WO2019051742A1 - 一种紫外线吸收高透明硅橡胶的制备方法 - Google Patents

一种紫外线吸收高透明硅橡胶的制备方法 Download PDF

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WO2019051742A1
WO2019051742A1 PCT/CN2017/101802 CN2017101802W WO2019051742A1 WO 2019051742 A1 WO2019051742 A1 WO 2019051742A1 CN 2017101802 W CN2017101802 W CN 2017101802W WO 2019051742 A1 WO2019051742 A1 WO 2019051742A1
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parts
silicone rubber
stirring
vinyl
silicone oil
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PCT/CN2017/101802
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French (fr)
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韦荣群
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韦荣群
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of 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; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of 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; Compositions of derivatives of such polymers
    • 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
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/12—Polysiloxanes containing silicon bound to hydrogen
    • 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
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups

Definitions

  • the invention relates to a preparation method of ultraviolet absorption high transparent silicone rubber.
  • Optical polymer materials can be used for optical bonding, lens or optical sheets and substrates, and can be used in the following components: optical film, optical filter, CCD optical system, photographic equipment, optical communication and waveguide, optical fiber, light Sensors, holographic optics, interferometers, optical couplers, optical lenses such as microlenses, lenticular lenses, prismatic lenses, Fresnel lenses, and the like.
  • Polymers currently available for the preparation of optical components and their components are: polymethyl methacrylate, polyurethane, polycarbonate, polyvinyl chloride, polystyrene, polyester, epoxy, cycloolefin polymer, silicone Alkane, etc.
  • polysiloxanes have attracted wide attention of researchers due to their excellent high temperature resistance, weather resistance, ultraviolet resistance, aging resistance and the like, and have been produced into various optical sheets, substrates or optical adhesives.
  • Polymer materials such as polymethyl methacrylate and polyvinyl chloride have high light transmittance and are easy to process, but they are prone to aging and deformation when subjected to excessive cooling, overheating, ultraviolet rays or other radiation environments, which may result in a decrease in lens performance stability. It can't even be used.
  • Silicone materials have a series of excellent properties such as excellent weather resistance, high temperature resistance and yellowing resistance, and have obvious advantages over other materials. It has been widely used in the preparation of optical components. For example, a silicone-based optical material can be used in place of the conventional polymethyl acrylate to avoid problems such as poor aging resistance.
  • the silicone material is crosslinked by exposing the uncured silicone composition to an electron beam.
  • this method requires special equipment and is costly. Therefore, development of a polysiloxane composition which can be rapidly vulcanized at room temperature or slightly higher temperature, and at the same time development of a transparent silicone elastomer which can absorb light of a certain region (such as ultraviolet rays) and has outstanding aging resistance. It is of great significance to protect related devices from UV damage.
  • a method for preparing ultraviolet-absorbing high-transparency silicone rubber comprising the steps of: 20-30 parts of vinyl silicone resin, 15-29 parts of vinyl-terminated silicone oil, 0.5-1.5 parts of inhibitor and 0.03-0.07 parts of platinum complex
  • the catalyst was stirred 3-5 times at a rate of 1800 r/min in a high-speed stirrer, stirring for 20-40 s each time; after mixing well, 10-18 parts of hydrogen-containing silicone oil and 1-2 parts of ultraviolet absorber diluted with a solvent were added.
  • the vinyl silicone resin has a weight fraction of 25.
  • it is vulcanized at 42 ° C for 2 h.
  • the silicone rubber prepared by the method provided by the invention can achieve better light transmittance and ultraviolet absorption effect, and the aging resistance effect is also good.
  • a method for preparing ultraviolet-absorbing high-transparency silicone rubber comprising the steps of: 25 parts of vinyl silicone resin, 22 parts of vinyl-terminated silicone oil, 1 part of inhibitor and 0.05 part of platinum complex catalyst in a high-speed stirrer at 1800r Stir 4 times at a rate of /min, stirring for 30 s each time; after mixing thoroughly, add 14 parts of hydrogen-containing silicone oil and 1.5 parts of UV absorber diluted with solvent, stir 6 times at a rate of 1800 r/min, stirring for 30 s each time; The above mixture was vulcanized at 42 ° C for 2 h and cooled to room temperature; each raw material was in parts by weight.
  • a method for preparing ultraviolet-absorbing high-transparency silicone rubber comprising the steps of: 20 parts of vinyl silicone resin, 15 parts of vinyl-terminated silicone oil, 0.5 parts of inhibitor and 0.03 parts of platinum complex catalyst in a high-speed stirrer at 1800r Stir three times at a rate of /min, stirring for 20 s each time; after mixing thoroughly, add 10 parts of hydrogen-containing silicone oil and 1 part of UV absorber diluted with solvent, stir 5 times at a rate of 1800 r/min, stirring for 20 s each time; The above mixture was vulcanized at 40 ° C for 1 h and cooled to room temperature; each raw material was in parts by weight.
  • a method for preparing ultraviolet-absorbing high-transparency silicone rubber comprising the steps of: 30 parts of vinyl silicone resin, 29 parts of vinyl-terminated silicone oil, 1.5 parts of inhibitor and 0.07 parts of platinum complex catalyst in a high-speed stirrer at 1800r Stir at a rate of /min 5 times, stirring for 40 s each time; after mixing thoroughly, add 18 parts of hydrogen-containing silicone oil and 2 parts of UV absorber diluted with solvent, stir 7 times at a rate of 1800 r/min, stirring for 40 s each time; The above mixture was vulcanized at 44 ° C for 3 h and cooled to room temperature; each of the starting materials was in parts by weight.
  • the silicone rubber prepared by the method provided by the invention can achieve better light transmittance and ultraviolet absorption effect, and the aging resistance effect is also good.

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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)
  • Compositions Of Macromolecular Compounds (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

一种紫外线吸收高透明硅橡胶的制备方法，步骤如下：将20-30份乙烯基硅树脂、15-29份乙烯基封端硅油，0.5-1.5份抑制剂和0.03-0.07份铂配合物催化剂在高速搅拌仪中以1800r/min的速率搅拌3-5次，每次搅拌20-40s；充分混合后再加入10-18份含氢硅油和1-2份用溶剂稀释的紫外线吸收剂，以1800r/min的速率搅拌5-7次，每次搅拌20-40s；将以上混合物在40-44℃下硫化1-3h，冷却至室温即得；各原料均为重量份。提供的方法制得的硅橡胶可以实现较好的透光率及紫外线吸收效果，同时耐老化效果也较好。

Description

一种紫外线吸收高透明硅橡胶的制备方法 技术领域
本发明涉及一种紫外线吸收高透明硅橡胶的制备方法。
背景技术
相对于传统无机材料，聚合物材料除了保持传统无机材料的优异性能外，还具有质量轻、成本低、工艺简单、机械性能好等优点。光学聚合物材料可用于光学粘接、制成透镜或光学片材及基片，并可用于以下构件：光学膜、光学过滤器、CCD光学系统、摄影摄像器材、光学通信及波导、光纤、光传感器、全息光学器件、干涉仪、光耦合器、光学透镜如微透镜、双凸透镜、棱透镜、菲涅尔透镜等。目前可用于制备光学元件及其组件的聚合物有：聚甲基丙烯酸甲酯、聚氨酯、聚碳酸酯、聚氯乙烯、聚苯乙烯、聚酯、环氧树脂、环烯烃聚合物、聚硅氧烷等。其中聚硅氧烷由于其优异的耐高低温、耐候性、耐紫外、耐老化等特性而引起研究者广泛的关注，并且被制成多种光学片材、基片或光学粘接剂等。聚甲基丙烯酸甲酯及聚氯乙烯等聚合物材料透光率高，易加工，但在处于过冷、过热、紫外线或其它辐射环境时容易发生老化、变形，会导致透镜性能稳定性下降，甚至无法使用。
有机硅材料具有优异的耐候性、耐高低温性及抗黄变等一系列优良的性能，相比其它材料具有明显优势。目前已广泛应用于制备光学元件。例如，基于聚硅氧烷的光学材料用以代替传统的聚丙烯酸甲酯，可以避免耐老化性差等问题。其中通过使未固化的聚硅氧烷组合物暴露于电子束以使有机硅材料交联。但这种方法需要特殊的装置、成本较高。因此，开发一种在室温或稍高温度下可快速硫化的聚硅氧烷组合物，以及同时开发一种可吸收一定区域光波(如紫外线)且具有突出的耐老化性的透明有机硅弹性体，对于保护相关器件不受紫外线伤害具有很大意义。
发明内容
本发明的目的在于提供一种紫外线吸收高透明硅橡胶的制备方法。
本发明通过下面技术方案实现：
一种紫外线吸收高透明硅橡胶的制备方法，包括如下步骤：将20-30份乙烯基硅树脂、15-29份乙烯基封端硅油，0.5-1.5份抑制剂和0.03-0.07份铂配合物催化剂在高速搅拌仪中以1800r/min的速率搅拌3-5次，每次搅拌20-40s；充分混合后再加入10-18份含氢硅油和1-2份用溶剂稀释的紫外线吸收剂，以1800r/min的速率搅拌5-7次，每次搅拌20-40s；将以上混合物在40-44℃下硫化1-3h，冷却至室温即得；各原料均为重量份。
优选地，乙烯基硅树脂的重量份为25。
优选地，充分混合后再加入14份含氢硅油和1.5份用溶剂稀释的紫外线吸收剂，以1800r/min的速率搅拌6次，每次搅拌30s。
优选地，在42℃下硫化2h。
本发明技术效果：
本发明提供的方法制得的硅橡胶可以实现较好的透光率及紫外线吸收效果，同时耐老化效果也较好。
具体实施方式
下面结合实施例具体介绍本发明的实质性内容。
实施例1
一种紫外线吸收高透明硅橡胶的制备方法，包括如下步骤：将25份乙烯基硅树脂、22份乙烯基封端硅油，1份抑制剂和0.05份铂配合物催化剂在高速搅拌仪中以1800r/min的速率搅拌4次，每次搅拌30s；充分混合后再加入14份含氢硅油和1.5份用溶剂稀释的紫外线吸收剂，以1800r/min的速率搅拌6次，每次搅拌30s；将以上混合物在42℃下硫化2h，冷却至室温即得；各原料均为重量份。
实施例2
一种紫外线吸收高透明硅橡胶的制备方法，包括如下步骤：将20份乙烯基硅树脂、15份乙烯基封端硅油，0.5份抑制剂和0.03份铂配合物催化剂在高速搅拌仪中以1800r/min的速率搅拌3次，每次搅拌20s；充分混合后再加入10份含氢硅油和1份用溶剂稀释的紫外线吸收剂，以1800r/min的速率搅拌5次，每次搅拌20s；将以上混合物在40℃下硫化1h，冷却至室温即得；各原料均为重量份。
实施例3
一种紫外线吸收高透明硅橡胶的制备方法，包括如下步骤：将30份乙烯基硅树脂、29份乙烯基封端硅油，1.5份抑制剂和0.07份铂配合物催化剂在高速搅拌仪中以1800r/min的速率搅拌5次，每次搅拌40s；充分混合后再加入18份含氢硅油和2份用溶剂稀释的紫外线吸收剂，以1800r/min的速率搅拌7次，每次搅拌40s；将以上混合物在44℃下硫化3h，冷却至室温即得；各原料均为重量份。
本发明提供的方法制得的硅橡胶可以实现较好的透光率及紫外线吸收效果，同时耐老化效果也较好。

Claims (4)

  1. 一种紫外线吸收高透明硅橡胶的制备方法，其特征在于包括如下步骤：将20-30份乙烯基硅树脂、15-29份乙烯基封端硅油，0.5-1.5份抑制剂和0.03-0.07份铂配合物催化剂在高速搅拌仪中以1800r/min的速率搅拌3-5次，每次搅拌20-40s；充分混合后再加入10-18份含氢硅油和1-2份用溶剂稀释的紫外线吸收剂，以1800r/min的速率搅拌5-7次，每次搅拌20-40s；将以上混合物在40-44℃下硫化1-3h，冷却至室温即得；各原料均为重量份。
  2. 根据权利要求1所述的制备方法，其特征在于：乙烯基硅树脂的重量份为25。
  3. 根据权利要求1所述的制备方法，其特征在于：充分混合后再加入14份含氢硅油和1.5份用溶剂稀释的紫外线吸收剂，以1800r/min的速率搅拌6次，每次搅拌30s。
  4. 根据权利要求1所述的制备方法，其特征在于：在42℃下硫化2h。
PCT/CN2017/101802 2017-09-14 2017-09-15 一种紫外线吸收高透明硅橡胶的制备方法 WO2019051742A1 (zh)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101016446A (zh) * 2007-02-15 2007-08-15 东莞市贝特利新材料有限公司 一种有机硅电子灌封材料
CN103122149A (zh) * 2013-03-18 2013-05-29 株洲时代新材料科技股份有限公司 光学封装用高折射率高透明硅橡胶及其制备方法
CN106380862A (zh) * 2016-10-26 2017-02-08 三友（天津）高分子技术有限公司 紫外发光二极管封装用有机聚硅氧烷组合物及制备方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101016446A (zh) * 2007-02-15 2007-08-15 东莞市贝特利新材料有限公司 一种有机硅电子灌封材料
CN103122149A (zh) * 2013-03-18 2013-05-29 株洲时代新材料科技股份有限公司 光学封装用高折射率高透明硅橡胶及其制备方法
CN106380862A (zh) * 2016-10-26 2017-02-08 三友（天津）高分子技术有限公司 紫外发光二极管封装用有机聚硅氧烷组合物及制备方法

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