CN113652193B - 一种高强度流淌型硅胶及其制备方法和应用 - Google Patents
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000000741 silica gel Substances 0.000 title claims abstract description 26
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- -1 polymethylphenylsiloxane Polymers 0.000 claims abstract description 29
- 229920002050 silicone resin Polymers 0.000 claims abstract description 25
- 125000003545 alkoxy group Chemical group 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 17
- 229920001921 poly-methyl-phenyl-siloxane Polymers 0.000 claims abstract description 13
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 11
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 229920001296 polysiloxane Polymers 0.000 claims description 7
- 239000006227 byproduct Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- YQGOWXYZDLJBFL-UHFFFAOYSA-N dimethoxysilane Chemical compound CO[SiH2]OC YQGOWXYZDLJBFL-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 239000008213 purified water Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000007822 coupling agent Substances 0.000 claims description 5
- AHUXYBVKTIBBJW-UHFFFAOYSA-N dimethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OC)(OC)C1=CC=CC=C1 AHUXYBVKTIBBJW-UHFFFAOYSA-N 0.000 claims description 5
- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 5
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims 2
- 239000000499 gel Substances 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 abstract description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000853 adhesive Substances 0.000 abstract description 6
- 239000003431 cross linking reagent Substances 0.000 abstract description 6
- 229910000077 silane Inorganic materials 0.000 abstract description 6
- 239000010936 titanium Substances 0.000 abstract description 4
- 229910052719 titanium Inorganic materials 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 18
- 239000011248 coating agent Substances 0.000 description 8
- 238000000576 coating method Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 8
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 7
- 239000003960 organic solvent Substances 0.000 description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 6
- 238000003860 storage Methods 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 4
- 229920002554 vinyl polymer Polymers 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 3
- 150000007529 inorganic bases Chemical class 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 125000003944 tolyl group Chemical group 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
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- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 239000012779 reinforcing material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- YLJJAVFOBDSYAN-UHFFFAOYSA-N dichloro-ethenyl-methylsilane Chemical compound C[Si](Cl)(Cl)C=C YLJJAVFOBDSYAN-UHFFFAOYSA-N 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- CVQVSVBUMVSJES-UHFFFAOYSA-N dimethoxy-methyl-phenylsilane Chemical compound CO[Si](C)(OC)C1=CC=CC=C1 CVQVSVBUMVSJES-UHFFFAOYSA-N 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- ZLNAFSPCNATQPQ-UHFFFAOYSA-N ethenyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)C=C ZLNAFSPCNATQPQ-UHFFFAOYSA-N 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
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- 239000012744 reinforcing agent Substances 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
本发明涉及一种高强度流淌型硅胶及其制备方法和应用。该高强度流淌型硅胶的原料组成包括:烷氧基封端聚甲基苯基硅氧烷100份、烷氧基封端硅树脂25份‑100份、硅烷交联剂4.5份‑10份、硅烷偶联剂0.7份‑2份和含钛催化剂0.15份‑2份。本发明还提供了上述硅胶的制备方法。本发明的硅胶具有高透明度、高强度、高接着强度,可以用于电子/电气设备主板的薄层密封。
Description
技术领域
本发明涉及一种硅胶,尤其涉及一种高强度流淌型硅胶,属于聚合物技术领域。
背景技术
电子/电气设备涂敷硅胶的选择上,主要考虑到以下几个方面:
(1)为了能够更好的涂敷电路板,形成薄层密封,产品要易流平。
(2)作为电子/电气设备主板的涂敷,产品固化过程不能产生腐蚀性的副产物,且要具有高粘接性能。
(3)作为电缆终端、连接器、晶体振荡器及厚薄混合电路板的涂层,产品固化后要具有较好的韧性。
目前市面上的涂敷产品主要有烷氧基封端聚二甲基硅氧烷体系、α-氢-ω-羟基-聚二甲基硅氧烷体系或α-氢-ω-羟基-聚二甲基硅氧烷添加甲基羟基硅树脂补强体系,前两个体系胶体的强度较差(拉伸强度一般只有0.3MPa)、粘接强度低,α-氢-ω-羟基-聚二甲基硅氧烷加硅树脂补强体系需要添加溶剂稀释才可以涂敷,含溶剂不环保且贮存稳定性不好,都不是理想的涂敷材料。
发明内容
为了解决上述技术问题,本发明的目的在于提供一种具有高透明度、高强度和高接着强度的流淌型硅胶及其制备方法。
本发明的另一目的,在于提供一种可以用于电子/电气设备主板的密封。
为了实现上述任一目的,本发明首先提供了一种高强度流淌型硅胶,其中,该高强度流淌型硅胶的原料组成包括以下重量份的组分:烷氧基封端聚甲基苯基硅氧烷100份、烷氧基封端硅树脂25份-100份(优选50份-100份)、硅烷交联剂4.5份-10份、硅烷偶联剂0.7份-2份和含钛催化剂0.15份-2份。
本发明的高强度流淌型硅胶,通过在烷氧基封端聚硅氧烷、烷氧基封端硅树脂中引入苯基基团,可以提高产品硬度;以及,特定的烷氧基封端硅树脂,可以明显的提升产品强度,同时用烷氧基封端的硅树脂作为补强材料,可以使产品保持流淌性,易于浸涂、涂刷电路板。
在本发明的一具体实施方式中,采用的烷氧基封端聚甲基苯基硅氧烷的结构如下式所示:
((RO)2CH3SiCH2CH2)(R1 2SiO)a(CH2CH2 Si CH3(RO)2);
其中,所述R为甲基或乙基;
R1为甲基或苯基,且必含苯基,
50≤a≤200,a为整数。
在本发明的高强度流淌型硅胶中,采用烷氧基硅树脂作为补强剂,在提高产品韧性的同时可以保持产品良好的流淌性,有利于对电子/电气设备主板的涂敷。烷氧基封端的聚硅氧烷和硅树脂的协同作用,在固化过程释放醇类的副物,对电子元件无腐蚀作用,可广泛应用于电子电器及建筑行业,作为一种绿色环保的胶黏剂醇型密封胶符合市场应用的趋势。
在本发明的一具体实施方式中,采用的烷氧基封端硅树脂具有如下的结构:
((RO)2CH3SiCH2CH2)m(R2 2SiO)n(R2SiO1.5)x(SiO2)y;
其中,R为甲基或乙基,
R2为甲基或苯基,且必含苯基,
1.5<(3m+2n+x):(m+n+x+y)<1.9,x、y、m、n均为整数。
在本发明的高强度流淌型硅胶中,烷氧基封端的甲基苯基聚硅氧烷和烷氧基封端(的甲基苯基)硅树脂都是一类以重复的Si-O键为主链,硅原子上直接连有甲基和苯基的聚合物,烷氧基代替硅羟基可以降低在生产过程产生的高峰现象,同时可以提高产品的贮存稳定性,在结构中引入苯基基团,可以提高产品的硬度和对基材的粘接强度。
在本发明的一具体实施方式中,采用的硅烷交联剂为:Rb-Si(OR)4-b,其中R为甲基或乙基,0≦b<4,b为整数。
在本发明的一具体实施方式中,采用的硅烷偶联剂为烷偶联剂为含氨基的硅氧烷。
在本发明的一具体实施方式中,采用的含钛催化剂为钛酸酯催化剂。
本发明还提供了上述高强度流淌型硅胶的制备方法,该制备方法包括以下步骤:
向烷氧基封端聚甲基苯基硅氧烷、烷氧基封端硅树脂中加入硅烷交联剂、硅烷偶联剂和含钛催化剂在高真空下搅拌,得到高强度流淌型硅胶。
在本发明的一具体实施方式中,烷氧基封端聚甲基苯基硅氧烷按照以下步骤制备得到;
将二甲基二甲氧基硅烷、二苯基二甲氧基硅烷、水、有机溶剂、无机碱混合均匀,在70℃-80℃下水解反应4-8小时;其中,所述二甲基二甲氧基硅烷、二苯基二甲氧基硅烷、水、有机溶剂、无机碱的重量比为400-600:800-1200:400-600:600-1000:4-6;
萃取去除水和副产物,抽真空去除溶剂,缓慢升温至90-100℃反应4-6小时,滴加乙烯基封端剂,反应小时1-3小时;加入有机溶剂溶解,水洗至中性,分去下层的水份;
加热至100-120℃回流脱水,脱干水份后冷却至40℃-50℃冷却,加入铂金催化剂分散均匀,滴加甲基氢基二甲氧基硅烷,反应6-10小时,脱去溶剂,得到烷氧基封端聚甲基苯基硅氧烷;其中,甲基氢基二甲氧基硅烷与乙烯基封端剂的质量比为1-1.1:1。
在本发明的一具体实施方式中,制备烷氧基封端聚甲基苯基硅氧烷时,采用的无机碱为氢氧化钾、氢氧化钠或氢氧化锂;采用的有机溶剂为甲苯、二甲苯、环己烷中的一种或几种的组合;采用的乙烯基封端剂为四甲基二乙烯基硅氧烷。
在本发明的一具体实施方式中,采用的烷氧基封端硅树脂的制备方法包括以下步骤:
将两种或两种以上不同结构的有机硅单体、有机溶剂、水、无机碱混合均匀;在60℃-80℃反应5-10小时;水洗至中性,分去水份,得到乙烯基甲基苯基硅树脂溶液;其中,有机硅单体、有机溶剂、水、无机碱的质量比为1400-1600:700-900:600-800:4-6;
将乙烯基甲基苯基硅树脂溶液加热至100-120℃回流脱水,脱干水份后冷却至40℃-50℃冷却,加入铂金催化剂分散均匀,滴加甲基氢基二甲氧基硅烷,反应6-10小时,脱去溶剂,得到烷氧基封端硅树脂树脂;其中,甲基氢基二甲氧基硅烷与乙烯基封端剂的质量比为1-1.1:1。
在本发明的一具体实施方式中,制备烷氧基封端硅树脂时,采用的有机硅单体为六甲基二硅氧烷、甲基乙烯基二甲氧硅烷、甲基乙烯基二氯硅烷、乙烯基三甲氧基硅烷、苯基三乙氧基硅烷、苯基三甲氧基硅烷、甲基苯基二甲氧基硅烷、二苯基二甲氧基硅烷、正硅酸乙酯中的一种或几种的组合;采用的无机碱为氢氧化钾、氢氧化钠或氢氧化锂;采用的有机溶剂为甲苯、二甲苯、环己烷中的一种或几种的组合。
本发明的高强度流淌型硅胶可以用于密封电子/电气设备。
本发明的高强度流淌型硅胶无溶剂,具有高透明度、高强度、高接着强度;主要应用于电子/电气设备主板的薄层密封,固化后形成坚固的保护层,起防潮、防碰撞、保护电子元件的作用。
本发明的高强度流淌型硅胶在烷氧基封端的聚硅氧烷和硅树脂中引入苯基,可以提高产品的硬度和对基材的粘接;同时,烷氧基封端,使产品的贮存期更稳定,同时用烷氧基封端的硅树脂作为补强材料,可以提升产品的透明度和使产品更具流淌性,易于浸涂和涂刷;此外,不含溶剂涂敷液,且催化剂没有用传统的含重金属有机锡,使产品更环保。另外,本发明的高强度流淌型硅胶的贮存稳定,在固化过程放出非腐蚀性副产物,是理想的单组分室温固化硅胶。
具体实施方式
实施例1-5
实施例1-5提供了一种高强度流淌型硅胶,制备方法如下:
1)烷氧基封端甲基苯基聚硅氧烷制备方法包括如下的步骤:
①在5000ml的四口烧瓶中加入500克二甲基二甲氧基硅烷、1000克二苯基二甲氧基硅烷、500克纯净水、800克环己烷、5克氢氧化钾,混合均匀;
②升温至73℃,水解反应5小时;
③萃取分去纯净水和反应副产物,缓慢升温至90℃反应5小时,滴加25克四甲基二乙烯基硅氧烷,反应2小时;
④加入1000克环己烷,水洗至中性,分去下层的水份;
⑤加热回流脱水,冷却至40℃,加入0.2克3000ppm铂金催化剂分散均匀,缓慢滴加25克甲基氢基二甲氧基硅烷,反应6小时,脱去溶剂可得烷氧基封端聚甲基苯基硅氧烷。
2)烷氧基封端硅树脂的制备方法包括如下的步骤:
①在5000ml四口烧瓶中加入六甲基二硅氧烷100g、四甲基二乙烯基硅氧烷117克、甲基三乙氧基硅烷300g、苯基三甲氧基硅烷1000g、环己烷800克、纯净水700克、氢氧化钾5克,搅拌均匀;
②升温至73℃反应6小时;
③萃取去除水份,水洗至中性,分去水份,得乙烯基甲基苯基硅树脂;
④加热回流脱水,冷却至40℃,加入0.2克3000ppm铂金催化剂分散均匀,缓慢滴加120克甲基氢基二甲氧基硅烷,反应6小时,脱去溶剂可得烷氧基封端硅树脂。
3)在烷氧基封端聚甲基苯基硅氧烷和烷氧基封端硅树脂中加入交联剂、偶联剂和钛酸酯催化剂在高真空下搅拌均匀,各材料的配比如表1。
表1
对比例1-3
取市面上普通的烷氧基封端的二甲基聚硅氧烷或者α-氢-ω-羟基-聚二甲基硅氧烷,加入交联剂、偶联剂、钛酸酯催化剂或二丁基月桂酸锡在高真空下搅拌均匀,各材料的配比如表2。
表2
测试结果如表3所示。
表3
从表3中可得出,本发明制备得到的高强度流淌型硅胶具有贮存稳定,拉伸强度大,伸长率大,粘接强度好,硬度高等特点,是理想的涂溥材料,能够广泛应用于电路板中保持电子元件。
上述实施例只为说明本发明的技术构思及特点,其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施,并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰,都应涵盖在本发明的保护范围之内。
Claims (3)
1.一种高强度流淌型硅胶,其中,该高强度流淌型硅胶的原料组成由以下重量份的组分组成:烷氧基封端聚甲基苯基硅氧烷100份、烷氧基封端硅树脂 100份、甲基三甲氧硅烷9份、硅烷偶联剂2份和钛酸酯催化剂2份;
所述烷氧基封端聚甲基苯基硅氧烷的制备方法如下:
(1)在5000ml的四口烧瓶中加入500克二甲基二甲氧基硅烷、1000克二苯基二甲氧基硅烷、500克纯净水、800克环己烷和5克氢氧化钾,混合均匀;
(2)升温至73℃,水解反应5小时;
(3)萃取分去纯净水和反应副产物,缓慢升温至90℃反应 5小时,滴加25克四甲基二乙烯基硅氧烷,反应2小时;
(4)加入1000克环己烷,水洗至中性,分去下层的水分;
(5)加热回流脱水,冷却至40℃,加入0.2克3000ppm铂金催化剂分散均匀,缓慢滴加25克甲基氢基二甲氧基硅烷,反应6小时,脱去溶剂可得烷氧基封端聚甲基苯基硅氧烷;
所述烷氧基封端硅树脂的制备方法如下:
(1)在5000ml四口烧瓶中加入六甲基二硅氧烷100g、四甲基二乙烯基硅氧烷117克、甲基三乙氧基硅烷300g、苯基三甲氧基硅烷1000g、环己烷800克、纯净水700克、氢氧化钾5克,搅拌均匀;
(2)升温至73℃反应6小时;
(3)萃取去除水分, 水洗至中性,分去水分,得乙烯基甲基苯基硅树脂;
(4)加热回流脱水,冷却至40℃,加入0.2克3000ppm铂金催化剂分散均匀,缓慢滴加120克甲基氢基二甲氧基硅烷,反应6小时,脱去溶剂可得烷氧基封端硅树脂;
硅烷偶联剂为偶联剂KH550和偶联剂KH792按质量比1:1组成的混合物。
2.权利要求1所述的高强度流淌型硅胶的制备方法,包括以下步骤:
向烷氧基封端聚甲基苯基硅氧烷、烷氧基封端硅树脂中加入甲基三甲氧硅烷、硅烷偶联剂和钛酸酯催化剂在高真空下搅拌,得到所述高强度流淌型硅胶。
3.权利要求1所述的高强度流淌型硅胶的应用,该高强度流淌型硅胶用于密封电子/电气设备。
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