点的聚酰胺,和至少一种在25℃下优选具有750-100,000mPa.s的粘度并且是OH封端的液体聚硅氧烷化合物,其中所述热塑性组合物可通过包括以下步骤的方法获得:
1a)将所述至少一种聚酰胺加热到高于该至少一种聚酰胺的熔点并且优选低于185℃的温度;
2a)在搅拌下加入所述至少一种液体聚硅氧烷至步骤1a)的加热的化合物中,其中所述温度保持在高于所述至少一种聚酰胺的熔点,并且优选低于185℃;以及
3a)将步骤2a)得到的混合物优选在80℃-180℃,更优选110-140℃下混合。
根据本发明的热塑性组合物在密封剂中,在粘合剂中,或作为流变改性剂或表面改性剂的用途。
一种包含根据本发明的热塑性组合物的热熔粘合剂。
根据本发明的热熔粘合剂在车辆部件、结构、窗户、玻璃窗、卫生应用、配件、屋顶、管道、设备应用和窗格粘合中的用途。
在权利要求中阐述更优选的实施方案。
在本说明书中,术语“一个”和“至少一个”与术语“一个或多个”相同,并且可以互换使用。
除非另有说明,在本发明中采用下述“实施例和测量方法”部分中描述的测量方法。
聚酰胺可以由不同的单体制备。优选地,选择分子量使得获得可以在低于250℃的温度下作为熔体加工的聚酰胺。可通过采用酸组分和二元胺组分作为起始原料得到聚酰胺,其中酸组分可以选自二羧酸和聚合羧酸或其组合,并且也可以进一步包含三元羧酸。聚酰胺及其制备通常是本领域技术人员已知的。优选采用酸封端的聚酰胺,更优选直链酸封端的聚酰胺。
适合的二元羧酸的实例包括C4-C60二元羧酸,特别是己二酸、壬二酸、琥珀酸、十二烷二酸、戊二酸、辛二酸、马来酸、庚二酸、癸二酸、十一烷二酸或芳族二羧酸,例如对苯二甲酸、邻苯二甲酸、间苯二甲酸或这些二羧酸的混合物。二元羧酸是本领域公知的并且是可商购的。聚合脂肪酸也是适合的。聚合脂肪酸,有时在文献中称为“二聚酸”,是由脂肪酸的聚合形成的复杂混合物。这些聚合脂肪酸是通过连接不饱和长链一元脂肪酸例如亚麻酸或油酸得到的。也可以使用聚合脂肪酸的混合物,聚合脂肪酸的混合物是从妥尔油脂肪酸的聚合得到的可商购获得的那些。这些聚合脂肪酸优选具有以下典型组成:基于组合物的总重量,约0-5重量%的C18一元酸(单体),60-95重量%、有时高达约98重量%的C36二元酸(二聚体),约1-35重量%的C54和更高级的多元酸(三聚体)。聚合脂肪酸中单体、二聚体和三聚体的相对比例取决于起始原料的性质、聚合的条件和纯化的程度。更纯级别的聚合脂肪酸可以通过蒸馏得到并且包含至少70重量%,优选80重量%并且通常高达95重量%或甚至98重量%的二聚脂肪酸。聚合脂肪酸可以是未氢化的或氢化的。
作为次要成分,也可以使用一元羧酸或三元羧酸,但优选避免交联的聚酰胺。除了聚合脂肪酸之外,酸组分还可以包含C4-C12二元羧酸。
在优选的实施方案中聚酰胺的羧酸组分可以包含约20-99mol%的聚合脂肪酸和约1-80mol%的至少一种C4-C12二元羧酸,优选这种混合物包含约30-95mol%的聚合脂肪酸和约5-70mol%的C4-C12二元羧酸。
二元胺组分优选选自一种或多种脂肪族二元胺,更优选具有偶数个碳原子,其中胺基优选位于碳链的末端。脂肪族二元胺可以包含2-20个碳原子,其中碳链可以是线性的或轻微支化的。具体的实例有1,2-乙二胺、1,3-二氨基丙烷、二亚乙基三胺、二亚丙基三胺、1,4-二氨基丁烷、1,3-二氨基戊烷、甲基戊二胺、1,6-己二胺、三甲基己二胺、2-(2-氨基甲氧基)乙醇、2-甲基戊二胺、1,8-二氨基辛烷、新戊二胺、二氨基二丙基甲胺、1,12-二氨基十二烷。特别优选的脂肪族二胺是具有偶数个碳原子的C4-C12二元胺。另一组二元胺衍生自如上所述的聚合脂肪酸,其包含伯氨基而不是羧基。
二元胺组分也可以包含环状二胺或杂环二胺例如,1,4-环己二胺、4,4'-二氨基-二环己基甲烷、哌嗪、环己烷-双-(甲胺)、异佛尔酮二胺、二甲基哌嗪、二哌啶基丙烷、降冰片烷二胺、间苯二甲胺或其混合物。这种环状二胺的数均分子量优选为80g/mol-约300g/mol。另外,氨基组分可以包含聚氧化亚烷基二胺,例如聚氧化亚乙基二胺、聚氧化亚丙基二胺或双-(二氨基丙基)-聚四氢呋喃。聚氧化亚烷基二胺是可以商品名“Jeffamines”(Huntsman Co.)商购的。基于二元胺组分的总量,它们的数均分子量优选为200-4,000g/mol,更优选为400-2,000g/mol。通过GPC以聚苯乙烯为参照测量二元胺组分的数均分子量。
二元胺组分优选包含20-85mol%的偶数脂肪族二元胺和0-70mol%的环状二胺和0-60mol%的聚氧化亚烷基二胺,其中至少一种环状二胺或聚氧化亚烷基二胺存在于胺组分混合物中。
根据本发明的聚酰胺树脂可以通过常规的缩聚方法制备,并且起始原料的酸基团与胺基团以近似化学计量的量存在。在大多数情况下,优选在缩聚后存在残余酸基或残余氨基,更优选残余酸基。为了实现这个目的,使用的原料中具有不超过所有官能团的10当量%的过量酸基或胺基。除了游离羧酸,在缩聚反应中也可以使用其相应的甲基酯、乙基酯或丙基酯代替游离羧酸。聚酰胺组合物的熔融粘度可以通过加入少量的单官能羧酸例如硬脂酸来控制。
聚酰胺可以另外包含至多10mol%的具有5-18个碳原子的氨基羧酸或其环状衍生物。这种组分的实例包括6-氨基己酸,11-氨基十一烷酸,ω-月桂内酰胺和ε-己内酰胺。
当选择单官能、双官能或三官能的原材料作为单体时,应当选择其用量使得应该得到优选可熔融例如未交联的聚酰胺。例如,如果发生交联/凝胶,那么降低三官能组分的部分和/或增加单官能胺或脂肪酸的含量可以导致聚合物不容易凝胶。
EP 749 463 A中描述了基于二元羧酸和聚醚二胺的适合的聚酰胺的实例。EP 204315 A中公开了基于二聚脂肪酸和多胺的另一种类型的适合的聚酰胺。
例如,其它有用的聚酰胺是基于包含聚醚二胺的不含二聚脂肪酸的聚酰胺。它们可以由40-50mol%、优选50mol%的一种或多种C4-C18二元羧酸,5-45mol%、优选15-40mol%的至少一种脂肪族二胺,5-40mol%、优选20-30mol%的一种或多种脂环族二胺,0-40mol%、优选5-25mol%的聚醚二胺来制备,其中所加入的二胺的总量和二元羧酸的总量均为50mol%,使得二元羧酸组分和二元胺组分以大致相等的摩尔分数存在。在每种情况下,所有羧酸的总和和所有胺的总和应当相加为100mol%。
根据本发明的所述至少一种聚酰胺优选具有小于185℃,更优选为10-180℃,最优选为30-170℃的熔点。此外,软化点优选为50-200℃,更优选为60-150℃,最优选为70-90℃。粘度在80℃下优选为250-100,000mPa.s,在80℃下更优选为500-50,000mPa.s,在80℃下最优选为1,000-20,000mPa.s。
如果在热塑性组合物中包含多于一种聚酰胺,那么在步骤1a)中的温度应当高于具有较高熔点的聚酰胺的熔点。例如,如果热塑性组合物包含熔点为100℃的聚酰胺和熔点为120℃的第二种聚酰胺,那么在步骤1a)中的温度应当高于120℃。
基于热塑性组合物的总重量,所述至少一种聚酰胺的量优选为25-70重量%,更优选为30-60重量%,最优选为40-55重量%。
液体聚硅氧烷化合物在25℃下优选具有750-100,000mPa.s的粘度。更优选其为羟基封端的二有机聚硅氧烷化合物并在25℃下具有750-100,000mPa.s的粘度。
液体聚硅氧烷优选为二有机聚硅氧烷,其中更优选有机基团选自甲基、乙基、丙基、苯基和乙烯基或其组合。例如,二有机聚硅氧烷可以以非限制性的方式选自,聚二甲基硅氧烷,乙基甲基聚硅氧烷,烷基二甲基聚硅氧烷,聚苯甲基硅氧烷例如苯基聚二甲基硅氧烷、苯基聚三甲基硅氧烷和乙烯基甲基聚甲基硅氧烷,二甲基硅氧烷和甲基乙烯基硅氧烷的共聚物,以及这些聚合物和共聚物的混合物,其优选为羟基封端的。在优选的实施方案中,二有机聚硅氧烷是线性的。在更优选的实施方案中,二有机聚硅氧烷是聚二甲基硅氧烷,最优选为OH封端的。
在本发明的优选实施方案中,液体聚硅氧烷化合物的数均分子量为500-800,000g/mol,更优选为5,000-700,000g/mol,以及最优选为50,000-600,000g/mol。
液体聚硅氧烷化合物的示例性化合物具有式(I):
其中:
R1-R6独立地选自取代的或未取代的烷基、乙烯基、或芳基,更优选选自未取代的C1-C6烷基,最优选R1-R6是CH3;
X是羟基或NCO基,更优选X是羟基;以及
n和m为整数并且至少是1,更优选n+m之和至少是10,最优选n+m是10-3000,或者选择n和m使得式(I)的化合物的分子量为约14,000-84,000g/mol,更优选30,000-65,000g/mol,最优选为40,000-60,000g/mol。
在优选的实施方案中,式(I)中的R1-R6是甲基并且X是羟基。在进一步优选的实施方案中,R1-R6是甲基,X是羟基并且选择n和m使得式(I)的化合物的数均分子量为约14,000-84,000g/mol,更优选为30,000-65,000g/mol,最优选为40,000-60,000g/mol。
可以在式(I)中使用的示例性的取代的和未取代的烷基、乙烯基和芳基如下式(II)所述。
热塑性组合物可任选地包含至少一种稳定剂,所述稳定剂进一步在步骤2a)中加入。
根据本发明的稳定剂优选选自具有至少一个官能团的功能性二有机聚硅氧烷,其中所述官能团选自环氧、酸酐、硅烷醇、羧基、胺、噁唑啉或烷氧基或其组合。功能性二有机聚硅氧烷具有的数均分子量为至少700,优选700-60,000,更优选800-30,000g/mol。
根据本发明的稳定剂的实例包括环氧官能聚二甲基硅氧烷,例如单(2,3-环氧)丙基醚封端的聚二甲基硅氧烷、环氧丙氧基丙基封端的聚二甲基硅氧烷、(环氧环己基乙基)甲基硅氧烷二甲基硅氧烷共聚物、和(环氧丙氧基丙基)甲基硅氧烷二甲基硅氧烷共聚物;胺官能硅氧烷,例如氨丙基封端的聚二甲基硅氧烷、氨乙基氨丙基封端的聚二甲基硅氧烷、氨丙基接枝的聚二甲基硅氧烷、氨乙基氨丙基接枝的聚二甲基硅氧烷;包含酸酐基团的聚二甲基硅氧烷例如琥珀酸酐封端的聚二甲基硅氧烷和琥珀酸酐接枝的聚二甲基硅氧烷;硅烷醇封端的聚二甲基硅氧烷;包含羧基的聚二甲基硅氧烷,例如(单)羧基癸基封端的聚二甲基硅氧烷和羧基癸基封端的聚二甲基硅氧烷;和包含噁唑啉基团的聚二甲基硅氧烷,例如乙烯基噁唑啉接枝的聚二甲基硅氧烷.
在最优选的实施方案中,所述稳定剂是具有式(II)的氨基官能硅氧烷:
其中
每个R7是独立地选自取代的或未取代的C1-C6烷基和芳基,优选选自未取代的C1-C6烷基,更优选选自甲基或丙基,更优选R7是甲基;
每个R8独立地选自羟基、烷基、芳基乙烯基和苯基,优选为羟基或C1-C6烷基,最优选R8是羟基;以及
p是100-2,000的整数或选择以使得式(II)的化合物的数均分子量为400-20,000g/mol,优选为600-10,000g/mol,更优选为1,000-7,500g/mol;
以及R9独立地选自-R10-NH-R11、C1-C6烷基或H,前提条件为存在至少一个-R10-NH-R11,优选地所述至少一个-R10-NH-R11是氨基丙基,更优选存在5-30个、更优选存在7-15个-R10-NH-R11,其最优选为氨基丙基;
R10独立地选自C1-C6烷基或C1-C6烷氧基,优选R10独立地选自C1-C6烷基;
以及R11独立地选自氢、氨基烷基、氨基烯基、氨基芳基和氨基环烷基,优选R11是氢。
如本文所用,术语“独立地选自”表示分子中的每个R基团可以相同或不同。例如,式(II)的化合物中的每个R9对于p个[R7-SiR9-O]单元中的每一个都可以是不同的。优选存在三种不同类型的[R7-SiR9-O]单元,更优选存在两种不同类型的[R7-SiR9-O]单元。
如本文所用,术语“烷基”单独或组合表示可以被取代的直链和支链的饱和烃基,其含有1-10个碳原子,优选1-8个碳原子,更优选1-6个碳原子原子。这种基团的实例包括甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、2-甲基丁基、戊基、异戊基、己基、3-甲基戊基、辛基、2-乙基己基等。优选的取代基是F和苯基。在更优选的实施方案中“烷基”是未取代的。
如本文所用,术语“烯基”单独或组合定义为可以被取代的直链和支链烃基,其含有2-约18个碳原子,优选2-8个碳原子,更优选2-6个碳原子并包含至少一个双键,例如乙烯基、丙烯基、丁烯基、戊烯基、和己烯基。优选的取代基是F和苯基。在更优选的实施方案中,“烯基”是未取代的。
术语“亚烯基”单独或组合地定义为含有2-约18个碳原子,优选2-8个碳原子,更优选2-6个碳原子,并含有至少一个双键的直链和支链二价烃基,例如,亚乙烯基、亚丙烯基、亚丁烯基、亚戊烯基和亚己烯基。
术语“烷氧基”或“烷基氧基”单独或组合是指烷基醚基团,其中术语烷基如上所定义。优选的烷基醚基团包括甲氧基、乙氧基、正丙氧基、异丙氧基、正丁氧基、异丁氧基、仲丁氧基、叔丁氧基和己氧基。
术语“芳基”单独或组合是指含有6-18个,优选6-10个环碳原子的环状、双环或三环的芳香族基团,其中环状芳香族基团可以被F或苯基取代并且可以任选地包含杂原子例如N、S或O,前提条件为芳基是芳香族的。在优选的实施方案中芳基是未取代的并且不包含杂原子。
术语“乙烯基”是指未取代的或被F或苯基取代的乙烯基。在优选的实施方案中,乙烯基是未取代的。
术语“氨基烷基、氨基烯基、氨基芳基和氨基环烷基”包括氨基和如上定义“烷基”的烷基。
在优选的实施方案中,基于热塑性组合物的总重量,稳定剂以0.1-15重量%,更优选0.3-10重量%,最优选0.5-5重量%的量存在。在更优选的实施方案中,该稳定剂是氨基官能硅氧烷,最优选的是根据式(II)的氨基官能硅氧烷。
根据本发明的热塑性组合物可以用于密封剂、粘合剂,或用作流变改性剂或表面改性剂。
此外,本发明涉及包含根据本发明的热塑性组合物的热熔粘合剂。热熔粘合剂可以优选另外包含填料。在更优选的实施方案中热熔粘合剂另外地包含填料和添加剂。热熔粘合剂可以是非反应性热熔粘合剂,或另外包含交联剂并因此是反应性热熔粘合剂。
当在根据本发明的热熔胶中使用交联剂以得到反应性热熔胶时,所述交联剂优选选自正硅酸乙酯(TEOS)、TEOS缩聚物、甲基三甲氧基硅烷(MTMS)、乙烯基-三甲氧基硅烷、甲基乙烯基二甲氧基硅烷、二甲基二乙氧基硅烷、乙烯基三乙氧基硅烷、原硅酸四正丙酯、乙烯基三(甲基乙基酮肟)硅烷、甲基三(甲基乙基酮肟)硅烷、甲基三(甲基甲基酮肟)硅烷、三乙酰氨基甲基硅烷、双乙酰氨基二甲基硅烷、三(N-甲基乙酰氨基)甲基硅烷、双(N-甲基乙酰氨基)二甲基硅烷、(N-甲基乙酰胺基)甲基二烷氧基硅烷、三苯甲酰胺基甲基硅烷、三丙氧基甲基硅烷、烷基二烷氧基酰胺基硅烷、烷基烷氧基双酰胺基硅烷、(CH3Si(OC2H5)(CH3COC6H5)2、CH3Si(OC2H5)-(HCOC6H5)2、甲基二甲氧基(乙基甲基酮肟基)硅烷;甲基甲氧基双(乙基甲基酮肟)硅烷;甲基二甲氧基(缩醛-肟基)硅烷;甲基二甲氧基(甲基氨基甲酸酯基)硅烷;乙基二甲氧基(N-甲基-氨基甲酸酯基)硅烷;甲基二甲氧基异丙烯氧基硅烷;三甲氧基异丙烯氧基硅烷;甲基三异丙烯氧基硅烷;甲基二甲氧基(丁-2-烯-2-氧基)硅烷;甲基二甲氧基(1-苯基乙烯氧基)硅烷;甲基二甲氧基-2(1-乙氧羰基丙烯氧基)硅烷;甲基甲氧基二-N-甲基氨基硅烷;乙烯基二甲氧基甲基氨基硅烷;四-N,N-二乙基氨基硅烷;甲基二甲氧基甲基氨基硅烷;甲基三环己基氨基硅烷;甲基二甲氧基-乙基氨基硅烷;二甲基二-N,N-二甲基氨基硅烷;甲基二甲氧基异丙基氨基硅烷;二甲基二-N,N-二乙基氨基硅烷;乙基二甲氧基(N-乙基丙酰氨基)硅烷;甲基二甲氧基(N-甲基乙酰氨基)硅烷;甲基三(甲基乙酰氨基)硅烷;乙基二甲氧基(N-甲基乙酰氨基)硅烷;甲基三(甲基苯甲酰氨基)硅烷;甲基甲氧基双(N-甲基乙酰氨基)硅烷;甲基二甲氧基(己内酰胺)硅烷;三甲氧基(N-甲基乙酰氨基)硅烷;甲基二甲氧基乙基乙酰亚胺基硅烷;甲基二甲氧基-丙基乙酰亚胺基硅烷;甲基二甲氧基(N',N'-三甲基脲基)硅烷;甲基二甲氧基(N-烯丙基-N',N'-二甲基脲基)硅烷;甲基二甲氧基(N-苯基-N',N'-二甲基脲基)硅烷;甲基二甲氧基异氰酸酯基硅烷;二甲氧基二异氰酸酯硅烷;甲基二甲氧基-硫代异氰酸酯基硅烷;甲基甲氧基二硫代异氰酸酯基硅烷、四甲氧基硅烷、四乙氧基硅烷、四丙氧基硅烷、四丁氧基硅烷、甲基三甲氧基硅烷、甲基三乙氧基硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、苯基三甲氧基硅烷、苯基三乙氧基硅烷、3-氰基丙基三甲氧基硅烷、3-氰基丙基三乙氧基硅烷、3-(缩水甘油氧基)丙基三乙氧基硅烷、1,2-双(三甲氧基甲硅烷基)乙烷、环己基氨基乙基三乙氧基硅烷、吗啉基甲基三甲氧基硅烷、1,2-二(三乙氧基甲硅烷基)乙烷甲基三(甲基乙基酮肟基)硅烷、乙烯基三(甲基乙基酮肟基)硅烷、甲基三(乙酰异肟基)硅烷、乙基三(丙酮肟基)硅烷、乙烯基三(丙酮肟基)硅烷、苯基三(丙酮肟基)硅烷、四(甲基乙基酮肟)硅烷、甲基三乙酰氧基硅烷、乙基三乙酰氧基硅烷、乙烯基三乙酰氧基硅烷、二甲基二乙酰氧基硅烷、甲基乙烯基二乙酰氧基硅烷或其两种或多种的组合。
根据本发明的填料的实例是优选具有至少30m2/g的BET表面积的增强填料,例如炭黑、热解二氧化硅、沉淀二氧化硅、硅胶和硅铝混合氧化物。或者,所述填料可以是疏水化的,即其可以部分或全部用有机硅烷或硅氧烷处理以使它们具有较少的亲水并降低水含量或控制组合物的粘度和储存稳定性。这种化合物的商品名有Aerosil(R),HDK(R),Cab-O-Sil(R)等。另外根据本发明,还有优选具有小于30m2/g的BET表面积的非增强填料,例如粉碎和研磨的石英、石英粉、方石英、硅藻土、硅酸钙、硅酸锆、石墨或粘土例如高岭土、膨润土、蒙脱石(处理的/未处理的)、沸石,包括分子筛,例如硅酸铝钠、金属氧化物如氧化铝、二氧化钛、铁氧化物和锌氧化物和它们的混合氧化物、金属氢氧化物例如氢氧化铝、硫酸钡、碳酸钙、石膏、氮化硅、碳化硅、氮化硼、玻璃粉、碳粉、和聚合物粉末如丙烯腈、聚乙烯、聚丙烯、聚四氟乙烯、中空玻璃和塑料珠。在优选的实施方案中,填料选自上述包含硅原子的化合物。更优选的是粉碎和研磨的石英、石英粉、方英石、硅酸盐、热解二氧化硅、沉淀二氧化硅、硅胶和硅酸锆,最优选的填料是硅酸盐。根据DIN ISO 9277:2003-05测定BET表面积。
基于热熔粘合剂的总重量,根据本发明的热熔粘合剂组合物优选包含20-80重量%的根据本发明的热塑性组合物。在更优选的实施方案中包含30-70重量%,最优选45-60重量%的根据本发明的热塑性组合物。
基于热熔粘合剂的总重量,根据本发明的热熔粘合剂包含20-60重量%的至少一种填料。在更优选的实施方案中包含15-50重量%,最优选20-30重量%的至少一种填料。
它可以含有本领域已知的其它添加剂。术语“添加剂”包括染料、触变剂(例如,脲衍生物、原纤化短纤维或纸浆短纤维)、色浆和/或颜料、导电添加剂(例如导电炭黑或高氯酸锂)、增塑剂、增粘剂、其它不同于根据本发明的聚酰胺的热塑性聚合物、稳定剂、促粘剂、流变添加剂、蜡、催化剂、除湿剂或其任何组合。
基于热熔粘合剂的总重量,根据本发明的热熔粘合剂组合物优选包含0.1-30重量%的添加剂。在更优选的实施方案中包含1-25重量%,最优选5-20重量%。在甚至更优选的实施方案中,添加剂选自稳定剂、促粘剂、增塑剂、增粘剂、与根据本发明的聚酰胺不同的热塑性聚合物、催化剂、除湿剂及其组合。
根据本发明的热熔粘合剂组合物可以包含增粘剂,例如衍生自松香酸、松香酸酯、其它松香酯、多萜树脂、萜烯/酚醛树脂、苯乙烯化萜烯、聚α-甲基苯乙烯、α-甲基苯乙烯-酚或脂肪族、芳族或芳族/脂肪族烃树脂或香豆酮/茚树脂的树脂。这些增粘树脂可以任选包含OH基团,以改善不同组分的相容性。
基于热熔粘合剂的总重量,根据本发明的热熔粘合剂组合物包含0.1-30重量%的至少一种增粘剂。在更优选的实施方案包含1-25重量%,最优选5-20重量%的至少一种增粘剂。
根据本发明的热熔粘合剂组合物可以包含其它热塑性聚合物。这些优选选自EVA、聚氨酯聚合物、橡胶型聚合物、苯乙烯共聚物、聚酯共聚物、聚碳酸酯、丙烯酸类、热塑性聚氨酯及其组合。
基于热熔粘合剂的总重量,根据本发明的热熔粘合剂组合物优选包含0.1-30重量%的至少一种其它热塑性聚合物。在更优选的实施方案中包含1-25重量%,最优选5-20重量%的至少一种其它热塑性聚合物。
根据本发明的热熔粘合剂组合物可以包含增塑剂,前提条件是这些增塑剂不会妨碍组合物的热熔能力,例如邻苯二甲酸酯、苯甲酸酯、蔗糖酯和磺酰胺。作为实例,可以提及液体邻苯二甲酸酯增塑剂,基于芳族酯的增塑剂,例如苯甲酸酯,或固体增塑剂如邻苯二甲酸二环己酯、环己烷二甲醇二苯甲酸酯等。其它增塑剂,如蔗糖醋酸异丁酸酯、邻/对甲苯磺酰胺或N-乙基邻甲苯磺酰胺也是适合的。
基于热熔粘合剂的总重量,根据本发明的热熔粘合剂组合物优选包含0.1-30重量%的增塑剂。在更优选的实施方案中包含1-25重量%,最优选为5-20重量%的增塑剂。
可以使用不同的组分作为稳定剂,例如抗氧化剂、UV稳定剂、水解稳定剂。这些组分的实例是高分子量的空间位阻酚、含硫和含磷的酚或胺。这包括空间位阻酚、多官能酚、硫醚、取代苯并三唑、受阻苯甲酮和/或空间位阻胺。水解稳定剂的实例包括低聚和/或聚合的脂肪族或芳族碳二亚胺。这些组分是市售的并且是本领域技术人员已知的。
优选可以使用单体、低聚或聚合形式的有机官能硅烷作为促粘剂。所述有机官能硅烷优选选自3-缩水甘油氧基-丙基三烷氧基硅烷、3-丙烯酰氧基丙基三烷氧基硅烷、3-氨基丙基三烷氧基硅烷、1-氨基烷基三烷氧基硅烷、α-甲基丙烯酰氧基甲基三烷氧基硅烷、乙烯基三烷氧基硅烷、N-氨基乙基-3-氨基丙基-甲基二烷氧基硅烷、苯基氨基丙基三烷氧基硅烷、氨基烷基三烷氧基二硅烷、异丁基甲氧基硅烷、N(2-氨基乙基)-3-氨基丙基三烷氧基硅烷、甲基丙烯酰氧基甲基-三乙氧基硅烷、其与烷氧基的混合物优选包括C1-C4单醇。基于热熔粘合剂组合物的总重量,优选用量为0.05-5重量%,特别为0.1-2重量%。
基于热熔粘合剂的总重量,根据本发明的热熔粘合剂组合物优选包含0.1-30重量%的选自稳定剂和促粘剂或其组合的化合物。在更优选的实施方案中包含1-25重量%,最优选5-20重量%的选自稳定剂和促粘剂或其组合的化合物。
除湿剂优选选自乙烯基三甲氧基硅烷、甲基三甲氧基硅烷、六甲基二硅氮烷、对甲苯磺酰基异氰酸酯(PTSI)或其组合。
基于热熔粘合剂的总重量,根据本发明的热熔粘合剂组合物优选包含0.1-5重量%的除湿剂。在更优选的实施方案中包含0.2-3重量%,最优选0.5-1重量%的除湿剂。
优选地,根据本发明的催化剂选自有机钛酸酯化合物、有机锡化合物、有机锆化合物、胺化合物、有机铝化合物、酸性磷酸酯、酸性磷酸酯和胺化合物的反应产物、饱和或不饱和多元羧酸或其酸酐、羧酸化合物和胺化合物反应产物的盐、以及辛酸铅。示例性的锡化合物是二月桂酸二丁基锡、马来酸二丁基锡、二乙酸二丁基锡、马来酸二辛基锡、邻苯二甲酸二丁基锡、辛酸亚锡、环烷酸亚锡、硬脂酸亚锡、叔碳酸亚锡、二丁基氧化锡和邻苯二甲酸酯的反应产物、二乙酰丙酮二丁基锡等螯合化合物和氧化二丁基锡。有机钛酸酯化合物的实例是钛酸酯类,例如钛酸四丁酯、钛酸四丙酯、钛酸四异丙酯和三乙醇胺钛酸酯,螯合化合物如四乙酰丙酮钛。示例性的有机铝化合物是三乙酰丙酮铝、三(乙酰乙酸乙酯)铝和二异丙氧基铝乙酰乙酸乙酯。示例性的锆化合物是四异丙醇锆、四丁氧基锆和四乙酰丙酮锆。示例性胺化合物是丁胺、辛胺、月桂胺、二丁胺、单乙醇胺、二乙醇胺、三乙醇胺、二亚乙基三胺、三亚乙基四胺、油胺、环己胺、苄胺、二乙基氨基丙基胺、苯二甲胺、三亚乙基二胺、胍、二苯基胍、2,4,6-三(二甲基氨基甲基)苯酚、吗啉、N-甲基吗啉、2-乙基-4-甲基咪唑和1,8-二氮杂双环[5.4.0]十一碳烯-7(DBU)。也可以使用这些胺与羧酸的盐。作为其它实例,可以提及由过量的多元胺和多元酸得到的低分子量聚酰胺树脂和由过量的多元胺和环氧化合物的反应产物。此外,可以提及有机铅化合物如辛酸铅、有机铁化合物如环烷酸铁、有机钒化合物、铋盐如三(2-乙基己酸)铋和三(新癸酸)铋,和由过量的有机羧酸和有机胺的反应产物。这些促进剂可以单独使用,也可以两种以上组合使用。在这些硅烷醇缩合催化剂中,从固化性的角度来看,优选有机金属化合物或包含有机金属化合物和胺化合物的组合体系。
基于热熔粘合剂的总重量,根据本发明的热熔粘合剂组合物优选包含0.1-5重量%的催化剂。在更优选的实施方案中包含0.2-3重量%,最优选0.5-1重量%的催化剂。
实施例和测量方法
分子量测定
通过凝胶渗透色谱(GPC)在相同的色谱条件下分析相应的硅氧烷化合物的分子量和摩尔质量分布。将测试样品溶解在甲苯中,并将所制备的样品溶液通过0.20μm针筒式过滤器过滤到分析瓶中。使用Styragel色谱柱使用GPC分离技术在80℃下进行甲苯洗脱和折射率检测,通过液相色谱法分析所制备的样品溶液。基于用聚苯乙烯标准进行的外部校准测定待测试物质的数均分子量(Mn)和重均分子量(Mw)。
熔融粘度(本发明中也称为粘度)
使用Brookfield粘度计型号RVDV-1+,用粘度标准油校准,用106型温度控制器和Thermosel装置测量熔融粘度。将10-12g粘合剂称重到一次性铝粘度计管中。将管插入粘度计中并在160℃下平衡30分钟。将预热的27号转子插入到粘合剂中并在160℃下旋转30分钟;根据测量的粘度范围调整旋转速度。然后在160℃下测量初始粘度V1。
拉伸强度
根据ASTM D412/DIN 53504/ISO 37,使用装备有5kN的测力传感器的Sun 5型Galdabini测力计测定拉伸强度。在试验期间,机器保持500mm/min的位移速率。该机器记录最高拉伸应力以确定拉伸强度。
硬度
根据ASTM D2240/DIN53505/ISO868/ISO,使用配备有测量邵氏类型A系统的ATSfaar硬度计测定硬度。产物在25℃/50%HR下固化7天,以制备2mm厚的片。使用2片进行测量以获得6mm厚度。
搭接剪切(基板:Al-Al和不锈钢-不锈钢)
根据ASTM D1002-05/ASTM D3163/ISO 4587/DIN EN 1465,使用装备有5kN的测力传感器的Sun 5型Galdabini测力计测定搭接剪切。以12.7mm×25.4mm的重叠组装两个基板制备样品。间隙为1mm。在测试前,产品在25℃/50%HR下固化7天。
软化点
使用PAC环和HRB 754型球仪来测定软化点。软化点的定义为,当样品在油浴中以规定的速率加热时,保持在水平环内的样品盘在钢球的重量下下降预定距离的温度。在1.6克产品用3.5克金属球进行测试。
热塑性组合物的制备
方法A1
将聚酰胺在惰性气氛(氮气)中在烧瓶中熔融并加热至高于其熔点。然后在搅拌(约200rpm)下逐渐加入液体硅氧烷化合物,同时混合物的温度保持在聚酰胺的熔点以上。将混合物在聚酰胺的熔点之上混合30分钟至1小时(约2400-2800rpm),随后移出。冷却后,得到固体热塑性组合物。
方法A2(对照方法)
将聚酰胺、液体聚硅氧烷化合物和稳定剂一起置于烧瓶中,并在惰性气氛(氮气)中加热到聚酰胺的熔点以上搅拌30分钟到1小时(约2400-2800rpm)。冷却后,得到液体组合物。
制备热熔粘合剂
方法B
向混合器中加入方法A1中得到的热塑性组合物,并加热至热塑性混合物为液体的温度。随后加入填料。然后使混合物达到105-120℃的温度,并施加动态真空约2小时。将混合物冷却至60℃,并加入任选的添加剂和组合物的其它组分。最后将混合物搅拌,同时施加动态真空约20分钟,得到热熔粘合剂。
如果期望得到反应性热熔体,将混合物冷却至75-85℃,加入交联剂,并施加动态真空步骤2小时之后和在冷却至60℃之前,施加动态真空约1小时。
实施例1
根据方法A1制备热塑性组合物。
组成:
40重量%的聚酰胺(Technomelt PA 6730,具有约85℃的熔点)
57.5重量%的液体聚硅氧烷(在25℃下粘度为20,000mPas,OH封端)
2.5重量%的氨基官能硅氧烷(购自CHT的Hansa AS 8020)
实施例2
根据方法A1制备热塑性组合物。
组成:
40重量%的聚酰胺(Technomelt PA 6730,具有约85℃的熔点)
57.5重量%的液体聚硅氧烷(在25℃下粘度为20,000mPas,OH封端)
2.5重量%的氨基官能硅氧烷(购自CHT的Hansa ASR 7020)
实施例3
根据方法A1制备热塑性组合物。
组成:
30重量%的聚酰胺(Technomelt PA 2006,具有约110℃的熔点)
67.5重量%的液体聚硅氧烷(在25℃下粘度为3,500mPas;OH封端)
2.5重量%的氨基官能硅氧烷(购自CHT的Hansa AS 7020)
实施例4
根据方法A1制备热塑性组合物。
组成:
40重量%的聚酰胺(Technomelt PA 6730,具有约85℃的熔点)
57.5重量%的液体聚硅氧烷(在25℃下粘度为20,000mPas;OH封端)
2.5重量%的氨基官能硅氧烷(购自CHT的Hansa ASR 7020)
对比例5-7
根据方法A2制备对比例5-7。使用实施例1-4中的化合物和量。在对比例5-7中,仅得到没有显示任何热塑性的液体。
实施例8
根据方法B制备热熔粘合剂。
50重量%的根据实施例2的热塑性组合物
6.1重量%的CH3封端的聚二甲基硅氧烷(在25℃下粘度为1,000mPas)
33.1重量%的Silbond 8000TST(填料)
5重量%的Aerosil R974(处理的二氧化硅;填料)
1重量%的Raven 1020(炭黑)
2.95重量%的LM 400(交联剂)
1.65重量%的Silane A 1110(促粘剂)
0.2重量%的Formrez UL 28(催化剂)
0.1重量%的六甲基二硅氮烷(除湿剂)
得到的热熔体具有如下性质:
在6.2巴和95℃下的挤出:34.61(g/min)
拉伸强度:1.62(g/min)
断裂伸长率:230%
硬度(邵氏A):45
搭接剪切(铝):1.167N/mm2
搭接剪切(不锈钢):1.15N/mm2
Claims (15)
1.一种热塑性组合物,其包含至少一种优选具有小于185℃的熔点的聚酰胺和至少一种在25℃下优选具有750-100,000mPas的粘度并且是OH封端的液体聚硅氧烷化合物,其中所述热塑性组合物可通过包括以下步骤的方法得到:
1a)加热所述至少一种聚酰胺至高于该至少一种聚酰胺的熔点并且优选低于185℃的温度;
2a)在搅拌下向步骤1a)的加热的化合物中加入所述至少一种液体聚硅氧烷化合物,其中所述温度保持在高于所述至少一种聚酰胺的熔点并且优选低于185℃;以及
3a)优选在80-180℃下,更优选在110-140℃下将步骤2a)得到的混合物混合。
2.根据权利要求1所述的热塑性组合物,其中在步骤2a)中另外加入至少一种稳定剂。
3.根据权利要求1或2所述的热塑性组合物,其中基于所述热塑性组合物的总重量,所述至少一种聚酰胺以25-70重量%的量存在。
4.根据权利要求2或3所述的热塑性组合物,其中所述稳定剂是与所述至少一种液体聚硅氧烷不同的氨基官能硅氧烷,优选以基于所述热塑性组合物的总重量0.1-15重量%的量存在。
5.根据权利要求1-4中任一项所述的热塑性组合物在密封剂中,在粘合剂中,或作为流变改性剂或表面改性剂的用途。
6.一种热熔粘合剂,其包含根据权利要求1-4中任一项所述的热塑性组合物。
7.根据权利要求6所述的热熔粘合剂,其还包含填料和任选存在的添加剂。
8.根据权利要求6或7所述的热熔粘合剂,其还包含交联剂。
9.根据权利要求8所述的热熔粘合剂,其中所述交联剂选自甲基三(二甲基酮肟)硅烷、乙烯基三(甲基乙基酮肟)硅烷、甲基三(甲基乙基酮肟)硅烷及其组合。
10.根据权利要求6-9中任一项所述的热熔粘合剂,基于所述热熔粘合剂的总重量,其包含20-80重量%的根据权利要求1-4中任一项所述的热塑性组合物。
11.根据权利要求7-10中任一项所述的热熔粘合剂,基于所述热熔粘合剂的总重量,其包含10-60重量%的所述填料。
12.根据权利要求7-11中任一项所述的热熔粘合剂,其中所述填料是硅酸盐。
13.根据权利要求7-12中任一项所述的热熔粘合剂,其中所述至少一种添加剂选自促粘剂、稳定剂、增粘剂、其它热塑性聚合物、增塑剂、催化剂、除湿剂及其组合。
14.根据权利要求7-13中任一项所述的热熔粘合剂,其中,基于所述热熔粘合剂的总重量,所述至少一种添加剂以0.1-30重量%的量存在。
15.根据权利要求6-14中任一项所述的热熔粘合剂在车辆部件、结构、窗户、玻璃窗、卫生应用、配件、屋顶、管道、设备应用和窗格粘合中的用途。
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PCT/EP2015/076944 WO2016096305A1 (en) | 2014-12-18 | 2015-11-18 | Thermoplastic composition comprising a polyamide and a polysiloxane |
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JP7346407B2 (ja) | 2018-02-01 | 2023-09-19 | ダウ シリコーンズ コーポレーション | 組成物、それを用いて形成されるポリマー複合体物品、およびその調製方法 |
CN113249083A (zh) * | 2021-05-12 | 2021-08-13 | 上海尤耐有机硅材料有限公司 | 一种能深层固化缩合有机硅电子灌封胶及其制造方法 |
KR102468182B1 (ko) * | 2021-12-29 | 2022-11-16 | 실버스타케미칼(주) | 차량용 폴리아마이드 핫멜트 접착수지 제조방법 |
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JP6793646B2 (ja) | 2020-12-02 |
WO2016096305A1 (en) | 2016-06-23 |
US20170267862A1 (en) | 2017-09-21 |
US10160859B2 (en) | 2018-12-25 |
PL3034557T3 (pl) | 2021-05-04 |
CA2970851A1 (en) | 2016-06-23 |
CN107109063B (zh) | 2021-02-19 |
KR20170095261A (ko) | 2017-08-22 |
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