Method for synthesizing epoxy modified organosiloxane

A technology for organosiloxane and epoxy modification, which is applied in the field of synthesizing epoxy-modified organosiloxane, which can solve problems such as loss of activity, reduce inconsistency, improve stability and storage, and facilitate reaction conditions The effect of control

Inactive Publication Date: 2014-09-03
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, only sulfur-containing platinum and rhodium catalysts are active in the presence of tertiary amines, while other commonly used silicon hydrogen catalysts, such as Wilkinson catalyst (RhCl((C6H5) 3 P) 3 ), Lamoreaux catalyst (H 2 PtCl 6 Octanol solution), Spaier catalyst (chloroplatinic acid) and Karstedt catalyst (Pt-siloxane complex), etc., will lose activity under the action of tertiary amine

Method used

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  • Method for synthesizing epoxy modified organosiloxane
  • Method for synthesizing epoxy modified organosiloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 3g of 1,2-epoxy-4-vinylcyclohexane to a 100ml three-necked flask equipped with a mechanical stirring device and a thermometer, add 15ml of toluene as a solvent, add 3g of ethanol as a stabilizer, add 0.17g of chloroplatinic acid- Divinyltetramethyldisiloxane complex catalyst (also known as Karstedt's catalyzer, the mass content of Pt is 2.6%), at reaction temperature is that this mixture is stirred at 80 ℃, uses dropping funnel to drop 15ml toluene and simultaneously 20g structure is MD 80 D. 6 H M mixed solution of polydimethylsiloxane. After 8 hours of reaction at 80° C., the hydrosilylation reaction can be completed. Examination of the product using infrared spectroscopy revealed complete disappearance of the silicon hydrogen peak. The mixture was vacuum distilled at 50° C. for 1 hour to remove light fractions to obtain 21.4 g of an epoxy-modified organosiloxane product. The epoxy equivalent weight of the product was determined to be 1090.

Embodiment 2

[0033] Add 20g of the structure MD to a 100ml three-neck flask equipped with a mechanical stirring device and a thermometer. 80 D. 6 HM polydimethylhydrogen silicone oil, add 15ml toluene as solvent, do not add any lower alcohol as stabilizer, add 0.17g chloroplatinic acid-divinyltetramethyldisiloxane complex catalyst (also known as Karstedt's catalyst), the mixture was stirred at a reaction temperature of 80° C., and a mixed solution of 15 ml of toluene and 3 g of 1,2-epoxy-4-vinylcyclohexane was added dropwise using a dropping funnel. After reacting for 80 minutes, the system gelled immediately and the reaction could not be continued.

Embodiment 3

[0035] Add 9g of 1,2-epoxy-4-vinylcyclohexane and 15ml of toluene to a 100ml three-necked flask equipped with a mechanical stirring device and a thermometer as a solvent, add 3g of ethanol as a stabilizer, add 0.17g of chloroplatinic acid-di Vinyltetramethyldisiloxane complex catalyst (also known as Karstedt's catalyst), the mixture was stirred at a reaction temperature of 70 ° C, while using a dropping funnel to drop 15ml of toluene and 20g of MD 42 D. 12 H M mixed solution of polydimethylsiloxane. After 8 hours at 70°C, the hydrosilylation reaction can be completed. Examination of the product using infrared spectroscopy revealed complete disappearance of the silicon hydrogen peak. The mixture was vacuum distilled at 50° C. for 1 hour to remove light fractions to obtain 22.1 g of an epoxy-modified organosiloxane product. The epoxy equivalent weight of the product was determined to be 473.

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Abstract

The invention discloses a method for synthesizing epoxy modified organosiloxane, which is characterized in that in a silicon hydrogen addition reaction of Si-H group-containing polysiloxanes or polysilane and an alkenyl epoxy compound, by taking a Lamoreaux catalyst, a Spaier catalyst or a Karstedt catalyst, lower alcohol is simultaneously added for being as a stabilizing agent, an epoxy compound open loop reaction due to a platinum catalyst can be eliminated, product viscosity is stabilized, and the product quality can be effectively controlled.

Description

technical field [0001] The invention relates to a method for synthesizing epoxy-modified organosiloxane by adding an inhibitor during the hydrosilylation reaction to inhibit ring opening of epoxy groups. Background technique [0002] The hydrosilylation reaction of polyhydrogenmethylsiloxane and unsaturated epoxy compound is a very convenient and simple method for synthesizing functional polymethylsiloxane. The reaction can be expressed as: [0003] [0004] wherein Q represents an epoxy group. The above-mentioned hydrosilylation reactions are usually carried out under the action of platinum catalysts. However, some studies have found that when platinum catalysts are used to produce epoxy-modified polyorganosiloxanes, the epoxy groups will undergo ring-opening reactions, resulting in loss of control of product viscosity, and even gelation in severe cases. In addition, in the presence of a platinum catalyst, the synthesized product still has a tendency to gel slowly due...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/06
Inventor 沈江南余宏伟杨姗姗裘俊红
Owner ZHEJIANG UNIV OF TECH
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