CN106349460A - High-temperature-resistant organic silicon-modified epoxy resin and method for preparing same - Google Patents
High-temperature-resistant organic silicon-modified epoxy resin and method for preparing same Download PDFInfo
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- CN106349460A CN106349460A CN201610806514.5A CN201610806514A CN106349460A CN 106349460 A CN106349460 A CN 106349460A CN 201610806514 A CN201610806514 A CN 201610806514A CN 106349460 A CN106349460 A CN 106349460A
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 54
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 3
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 10
- WSFQLUVWDKCYSW-UHFFFAOYSA-M sodium;2-hydroxy-3-morpholin-4-ylpropane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(O)CN1CCOCC1 WSFQLUVWDKCYSW-UHFFFAOYSA-M 0.000 claims description 10
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 9
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 5
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 4
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 2
- 229960004889 salicylic acid Drugs 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 3
- 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 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 125000003944 tolyl group Chemical group 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract description 7
- 230000032683 aging Effects 0.000 abstract description 4
- 239000008204 material by function Substances 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 10
- 238000000354 decomposition reaction Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229920002050 silicone resin Polymers 0.000 description 5
- 239000003973 paint Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000007385 chemical modification Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 230000004224 protection Effects 0.000 description 2
- 239000002966 varnish Substances 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004634 thermosetting polymer Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
- C08G59/1438—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Emergency Medicine (AREA)
- General Chemical & Material Sciences (AREA)
- Epoxy Resins (AREA)
- Silicon Polymers (AREA)
Abstract
本发明属于高分子功能材料领域，公开了一种耐高温有机硅改性环氧树脂及其制备方法。所述制备方法为：按重量份计，将10～25份有机硅中间体、15～60环氧树脂、25～75溶剂依次加入到反应器中，搅拌并加热升温到70～80℃，待其混合均匀后，加入催化剂，然后加热升温到95～185℃反应2～8h，降温后得到所述耐高温有机硅改性环氧树脂。本发明制备工艺简单，所制备的有机硅改性环氧树脂具有耐高温、耐紫外老化、硬度高、储存稳定性好等特性。
The invention belongs to the field of polymer functional materials, and discloses a high-temperature-resistant organosilicon-modified epoxy resin and a preparation method thereof. The preparation method is as follows: in parts by weight, 10-25 parts of organosilicon intermediate, 15-60 parts of epoxy resin, and 25-75 parts of solvent are sequentially added to the reactor, stirred and heated to 70-80 °C, and wait for After mixing evenly, add a catalyst, then heat up to 95-185° C. to react for 2-8 hours, and obtain the high-temperature-resistant organosilicon-modified epoxy resin after cooling down. The preparation process of the invention is simple, and the prepared silicone modified epoxy resin has the characteristics of high temperature resistance, ultraviolet aging resistance, high hardness, good storage stability and the like.
Description
技术领域technical field
本发明属于高分子功能材料领域，具体涉及一种耐高温有机硅改性环氧树脂及其制备方法。The invention belongs to the field of polymer functional materials, and in particular relates to a high-temperature-resistant organosilicon-modified epoxy resin and a preparation method thereof.
背景技术Background technique
环氧树脂是指含有两个或两个以上环氧基团，并能通过环氧基团反应形成有用的热固性的高分子材料，它具有优异的电气性能、优良的附着力、较好的力学性能、良好的耐腐蚀性和耐化学药品性，在电子电气、机械加工、土木建筑、航空航天等众多领域有着广泛的应用。但是，环氧树脂由于碳-碳键、碳-氧键键能较低，高温下易分解，经紫外光照射后，易降解断链，严重限制了环氧树脂的应用。Epoxy resin refers to a polymer material that contains two or more epoxy groups and can form useful thermosetting polymer materials through the reaction of epoxy groups. It has excellent electrical properties, excellent adhesion, and good mechanical properties. Performance, good corrosion resistance and chemical resistance, it has a wide range of applications in many fields such as electrical and electronic, mechanical processing, civil engineering, aerospace and so on. However, due to the low carbon-carbon bond and carbon-oxygen bond energy of epoxy resin, it is easy to decompose at high temperature, and it is easy to degrade and break the chain after being irradiated by ultraviolet light, which seriously limits the application of epoxy resin.
有机硅树脂由于Si-O的键能为460kJ/mol，使得有机硅树脂具有优异的耐热性能，同时硅树脂还具有良好的耐候性、耐紫外老化、表面能低等优点。通过有机硅树脂的活性基团与环氧树脂的活性基团进行反应，实现环氧树脂的化学改性，制备的有机硅改性环氧树脂具有耐高温、耐紫外老化等特性。Since the bond energy of Si-O is 460kJ/mol, the silicone resin has excellent heat resistance, and the silicone resin also has the advantages of good weather resistance, UV aging resistance, and low surface energy. The chemical modification of the epoxy resin is realized by reacting the active groups of the silicone resin and the active groups of the epoxy resin, and the prepared silicone-modified epoxy resin has the characteristics of high temperature resistance, ultraviolet aging resistance and the like.
专利CN101525466和专利CN101085855用环氧树脂、有机硅树脂通过简单物理混合得到有机硅环氧树脂组合物。此组合物具有优良的抗紫外、抗高温性能，但是存在严重的相容性问题，同时主链上缺少有机硅链，对环氧树脂的性能改善有限。化学改性能很好地解决相容性问题。专利CN10253255A利用线性结构的有机硅树脂对环氧树脂进行化学改性，解决了两者之间相容性不好的问题，但是此制备方法，温度低时，反应时间长；温度高时，有机硅又会发生自身缩聚反应。Patent CN101525466 and patent CN101085855 use epoxy resin and silicone resin to obtain silicone epoxy resin composition through simple physical mixing. This composition has excellent anti-ultraviolet and high-temperature resistance properties, but there are serious compatibility problems, and at the same time, there is a lack of organic silicon chains on the main chain, so the improvement of the performance of epoxy resin is limited. Chemical modification can solve the compatibility problem very well. Patent CN10253255A utilizes linear structure silicone resin to chemically modify epoxy resin, which solves the problem of poor compatibility between the two, but this preparation method, when the temperature is low, the reaction time is long; when the temperature is high, the organic Silicon undergoes self-condensation reaction.
发明内容Contents of the invention
为了解决以上现有技术的缺点和不足之处，本发明的首要目的在于提供一种耐高温有机硅改性环氧树脂的制备方法。In order to solve the above shortcomings and deficiencies of the prior art, the primary purpose of the present invention is to provide a method for preparing a high-temperature-resistant silicone-modified epoxy resin.
本发明的另一目的在于提供一种通过上述方法制备得到的耐高温有机硅改性环氧树脂。Another object of the present invention is to provide a high temperature resistant silicone modified epoxy resin prepared by the above method.
本发明目的通过以下技术方案实现：The object of the invention is achieved through the following technical solutions:
一种耐高温有机硅改性环氧树脂的制备方法，包括如下制备步骤：A preparation method of high-temperature-resistant organosilicon-modified epoxy resin, comprising the following preparation steps:
按重量份计，将10～25份有机硅中间体、15～60环氧树脂、25～75溶剂依次加入到反应器中，搅拌并加热升温到70～80℃，待其混合均匀后，加入催化剂，然后加热升温到95～185℃反应2～8h，降温后得到所述耐高温有机硅改性环氧树脂。In parts by weight, add 10-25 parts of organosilicon intermediate, 15-60 parts of epoxy resin, and 25-75 parts of solvent into the reactor in sequence, stir and heat up to 70-80 ° C, after they are mixed evenly, add catalyst, and then heated up to 95-185° C. to react for 2-8 hours, and the high-temperature-resistant organosilicon-modified epoxy resin was obtained after cooling down.
所述有机硅中间体选自如下结构通式的化合物：The organosilicon intermediate is selected from compounds of the following general structural formula:
其中X和Y相同或不同，选自C1～C6的直链或支链烷基或苯基；Wherein X and Y are the same or different, and are selected from C 1 to C 6 linear or branched alkyl or phenyl;
其中R’和R”相同或不同，选自H、CH3或CH3CH2。Wherein R' and R" are the same or different, and are selected from H, CH 3 or CH 3 CH 2 .
优选地，所述有机硅中间体为瓦克IC-368、瓦克SY-231、瓦克SY-300、道康宁RSN-6018、道康宁LX-0301中的至少一种；更优选道康宁RSN-6018。Preferably, the silicone intermediate is at least one of Wacker IC-368, Wacker SY-231, Wacker SY-300, Dow Corning RSN-6018, and Dow Corning LX-0301; more preferably Dow Corning RSN-6018.
优选地，所述环氧树脂为双酚A型环氧树脂E20、E21、E42、E44、E51中的至少一种；更优选为双酚A型环氧树脂E20。Preferably, the epoxy resin is at least one of bisphenol A epoxy resins E20, E21, E42, E44, E51; more preferably bisphenol A epoxy resin E20.
优选地，所述的溶剂为甲苯、二甲苯、丁酮、环己酮、乙酸乙酯、乙酸丁酯中的至少一种；更优选为环己酮与乙酸丁酯的混合物。Preferably, the solvent is at least one of toluene, xylene, butanone, cyclohexanone, ethyl acetate, and butyl acetate; more preferably a mixture of cyclohexanone and butyl acetate.
优选地，所述的催化剂为二月桂酸二丁基锡、环烷酸锌、硝酸、水杨酸、四甲基氢氧化铵中的至少一种；更优选为环烷酸锌。Preferably, the catalyst is at least one of dibutyltin dilaurate, zinc naphthenate, nitric acid, salicylic acid and tetramethylammonium hydroxide; more preferably zinc naphthenate.
本发明所述的有机硅改性环氧树脂的反应原理图如图1所示。The reaction schematic diagram of the organosilicon-modified epoxy resin of the present invention is shown in FIG. 1 .
一种耐高温有机硅改性环氧树脂，通过上述方法制备得到。A high-temperature-resistant organosilicon-modified epoxy resin is prepared by the above-mentioned method.
相对于现有技术，本发明具有如下优点及有益效果：Compared with the prior art, the present invention has the following advantages and beneficial effects:
(1)本发明提供的制备方法，仅仅需要一步即可完成，反应快速、高效，工艺简单，条件易于控制；(1) The preparation method provided by the present invention can be completed in only one step, the reaction is fast and efficient, the process is simple, and the conditions are easy to control;
(2)本发明提供的有机硅中间体，苯基含量高，提高了有机硅组分的溶解度参数，增加了与环氧树脂的相容性，使得产品具有很好的储存稳定性；同时，高含量的苯基也提高了产品的耐温性能；(2) The organosilicon intermediate provided by the present invention has a high phenyl content, improves the solubility parameter of the organosilicon component, increases the compatibility with epoxy resin, and makes the product have good storage stability; meanwhile, The high content of phenyl also improves the temperature resistance of the product;
(3)本发明制备的有机硅改性环氧树脂，除了耐高温、储存稳定性好外，还具有耐紫外老化、硬度高等特点，给予基材多重保护。(3) In addition to high temperature resistance and good storage stability, the organosilicon-modified epoxy resin prepared by the present invention also has the characteristics of ultraviolet aging resistance and high hardness, and provides multiple protections for the substrate.
附图说明Description of drawings
图1为本发明所述有机硅改性环氧树脂的反应原理图。Fig. 1 is a schematic diagram of the reaction of the silicone-modified epoxy resin of the present invention.
具体实施方式detailed description
下面结合实施例对本发明作进一步详细的描述，但本发明的实施方式不限于此。The present invention will be further described in detail below in conjunction with examples, but the embodiments of the present invention are not limited thereto.
以下实施例测试结果参照以下测试标准：Following embodiment test result is with reference to following test standard:
色漆和清漆铅笔法测定漆膜硬度，GB/T 6739-2006；Determination of paint film hardness by pencil method for paints and varnishes, GB/T 6739-2006;
色漆和清漆漆膜的划格实验测定漆膜附着力，GB/T 9286-1998。Determination of paint film adhesion by cross-cut test of paint and varnish films, GB/T 9286-1998.
实施例1Example 1
取10g有机硅中间体道康宁RSN-6018，15g环氧树脂E20，25g环己酮与乙酸丁酯的混合物，依次加入到洁净的500ml四口烧瓶中，缓慢搅拌并加热升温到75℃，待其混合均匀后，加入0.05g环烷酸锌，然后加热升温到125℃，反应4.5h，并不断分出反应过程中生成的水，降温得到有机硅改性环氧树脂。Take 10g of silicone intermediate Dow Corning RSN-6018, 15g of epoxy resin E20, and 25g of a mixture of cyclohexanone and butyl acetate, and add them to a clean 500ml four-necked flask in sequence, stir slowly and heat up to 75°C, and wait for After mixing evenly, add 0.05g of zinc naphthenate, then heat up to 125°C, react for 4.5h, and continuously separate the water generated during the reaction, and lower the temperature to obtain a silicone-modified epoxy resin.
所得产品技术指标：Obtained product technical indicators:
起始分解温度：320℃；Initial decomposition temperature: 320°C;
硬度：5H；Hardness: 5H;
附着力：一级。Adhesion: Grade 1.
实施例2Example 2
取10g有机硅中间体道康宁RSN-6018，30g环氧树脂E20，40g环己酮与乙酸丁酯的混合物，依次加入到洁净的500ml四口烧瓶中，缓慢搅拌并加热升温到75℃，待其混合均匀后，加入0.1g环烷酸锌，然后加热升温到145℃，反应5.5h，并不断分出反应过程中生成的水，降温得到有机硅改性环氧树脂。Take 10g of silicone intermediate Dow Corning RSN-6018, 30g of epoxy resin E20, and 40g of a mixture of cyclohexanone and butyl acetate, and add them to a clean 500ml four-neck flask in turn, stir slowly and heat up to 75°C, and wait for After mixing evenly, add 0.1 g of zinc naphthenate, then heat up to 145° C., react for 5.5 hours, and continuously separate out the water generated during the reaction, and lower the temperature to obtain a silicone-modified epoxy resin.
所得产品技术指标：Obtained product technical indicators:
起始分解温度：280℃；Initial decomposition temperature: 280°C;
硬度：5H；Hardness: 5H;
附着力：一级。Adhesion: Grade 1.
实施例3Example 3
取10g有机硅中间体道康宁RSN-6018，45g环氧树脂E20，55g环己酮与乙酸丁酯的混合物，依次加入到洁净的500ml四口烧瓶中，缓慢搅拌并加热升温到75℃，待其混合均匀后，加入0.13g环烷酸锌，然后加热升温到155℃，反应6h，并不断分出反应过程中生成的水，降温得到有机硅改性环氧树脂。Take 10g of silicone intermediate Dow Corning RSN-6018, 45g of epoxy resin E20, and 55g of a mixture of cyclohexanone and butyl acetate, and add them to a clean 500ml four-necked flask in turn, stir slowly and heat up to 75°C, and wait for After mixing evenly, add 0.13 g of zinc naphthenate, then heat up to 155° C., react for 6 hours, and continuously separate out the water generated during the reaction, and cool down to obtain a silicone-modified epoxy resin.
所得产品技术指标：Obtained product technical indicators:
起始分解温度：240℃；Initial decomposition temperature: 240°C;
硬度4H；Hardness 4H;
附着力：0级。Adhesion: Level 0.
实施例4Example 4
取10g有机硅中间体道康宁RSN-6018，60g环氧树脂E20，70g环己酮与乙酸丁酯的混合物，依次加入到洁净的500ml四口烧瓶中，缓慢搅拌并加热升温到75℃，待其混合均匀后，加入0.14g环烷酸锌，然后加热升温到115℃，反应4h，并不断分出反应过程中生成的水，降温得到有机硅改性环氧树脂。Take 10g of silicone intermediate Dow Corning RSN-6018, 60g of epoxy resin E20, and 70g of a mixture of cyclohexanone and butyl acetate, and add them to a clean 500ml four-necked flask in sequence, stir slowly and heat up to 75°C, and wait for After mixing evenly, add 0.14 g of zinc naphthenate, then heat up to 115° C., react for 4 hours, and continuously separate out the water generated during the reaction, and lower the temperature to obtain a silicone-modified epoxy resin.
所得产品技术指标：Obtained product technical indicators:
起始分解温度：220℃；Initial decomposition temperature: 220°C;
硬度：4H；Hardness: 4H;
附着力：0级。Adhesion: Level 0.
实施例5Example 5
按照配制方案取25g有机硅中间体道康宁RSN-6018，15g环氧树脂E20，40g环己酮与乙酸丁酯的混合物，依次加入到洁净的500ml四口烧瓶中，缓慢搅拌并加热升温到75℃，待其混合均匀后，加入0.08g环烷酸锌，然后加热升温到135℃，反应5h，并不断分出反应过程中生成的水，降温得到有机硅改性环氧树脂。According to the preparation plan, take 25g of silicone intermediate Dow Corning RSN-6018, 15g of epoxy resin E20, and 40g of a mixture of cyclohexanone and butyl acetate, and add them to a clean 500ml four-necked flask in turn, stir slowly and heat up to 75°C , after it is mixed evenly, add 0.08g zinc naphthenate, then heat up to 135°C, react for 5h, and continuously separate the water generated in the reaction process, and cool down to obtain a silicone modified epoxy resin.
所得产品技术指标：Obtained product technical indicators:
起始分解温度：360℃；Initial decomposition temperature: 360°C;
硬度：5H；Hardness: 5H;
附着力：二级。Adhesion: Grade II.
实施例6Example 6
取20g有机硅中间体道康宁RSN-6018，55g环氧树脂E20，75g环己酮与乙酸丁酯的混合物，依次加入到洁净的500ml四口烧瓶中，缓慢搅拌并加热升温到75℃，待其混合均匀后，加入0.15g环烷酸锌，然后加热升温到170℃，反应7h，并不断分出反应过程中生成的水，降温得到有机硅改性环氧树脂。Take 20g of silicone intermediate Dow Corning RSN-6018, 55g of epoxy resin E20, and 75g of a mixture of cyclohexanone and butyl acetate, and add them to a clean 500ml four-necked flask in turn, stir slowly and heat up to 75°C, and wait for After mixing evenly, add 0.15g of zinc naphthenate, then heat up to 170°C, react for 7 hours, and continuously separate the water generated during the reaction, and lower the temperature to obtain a silicone-modified epoxy resin.
所得产品技术指标：Obtained product technical indicators:
起始分解温度：280℃；Initial decomposition temperature: 280°C;
硬度：4H；Hardness: 4H;
附着力：0级。Adhesion: Level 0.
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其它的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。The above-mentioned embodiment is a preferred embodiment of the present invention, but the embodiment of the present invention is not limited by the above-mentioned embodiment, and any other changes, modifications, substitutions, combinations, Simplifications should be equivalent replacement methods, and all are included in the protection scope of the present invention.
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