CN106751346A - 含氟单体改性有机硅封装材料的合成方法 - Google Patents
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Abstract
本发明涉及合成橡胶工业技术领域，具体涉及一种含氟单体改性有机硅封装材料的合成方法。含氟单体改性有机硅封装材料的合成方法，将乙烯基聚硅氧烷和偶联剂加入到密闭的四口烧瓶中，常温下后升温，滴加溶有含氟甲基丙烯酸庚酯单体和甲苯混合液，继续搅拌直至溶液透明无分层现象存在；降温，减压蒸馏除去甲苯溶剂，然后冷却至室温；将改性乙烯基聚硅氧烷与MVQ树脂、铂金水催化剂及稀释剂加入到密闭四口瓶中，在常温下搅拌后加入含氢聚硅氧烷和偶联剂，继续搅拌，经超声和脱泡后制得密封保存的透明液体，即得透明有机硅封装材料。本发明透光率达到85％以上，且具有较好的耐紫外辐射性能和热性能，同时涂层表面的疏水性可起到防污防潮的作用。
Description
技术领域
本发明涉及合成橡胶工业技术领域，具体涉及一种含氟单体改性有机硅封装材料的合成方法。
背景技术
功率型半导体发光二极管是近年开发的一种新型“绿色固体照明”光源，因其具有节能高效、环保及使用寿命长等优点，已在工业领域得到广泛应用。研究表明，高亮度白光LED有望取代传统白炽灯应用于普通家庭的照明，但这也对LED封装所使用的材料提出了更高要求。白光LED使用的封装材料要求具有高透光率和耐紫外老化性能，这些性能与其结构有着必然联系。
传统LED主要是采用环氧树脂作为封装材料，其固化后交联密度大并形成三维网状结构，性能非常优异。但同时其也存在内应力大、高温易破裂及耐紫外老化性能弱等弊端。近年来有机硅材料的开发与应用为LED的发展提供了新的机遇，其优异的耐热性、耐候性及透光性等大幅度提高了LED的发光效率和使用寿命。该封装材料的耐紫外老化功能主要是通过向有机硅聚合物分子中引入苯基基团来实现，该基团可有效屏蔽紫外线、提高材料的折射率。但由于苯基基团易发黄，且制备工艺复杂、价格昂贵，不利于其应用范围的拓展。目前国内使用的封装材料主要是进口硅树脂（美国道康宁、日本信越公司等生产），因此开发高性能的有机硅封装材料具有重要意义。氟硅化合物的介电常数和极化因子很小，且分子空间结构稳定，对碳碳键具有很好的紫外屏蔽作用。此前国内外主要报道了含氟材料应用于织物和太阳能产品的封装，但有关在ＬＥＤ封装上的应用并不多见。
发明内容
本发明旨在提出一种含氟单体改性有机硅封装材料的合成方法。
本发明的技术方案在于：
含氟单体改性有机硅封装材料的合成方法，包括如下步骤：
（1）含氟单体改性乙烯基聚硅氧烷的制备
将50~60g的乙烯基聚硅氧烷和偶联剂加入到密闭的四口烧瓶中，常温下均匀搅拌0.5~1h后升温至45～55℃，边搅拌边滴加溶有2~2.2g含氟甲基丙烯酸庚酯单体和2~2.5g催化剂的甲苯混合液，反应2~2.5h后继续搅拌直至溶液透明无分层现象存在；降温至30~33℃，减压蒸馏除去甲苯溶剂并保温1~1.2h，然后冷却至室温，真空脱泡后密封保存；
（2）透明有机硅封装材料的制备
将35~40g改性乙烯基聚硅氧烷与8~10g的MVQ树脂、0.5~1g铂金水催化剂及稀释剂加入到有氮气保护的密闭四口瓶中，在常温下搅拌1~1.5ｈ后加入18~20g含氢聚硅氧烷和1~1.2g的偶联剂，继续均匀搅拌4~4.5h，经超声和脱泡后制得密封保存的透明液体，将其置于150~180℃的真空加热烘干箱中固化3~4h，即得透明有机硅封装材料。
所述的偶联剂为A151。
所述的步骤（1）中甲苯中的催化剂为二月桂酸二丁基锡。
所述的脱泡为真空脱泡。
本发明的技术效果在于：
本发明以含氟单体改性的端乙烯基聚硅氧烷为基础聚合物，通过引入ＭＶＱ树脂可以制备用于LED封装的透明有机硅材料。有机硅封装材料的力学性能较好，透光率达到85％以上，且具有较好的耐紫外辐射性能和热性能，同时涂层表面的疏水性可起到防污防潮的作用。
具体实施方式
含氟单体改性有机硅封装材料的合成方法，包括如下步骤：
实施例1
（1）含氟单体改性乙烯基聚硅氧烷的制备
将50g的乙烯基聚硅氧烷和偶联剂加入到密闭的四口烧瓶中，常温下均匀搅拌0.5h后升温至45℃，边搅拌边滴加溶有2g含氟甲基丙烯酸庚酯单体和2g催化剂的甲苯混合液，反应2h后继续搅拌直至溶液透明无分层现象存在；降温至30℃，减压蒸馏除去甲苯溶剂并保温1h，然后冷却至室温，真空脱泡后密封保存；
（2）透明有机硅封装材料的制备
将35g改性乙烯基聚硅氧烷与8g的MVQ树脂、0.5g铂金水催化剂及稀释剂加入到有氮气保护的密闭四口瓶中，在常温下搅拌1ｈ后加入18g含氢聚硅氧烷和1g的偶联剂，继续均匀搅拌4h，经超声和脱泡后制得密封保存的透明液体，将其置于150℃的真空加热烘干箱中固化3h，即得透明有机硅封装材料。
其中，所述的偶联剂为A151。所述的步骤（1）中甲苯中的催化剂为二月桂酸二丁基锡。所述的脱泡为真空脱泡。
实施例2
实施例1
（1）含氟单体改性乙烯基聚硅氧烷的制备
将60g的乙烯基聚硅氧烷和偶联剂加入到密闭的四口烧瓶中，常温下均匀搅拌1h后升温至55℃，边搅拌边滴加溶有2.2g含氟甲基丙烯酸庚酯单体和2.5g催化剂的甲苯混合液，反应2.5h后继续搅拌直至溶液透明无分层现象存在；降温至33℃，减压蒸馏除去甲苯溶剂并保温1.2h，然后冷却至室温，真空脱泡后密封保存；
（2）透明有机硅封装材料的制备
将40g改性乙烯基聚硅氧烷与10g的MVQ树脂、1g铂金水催化剂及稀释剂加入到有氮气保护的密闭四口瓶中，在常温下搅拌1~1.5ｈ后加入18~20g含氢聚硅氧烷和1.2g的偶联剂，继续均匀搅拌4.5h，经超声和脱泡后制得密封保存的透明液体，将其置于180℃的真空加热烘干箱中固化4h，即得透明有机硅封装材料。
其中，所述的偶联剂为A151。所述的步骤（1）中甲苯中的催化剂为二月桂酸二丁基锡。所述的脱泡为真空脱泡。
Claims (4)
1.含氟单体改性有机硅封装材料的合成方法，其特征在于：包括如下步骤：
（1）含氟单体改性乙烯基聚硅氧烷的制备
将50~60g的乙烯基聚硅氧烷和偶联剂加入到密闭的四口烧瓶中，常温下均匀搅拌0.5~1h后升温至45～55℃，边搅拌边滴加溶有2~2.2g含氟甲基丙烯酸庚酯单体和2~2.5g催化剂的甲苯混合液，反应2~2.5h后继续搅拌直至溶液透明无分层现象存在；降温至30~33℃，减压蒸馏除去甲苯溶剂并保温1~1.2h，然后冷却至室温，真空脱泡后密封保存；
（2）透明有机硅封装材料的制备
将35~40g改性乙烯基聚硅氧烷与8~10g的MVQ树脂、0.5~1g铂金水催化剂及稀释剂加入到有氮气保护的密闭四口瓶中，在常温下搅拌1~1.5ｈ后加入18~20g含氢聚硅氧烷和1~1.2g的偶联剂，继续均匀搅拌4~4.5h，经超声和脱泡后制得密封保存的透明液体，将其置于150~180℃的真空加热烘干箱中固化3~4h，即得透明有机硅封装材料。
2.根据权利要求1所述的含氟单体改性有机硅封装材料的合成方法，其特征在于：所述的偶联剂为A151。
3.根据权利要求1所述的含氟单体改性有机硅封装材料的合成方法，其特征在于：所述的步骤（1）中甲苯中的催化剂为二月桂酸二丁基锡。
4.根据权利要求1所述的含氟单体改性有机硅封装材料的合成方法，其特征在于：所述的脱泡为真空脱泡。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107325370A (zh) * | 2017-07-11 | 2017-11-07 | 苏州南尔材料科技有限公司 | 一种复合有机硅封装材料的制备方法 |
| CN107868339A (zh) * | 2017-11-30 | 2018-04-03 | 苏州南尔材料科技有限公司 | 一种复合有机硅封装材料的制备方法 |
| CN107936368A (zh) * | 2017-11-26 | 2018-04-20 | 苏州南尔材料科技有限公司 | 一种复合导电封装材料的制备方法 |
| CN108034257A (zh) * | 2017-12-08 | 2018-05-15 | 华南师范大学 | 一种有机硅水下封装材料及其制备方法 |
| CN117801775A (zh) * | 2024-01-15 | 2024-04-02 | 华中科技大学 | 氟化硅氧烷封装剂及其制备方法和应用 |
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2016
- 2016-11-24 CN CN201611043032.5A patent/CN106751346A/zh active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107325370A (zh) * | 2017-07-11 | 2017-11-07 | 苏州南尔材料科技有限公司 | 一种复合有机硅封装材料的制备方法 |
| CN107936368A (zh) * | 2017-11-26 | 2018-04-20 | 苏州南尔材料科技有限公司 | 一种复合导电封装材料的制备方法 |
| CN107868339A (zh) * | 2017-11-30 | 2018-04-03 | 苏州南尔材料科技有限公司 | 一种复合有机硅封装材料的制备方法 |
| CN108034257A (zh) * | 2017-12-08 | 2018-05-15 | 华南师范大学 | 一种有机硅水下封装材料及其制备方法 |
| CN108034257B (zh) * | 2017-12-08 | 2022-05-31 | 华南师范大学 | 一种有机硅水下封装材料及其制备方法 |
| CN117801775A (zh) * | 2024-01-15 | 2024-04-02 | 华中科技大学 | 氟化硅氧烷封装剂及其制备方法和应用 |
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