CN105682918B - 硅橡胶‑氟树脂层合体 - Google Patents
硅橡胶‑氟树脂层合体 Download PDFInfo
- Publication number
- CN105682918B CN105682918B CN201480048696.3A CN201480048696A CN105682918B CN 105682918 B CN105682918 B CN 105682918B CN 201480048696 A CN201480048696 A CN 201480048696A CN 105682918 B CN105682918 B CN 105682918B
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- Prior art keywords
- fluororesin
- silicon rubber
- weight
- layer
- epoxy resin
- Prior art date
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 38
- 239000003822 epoxy resin Substances 0.000 claims abstract description 56
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 56
- 229910000077 silane Inorganic materials 0.000 claims abstract description 48
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000463 material Substances 0.000 claims abstract description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 18
- 229910052710 silicon Inorganic materials 0.000 claims description 16
- 239000010703 silicon Substances 0.000 claims description 16
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 11
- 239000006185 dispersion Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 2
- 230000037431 insertion Effects 0.000 claims 1
- 238000003780 insertion Methods 0.000 claims 1
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 17
- 230000007774 longterm Effects 0.000 abstract description 12
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 20
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- 125000000524 functional group Chemical group 0.000 description 11
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 10
- 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 description 9
- 238000000034 method Methods 0.000 description 9
- 238000000576 coating method Methods 0.000 description 8
- 229910052731 fluorine Inorganic materials 0.000 description 8
- 239000011737 fluorine Substances 0.000 description 8
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
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- 229940106691 bisphenol a Drugs 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000806 elastomer Substances 0.000 description 3
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical compound FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 3
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- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000004026 adhesive bonding Methods 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
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- ZFVMWEVVKGLCIJ-UHFFFAOYSA-N bisphenol AF Chemical compound C1=CC(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C=C1 ZFVMWEVVKGLCIJ-UHFFFAOYSA-N 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
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- 238000005323 electroforming Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000004848 polyfunctional curative Substances 0.000 description 2
- 229920002620 polyvinyl fluoride Polymers 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
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- 229910052719 titanium Inorganic materials 0.000 description 2
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- VHSBTBDMKDUVKG-UHFFFAOYSA-N (dimethylcarbamothioyltrisulfanyl) n,n-dimethylcarbamodithioate Chemical compound CN(C)C(=S)SSSSC(=S)N(C)C VHSBTBDMKDUVKG-UHFFFAOYSA-N 0.000 description 1
- ODIGIKRIUKFKHP-UHFFFAOYSA-N (n-propan-2-yloxycarbonylanilino) acetate Chemical compound CC(C)OC(=O)N(OC(C)=O)C1=CC=CC=C1 ODIGIKRIUKFKHP-UHFFFAOYSA-N 0.000 description 1
- RRZIJNVZMJUGTK-UHFFFAOYSA-N 1,1,2-trifluoro-2-(1,2,2-trifluoroethenoxy)ethene Chemical group FC(F)=C(F)OC(F)=C(F)F RRZIJNVZMJUGTK-UHFFFAOYSA-N 0.000 description 1
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 1
- URJFKQPLLWGDEI-UHFFFAOYSA-N 1-benzyl-2-methylimidazole Chemical compound CC1=NC=[C]N1CC1=CC=CC=C1 URJFKQPLLWGDEI-UHFFFAOYSA-N 0.000 description 1
- 150000004963 1-benzylimidazoles Chemical class 0.000 description 1
- YTWBFUCJVWKCCK-UHFFFAOYSA-N 2-heptadecyl-1h-imidazole Chemical class CCCCCCCCCCCCCCCCCC1=NC=CN1 YTWBFUCJVWKCCK-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
- 150000004941 2-phenylimidazoles Chemical class 0.000 description 1
- LLEASVZEQBICSN-UHFFFAOYSA-N 2-undecyl-1h-imidazole Chemical class CCCCCCCCCCCC1=NC=CN1 LLEASVZEQBICSN-UHFFFAOYSA-N 0.000 description 1
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- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- FVCSARBUZVPSQF-UHFFFAOYSA-N 5-(2,4-dioxooxolan-3-yl)-7-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C(C(OC2=O)=O)C2C(C)=CC1C1C(=O)COC1=O FVCSARBUZVPSQF-UHFFFAOYSA-N 0.000 description 1
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- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
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- 229920006361 Polyflon Polymers 0.000 description 1
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- 229910006095 SO2F Inorganic materials 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-N anhydrous cyanic acid Natural products OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
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- HRKQOINLCJTGBK-UHFFFAOYSA-N dihydroxidosulfur Chemical compound OSO HRKQOINLCJTGBK-UHFFFAOYSA-N 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 125000001160 methoxycarbonyl group Chemical group [H]C([H])([H])OC(*)=O 0.000 description 1
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 description 1
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
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- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- G—PHYSICS
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- G03G15/20—Apparatus for electrographic processes using a charge pattern for fixing, e.g. by using heat
- G03G15/2003—Apparatus for electrographic processes using a charge pattern for fixing, e.g. by using heat using heat
- G03G15/2014—Apparatus for electrographic processes using a charge pattern for fixing, e.g. by using heat using heat using contact heat
- G03G15/206—Structural details or chemical composition of the pressure elements and layers thereof
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- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/04—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B25/08—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
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- B32B27/304—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl halide (co)polymers, e.g. PVC, PVDC, PVF, PVDF
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- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
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- G—PHYSICS
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- G03G15/2003—Apparatus for electrographic processes using a charge pattern for fixing, e.g. by using heat using heat
- G03G15/2014—Apparatus for electrographic processes using a charge pattern for fixing, e.g. by using heat using heat using contact heat
- G03G15/2053—Structural details of heat elements, e.g. structure of roller or belt, eddy current, induction heating
- G03G15/2057—Structural details of heat elements, e.g. structure of roller or belt, eddy current, induction heating relating to the chemical composition of the heat element and layers thereof
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- B32B2250/24—All layers being polymeric
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- B32B2255/00—Coating on the layer surface
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Abstract
硅橡胶‑氟树脂层合体,其中,在基材上依次形成有硫化硅橡胶层和氟树脂层,该硅橡胶‑氟树脂层合体是在硫化硅橡胶层上依次形成含有30~80重量%的环氧树脂和70~20重量%的硅烷偶联剂的含环氧树脂的硅烷系底漆层、氟树脂系底漆层后再形成氟树脂层而构成的。该硅橡胶‑氟树脂层合体不仅初期粘合性不会降低,而且即使在热状态或长期加热等加热环境下已硫化的硅橡胶与氟树脂的粘合性也不会降低。
Description
技术领域
本发明涉及硅橡胶(silicone rubber,硅酮橡胶或有机硅橡胶)-氟树脂层合体。更详细而言,涉及复印机的色粉(toner,墨粉或调色剂)定影部件等中使用的硅橡胶-氟树脂层合体。
背景技术
通常,复印机等中使用的定影辊、定影带等色粉定影部件1使用如下部件:如图2所示,该部件是在环状基材2上形成由橡胶等弹性体构成的层3,再经由粘合剂层7在弹性层3上形成四氟乙烯-全氟烷基乙烯基醚共聚树脂[PFA]或聚四氟乙烯树脂[PTFE]等的氟树脂层6作为表层。
作为这样的定影辊、定影带等色粉定影部件,提出了各种部件。例如,专利文献1中提出了一种(silicone,硅酮或有机硅)橡胶-氟树脂层合体,该层合体可如下形成:在环状基材的表面经由橡胶层用粘合剂粘合有机硅系橡胶等的橡胶层,再于该橡胶层上使用有机硅系、酰亚胺系等的粘合剂粘合管状PFA而形成。
这样的色粉定影部件,从色粉定影性的角度考虑,要求氟树脂层的薄膜化,但薄膜化了的管状氟树脂难以进行内表面加工,存在着与弹性层的粘合差的问题。
针对所述问题,专利文献2~5中提出了各种硅橡胶-氟树脂层合体,其中还包括在弹性体层与氟树脂层之间设有底涂料层和/或底漆层的层合体。
专利文献2中提出了:在基材上依次形成有弹性层和表层的定影辊、定影带等,其中,所述定影辊、定影带的表层是通过使PFA管热收缩而形成的层,表层与弹性层经由含20~30重量%PFA的粘合剂材料粘合。所述定影辊、定影带,由于PFA管未进行内表面处理,所以成本低,还具有底漆层薄的特征,表面粗糙度小,初期粘合性也优异,但如后述比较例5所示,在热粘合力和长期加热试验后的粘合性方面仍不能满足要求。
专利文献3中提出了一种定影用部件,所述定影用部件是在形成于圆筒形或圆柱形基材上的弹性层上施行环氧系底漆等的底漆处理,再形成氟树脂层,之后用已加热收缩的热收缩性管完全覆盖,然后加热烧结而成膜。所述定影用部件的表面平滑,其表面粗糙度Rz达到5μm以下,但在初期粘合性、热粘合力、长期加热试验后的粘合性方面不满足要求。
专利文献4中公开了一种含氟层合体,该含氟层合体由基材、形成于基材上的底漆层和形成于该底漆层上的成型体层构成,当选择硅橡胶作为形成基材的耐热性橡胶时,底漆层由包含烷氧基硅烷单体聚合物(和有机钛酸酯化合物)在内的含官能团的含氟烯键性聚合物构成,成型体层由使用了热收缩PFA管的含氟树脂成型体形成。所述含氟层合体的表面粗糙度也小、初期粘合性也优异,但在热粘合力和长期加热试验后的粘合性方面仍不满足要求。
专利文献5中提出了一种加热辊,该加热辊是在金属制空心金属芯上设置硅橡胶包覆层、同时在最外层形成由PFA构成的薄膜而形成,该加热辊是在硅橡胶包覆层与PFA薄膜之间***双层结构的底漆层而形成,所述双层结构底漆层的下层由以硅树脂和硅烷偶联剂作为主要成分的混合物构成、而上层由以烷氧基改性氟树脂作为主要成分的混合物构成。所述加热辊具有均匀的膜厚,初期粘合性优异,同时表面粗糙度、热粘合力也显示出良好的值,但长期加热试验后的粘合性不满足要求。
关于粘合性,已知由于金属氧化物(例如氧化铁红Fe2O3)的活性度高、官能团也多,因此若将其添加在底漆中,则粘合性提高,但根据复印机用定影部件的粘合要求水平,有时无法满足要求。
如上所述,以往提出的部件均无法充分满足热粘合力、长期加热试验后的粘合性。这是由于:因硅橡胶与氟树脂的结构不同,所以相容性不好、特别是在已硫化的硅橡胶侧缺少反应性官能团,因此存在着硅橡胶侧的粘合性弱的倾向。
因此,即使形成氟系底漆,氟树脂与底漆通过加热熔融而粘合,但与硅橡胶的粘合力反而变弱。其结果,虽然初期可见氟树脂与硅橡胶粘合,但由于热状态或长期加热等加热环境,粘合性有时会降低。另外,已硫化的硅橡胶的表面呈惰性状态,在橡胶表面存在阻碍粘合性的低分子成分,有时会使底漆与橡胶的粘合恶化。
现有技术文献
专利文献
专利文献1:日本特开2004-276290号公报;
专利文献2:WO2008/126915;
专利文献3:日本特开平10-142988号公报;
专利文献4:WO2004/18201;
专利文献5:日本特开昭61-250668号公报;
专利文献6:日本特开平6-248116号公报。
发明内容
发明所要解决的课题
本发明的目的在于提供一种不仅初期粘合性不会降低、而且即使在热状态或长期加热等加热环境下已硫化的硅橡胶与氟树脂的粘合性也不会降低的硅橡胶-氟树脂层合体。
用于解决课题的手段
所述本发明的目的通过硅橡胶-氟树脂层合体来实现,所述硅橡胶-氟树脂层合体在基材上依次形成有硫化硅橡胶层和氟树脂层,其中,所述硅橡胶-氟树脂层合体是在硫化硅橡胶层上依次形成含有30~80重量%的环氧树脂和70~20重量%的硅烷偶联剂的含环氧树脂的硅烷系底漆层和氟树脂系底漆层,之后形成氟树脂层。
发明效果
本发明所涉及的硅橡胶-氟树脂层合体,通过在硅橡胶上形成含有一定比例的环氧树脂和硅烷偶联剂的含环氧树脂的硅烷系底漆层,使得含环氧树脂的硅烷系底漆层与已硫化的硅橡胶反应,而且硅烷偶联剂与氟树脂底漆反应,另外,通过添加环氧树脂,发挥可以提高硅橡胶与氟树脂在热状态下的粘合性的优异效果。
另外,由于PFA管通过加热而发生热熔融,使得氟树脂系底漆融合而与氟树脂粘合,因此由硫化硅橡胶的规格决定的粘合强度的偏差消失,可以获得粘合强度稳定的制品。
附图说明
图1是显示由本发明所涉及的硅橡胶-氟树脂层合体形成的定影辊的剖面图的一个例子的图。
图2是显示由现有的硅橡胶-氟树脂层合体形成的定影辊的剖面图的一个例子的图。
具体实施方式
作为基材,使用不锈钢、铁、铝等金属制基材;或聚酰胺树脂、聚酰亚胺树脂等耐热性树脂制基材,优选当为定影辊时使用不锈钢、铁、铝等,当为定影带时使用通过电铸法制造的金属带、镍电铸、聚酰亚胺树脂等,其厚度通常采用约10~100μm的厚度。另外,关于其形状,当用作定影辊时采用圆筒形状,当用作定影带时采用环形带形状。这里,定影部件是指复印机等的色粉定影部分使用的定影辊、定影带。
作为硅橡胶,使用二甲基硅橡胶、甲基苯基硅橡胶、氟硅橡胶、乙烯基硅橡胶等,它们通常以约50μm~1mm、优选约100~500μm的厚度在基材上形成硅橡胶层。通过加热等手段硫化的硅橡胶具有能够耐受在色粉等的定影温度下连续使用的程度的耐热性。
在硅橡胶层上首先形成含有30~80重量%的环氧树脂和70~20重量%的硅烷偶联剂的含环氧树脂的硅烷系底漆层。
作为环氧树脂,使用下述的环氧树脂:通过双酚A、双酚F、双酚AF、酚醛树脂等与环氧氯丙烷的反应得到的化合物;或由这些化合物得到的各种衍生物、例如双酚A型环氧树脂、双酚A型含溴环氧树脂、双酚F型环氧树脂、双酚AF型环氧树脂、双酚AD型环氧树脂、DPP酚醛型环氧树脂、苯酚醛型环氧树脂、甲酚醛型环氧树脂等的至少一种,优选甲酚醛型环氧树脂或双酚A型环氧树脂与苯酚醛型环氧树脂的混合物。这些环氧树脂以作为水性分散液的乳剂类型、或丙酮、丁酮等有机溶剂溶液或分散液的形式使用,其可以直接使用作为市售品的DIC制造的Epiclon N-665、N-670、N-673、N-695、840、850、860、1055、2050、N-730A、N-740、N-865、N-775、N-665-EXP-S、850-LC等。
作为硅烷偶联剂,使用含乙烯基、含环氧基、含甲基丙烯酰氧基、含氨基、含氯基、含巯基等的硅烷偶联剂,例如:乙烯基三氯硅烷、乙烯基三乙氧基硅烷、乙烯基三(β-甲氧基-乙氧基)硅烷、β-(3,4-环氧基环己基乙基)三甲氧基硅烷、γ-缩水甘油氧基丙基三甲氧基硅烷、γ-甲基丙烯酰氧基丙基三甲氧基硅烷、γ-氨基丙基三乙氧基硅烷、3-氨基丙基三乙氧基硅烷、3-氨基丙基三甲氧基硅烷、N-β-(氨基乙基)-γ-氨基丙基三甲氧基硅烷、N-β-(氨基乙基)-γ-氨基丙基甲基二甲氧基硅烷、N-苯基-γ-氨基丙基三甲氧基硅烷、γ-氯丙基三甲氧基硅烷、γ-巯基丙基三甲氧基硅烷、双[3-(三乙氧基甲硅烷基)丙基]四硫化物、专利文献6等中记载的γ-三甲氧基甲硅烷基丙基二甲基硫代氨基甲酰基四硫化物、γ-三甲氧基甲硅烷基丙基苯并噻唑基四硫化物等四硫化物类等的至少一种,优选下述式[I]或[II]所表示的硅烷化合物。
XnSi(OR)4-n [I]
R:碳原子数为1~3的烷基;
X:3-氨基丙基、N-β-(氨基乙基)-γ-氨基丙基、N-苯基-3-氨基丙基、3-甲基丙烯酰氧基丙基、3-缩水甘油氧基丙基、3-巯基丙基、乙烯基等;
n:1~3的整数;
R1 m(R2)n-Si-R3 4-m-n [II]
m、n:0~4的整数;
R1:碳原子数为10以下的烷基;
R2:碳原子数为10以下的烷氧基;
R3:碳原子数为10以下的甲基丙烯酰氧基烷基。
关于环氧树脂和硅烷偶联剂,以由上述各成分构成的含环氧树脂的硅烷系底漆成分的固体重量计,以30~80重量%、优选40~70重量%的比例使用环氧树脂,以70~20重量%、优选60~30重量%的比例使用硅烷偶联剂。若环氧树脂的配比少于上述值,则热粘合性、长期加热试验后的粘合性、定影性等变差,而当硅烷偶联剂的配比少于上述值时,长期加热试验后的粘合性、定影性等变差。
对在硅橡胶上涂刷含环氧树脂的硅烷系底漆的方法没有特别限定,例如通过浸渍法、喷雾法、辊涂法、刮刀涂布法、流涂法等来进行,关于涂布后的干燥条件也可以适当设定,例如在室温~约150℃、约5~30分钟的条件下进行,形成厚约1~10μm、优选约1~5μm的底漆层。
硅烷偶联剂还作为环氧树脂用固化剂而发挥作用,此外,作为环氧树脂用固化剂,还可以使用咪唑类、速固化性的硫醇类。作为咪唑类,可以列举:2-甲基咪唑、2-乙基-4-甲基咪唑、2-十一烷基咪唑、2-十七烷基咪唑、2-苯基咪唑、1-苄基咪唑、1-苄基-2-甲基咪唑、2,4-二氨基-6-[2-甲基咪唑啉-(1)]-乙基-s-三嗪等。
作为氟树脂系底漆,通常使用氟树脂的水性分散液,此外,还使用在氟树脂中添加有磷酸和铬酸的混合物而得到的物质;或添加有含三氟乙烯基醚基的磷酸酯化合物、聚醚砜树脂、聚酰胺酰亚胺树脂、聚酰亚胺树脂、聚苯硫醚树脂、有机钛酸酯等的氟树脂或含反应性官能团的氟树脂。这里,作为有机钛酸酯,可以列举:由Ti(IV)或Ti(III)与具有醇性羟基、酚性羟基或羧基的化合物形成的含Ti-O-C键的烷氧基钛、钛酰化物或钛螯合物等。通过使用所述的氟树脂系底漆,含环氧树脂的硅烷系底漆与PFA的粘合性提高。作为这样的底漆,使用市售品、例如三井DuPont Polychemicals制品PL-992CL、PL-990CL等。
这里,为了提高与含环氧树脂的硅烷系底漆层的粘合性,作为底漆层中使用的氟树脂,优选使用含有羧酸基或其衍生基团、羟基、腈基、氰酸酯基、氨基甲酰氧基、膦酰氧基、卤代膦酰氧基、磺基或其衍生基团和磺酰卤基等官能团作为其至少一部分的氟树脂。这里,作为官能团的具体例子,可以列举:-COOH、-CH2COOH、-COOCH3、-CONH2、-OH、-CH2OH、-CN、-CH2O(CO)NH2、-CH2OCN、-CH2OP(O)(OH)2、-CH2P(O)Cl2、-SO2F等。
具有所述官能团的氟树脂是在不会大幅损及热熔融性氟树脂的性质的范围内含有官能团的氟树脂,可以在热熔融性氟树脂的合成后通过添加或取代而导入官能团、或者在热熔融性氟树脂的合成时通过使具有官能团的单体共聚、优选在热熔融性氟树脂的合成时通过使具有官能团的单体共聚而得到。
氟树脂系底漆以其水性分散液、有机溶剂分散液等形式调制,再采用浸渍法、喷雾法、辊涂法、刮刀涂布法、流涂法等任意的涂刷方法将这些分散液以约1~20μm、优选约1~10μm的厚度涂布在含环氧树脂的硅烷系底漆层上。当涂布厚度比上述值厚时,表面产生凹凸,导热性变差。另一方面,当涂布厚度比上述值薄时,含环氧树脂的硅烷系底漆层暴露、或者与PFA管的热融合变难,进而粘合性恶化,因此不优选。
将氟树脂系底漆以水性分散液的形式使用时,其氟树脂浓度优选约10~20重量%,若以低于该值的浓度使用,则涂布斑点(深浅不均)变大,而若高于该值,则干燥后的被膜的凹凸变大。关于涂布后的干燥条件也可以适当设定,例如在室温~约150℃下、约5~30分钟的条件下进行。
在氟树脂系底漆层上层合热熔融性氟树脂,在所述氟树脂的熔点以上的温度、例如约260~350℃、优选约270~330℃下、约10~80分钟、优选约20~60分钟的条件下进行烧结。当烧结温度低于氟树脂的熔点时,氟树脂系底漆与通常以管状使用的氟树脂不发生热融合而导致粘合不良,而当烧结温度高于氟树脂的熔点时,硅橡胶发生热劣化。另外,当烧结时间比上述时间短时,有时会因PFA管的熔融不足而导致与氟树脂系底漆层的粘合不良,而当烧结时间比上述时间长时,硅橡胶有时会发生热劣化。
作为所述的热熔融性氟树脂,例如可以列举:四氟乙烯、六氟丙烯、全氟(烷基乙烯基醚)、偏二氟乙烯和氟乙烯等的聚合物或共聚物、或这些单体与乙烯的共聚物等。这些单体可以单独使用,也可以以两种以上的混合物的形式使用。
具体而言,可以列举:聚四氟乙烯[PTFE]、四氟乙烯-全氟(烷基乙烯基醚)共聚物[PFA]、四氟乙烯-六氟丙烯共聚物[FEP]、四氟乙烯-乙烯共聚物、四氟乙烯-六氟丙烯-全氟(烷基乙烯基醚)共聚物、聚偏二氟乙烯、聚氟乙烯、聚氯三氟乙烯、氯三氟乙烯-乙烯共聚物等或它们中的两种以上的组合,从弹性体的热劣化温度和成膜性的角度考虑,优选为四氟乙烯的共聚物,熔点较PTFE低的PFA、FEP例如可用作厚度为约5~20μm的热收缩性PFA管。
由上述构成形成的硅橡胶-氟树脂层合体当然可以作为平面状的层合体,还可以作为管状层合体的定影部件1,如图1所示,该管状层合体在环状基材2上依次形成有硅橡胶层3、含环氧树脂的硅烷系底漆层4、氟树脂系底漆层5和氟树脂层6。
实施例
接下来,就实施例来说明本发明。
实施例1
在作为基材的内径为40mm、壁厚为30μm、长410mm的环状镍带上涂布弹性层用硅烷系粘合剂(Dow Corning Toray公司制品DY39-042),再于其上使用分配器涂布硅橡胶(信越Silicone公司制品X34-2008),形成厚100μm的硅橡胶层,通过加热处理将硅橡胶层硫化成型。
使用喷雾器在硅橡胶层上涂刷下述含环氧树脂的硅烷系底漆,在常温下放置数分钟使溶剂挥发,形成厚2μm的含环氧树脂的硅烷系底漆层。
接着,使用喷雾器在含环氧树脂的硅烷系底漆层上涂刷由66重量份氟树脂(PFA的25重量%水溶液;三井DuPont Polychemicals制品PL-992CL)和34重量份水调制的氟树脂系底漆(固体浓度为16.5重量%),在室温条件下干燥,形成了厚2μm的氟树脂系底漆层,之后将厚10μm的未进行内表面处理的热收缩性PFA管(Gunze制品)在330℃下熔融包覆60分钟,得到了环状硅橡胶-氟树脂层合体。
实施例2
在实施例1中,在下层的含环氧树脂的硅烷系底漆成分中,将各成分量分别如下变更后使用:甲酚醛型环氧树脂量为4.37重量份(55.2重量%)、3-氨基丙基三乙氧基硅烷量为3.3重量份(41.7重量%)、乙烯基三乙氧基硅烷量为0.25重量份(3.2重量%)、丁酮量为4.64重量份。
实施例3
在实施例1中,在下层的含环氧树脂的硅烷系底漆成分中,将各成分量分别如下变更后使用:甲酚醛型环氧树脂量为5.34重量份(66.8重量%)、3-氨基丙基三乙氧基硅烷量为2.5重量份(31.3重量%)、乙烯基三乙氧基硅烷量为0.15重量份(1.9重量%)、丁酮量为5.67重量份。
实施例4
在实施例1中,在下层的含环氧树脂的硅烷系底漆成分中,将各成分量分别如下变更后使用:甲酚醛型环氧树脂量为4.37重量份(53.5重量%)、3-氨基丙基三乙氧基硅烷量为3.3重量份(40.4重量%)、乙烯基三乙氧基硅烷量为0.5重量份(6.1重量%)、丁酮量为4.64重量份。
实施例5
在实施例1中,在下层的含环氧树脂的硅烷系底漆成分中,将各成分量分别如下变更后使用:甲酚醛型环氧树脂量为4.37重量份(40.2重量%)、3-氨基丙基三乙氧基硅烷量为5.5重量份(50.6重量%)、乙烯基三乙氧基硅烷量为1.0重量份(9.2重量%)、丁酮量为4.64重量份。
实施例6
在实施例1中,在下层的含环氧树脂的硅烷系底漆成分中,将各成分量分别如下变更后使用:甲酚醛型环氧树脂量为4.37重量份(57.0重量%)、3-氨基丙基三乙氧基硅烷量为3.3重量份(43.0重量%)、丁酮量为4.64重量份,没有使用乙烯基三乙氧基硅烷。
比较例1
在实施例1中,在下层的含环氧树脂的硅烷系底漆成分中,将各成分量分别如下变更后使用:甲酚醛型环氧树脂量为1.0重量份(20.0重量%)、3-氨基丙基三乙氧基硅烷量为3.5重量份(70.0重量%)、乙烯基三乙氧基硅烷量为0.5重量份(10.0重量%)、丁酮量为1.0重量份。
比较例2
在实施例1中,在下层的含环氧树脂的硅烷系底漆成分中,将各成分量分别如下变更后使用:甲酚醛型环氧树脂量为7.3重量份(81.1重量%)、3-氨基丙基三乙氧基硅烷量为1.4重量份(15.6重量%)、乙烯基三乙氧基硅烷量为0.3重量份(3.3重量%)、丁酮量为7.7重量份。
比较例3
在实施例1中,在下层的含环氧树脂的硅烷系底漆成分中,将各成分量分别如下变更后使用:甲酚醛型环氧树脂量为2.4重量份(18.8重量%)、3-氨基丙基三乙氧基硅烷量为10重量份(78.1重量%)、乙烯基三乙氧基硅烷量为0.4重量份(3.1重量%)、丁酮量为2.6重量份。
比较例4
在实施例1中,在下层的含环氧树脂的硅烷系底漆成分中,将各成分量分别如下变更后使用:甲酚醛型环氧树脂量为4.3重量份(81.1重量%)、3-氨基丙基三乙氧基硅烷量为0.9重量份(17.0重量%)、乙烯基三乙氧基硅烷量为0.1重量份(1.9重量%)、丁酮量为3.7重量份。
比较例5
在实施例1中,仅设有上层的氟树脂系底漆层,没有设置下层的含环氧树脂的硅烷系底漆。
使用通过以上的各实施例和比较例得到的环状硅橡胶-氟树脂层合体,对初期粘合性、表面粗糙度、热粘合性、长期加热试验后的粘合性、定影性进行测定。
初期粘合性:ISO DIS2411所对应的JIS K6404-5涂橡胶布(rubber-coatedfabrics)、涂塑料布(plastics-coated fabrics)试验方法-依据第5部粘合试验进行剥离试验,观察断裂面,按照下述基准评价粘合性;
◎:橡胶断裂;
○:薄层橡胶断裂;
△:部分剥离;
×:整面剥离。
表面粗糙度:依据ISO 3274所对应的JIS B0651-1976,使用东洋精密制造的
Surfcom 1400A来测定Ra;
Ra为0.2以下的层合体评价为○、Ra超过0.2的层合体评价为×;
热粘合性:进行与初期粘合性相同的试验方法,评价170℃下的粘合性;
长期加热试验后的粘合性:进行与初期粘合性相同的试验方法,评价230℃、1000小时后的粘合性;
定影性:使用定影带在定影装置上形成图像,按照下述基准评价所定影部分的摩擦定影性;
○:印字图像良好且定影性良好;
×:印字图像不良或定影性不良。
所得结果见下表。
产业实用性
本发明所涉及的硅橡胶-氟树脂层合体,即使在热状态或长期加热等加热环境下,已硫化的硅橡胶与氟树脂的粘合性也不会下降,因此通过形成环状的构成,可有效用作复印机等的定影辊、定影带等色粉定影部件。
符号说明
1:定影部件;
2:基材;
3:硅橡胶层;
4:含环氧树脂的硅烷系底漆层;
5:氟树脂系底漆层;
6:氟树脂层;
7:粘合剂层。
Claims (6)
1.硅橡胶-氟树脂层合体,其中,在基材上依次形成有硫化硅橡胶层和氟树脂层,该硅橡胶-氟树脂层合体是在硫化硅橡胶层上依次形成含有30~80重量%的环氧树脂和70~20重量%的硅烷偶联剂的含环氧树脂的硅烷系底漆层和氟树脂系底漆层后再形成氟树脂层而构成的。
2.权利要求1所述的硅橡胶-氟树脂层合体,其中,硅烷偶联剂为3-氨基丙基三乙氧基硅烷、乙烯基三乙氧基硅烷或它们的混合物。
3.权利要求1所述的硅橡胶-氟树脂层合体,其中,氟树脂系底漆层是由氟树脂的固体浓度为10~20重量%的水性分散液或有机溶剂分散液形成的。
4.权利要求1所述的硅橡胶-氟树脂层合体,其中,氟树脂层是通过将依次形成有含环氧树脂的硅烷系底漆层和氟树脂系底漆层的基材***氟树脂制管中,之后加热至260~350℃使管收缩而形成的。
5.权利要求1~4中任一项所述的硅橡胶-氟树脂层合体,该层合体被用作复印机的色粉定影部件。
6.复印机的色粉定影部件,该色粉定影部件是由权利要求5所述的硅橡胶-氟树脂层合体形成的。
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