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Supported hydrosilylation catalyst and preparation method thereof

A technology for hydrosilylation reaction and catalyst, which is applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc. Low selectivity, catalyst deactivation and other problems, to achieve the effect of easy control, high catalytic activity and high selectivity

Inactive Publication Date: 2011-09-21
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these heterogeneous catalysts are used in hydrosilylation reactions, which are often carried out under high temperature and high pressure conditions. During the reaction process, platinum is easy to lose, and the catalyst is quickly deactivated.
In addition, the product selectivity obtained is not high, so the catalytic effect of these heterogeneous catalysts is not ideal

Method used

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  • Supported hydrosilylation catalyst and preparation method thereof
  • Supported hydrosilylation catalyst and preparation method thereof
  • Supported hydrosilylation catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1) Modify the surface of the carrier with a coupling agent: In a 500 mL reactor with a feeding port and a stirring device, add 20.0 g of silica gel and 250 mL of toluene, stir at room temperature for 10 min, add 10.0 g of γ-aminopropyltriethyl Oxysilane, stirred for 20 min, added dropwise a mixed solution of 10 mL of water and 30 mL of ethanol at room temperature, stirred for 2 h, heated to reflux at 100 °C and stirred for 2 h. Toluene and ethanol were removed to obtain a white powder, which was dried under vacuum at 80 °C for 24 h to obtain primary modified silica.

[0022] 2) Modify the surface of the carrier with a functional group compound: In a 250 mL three-necked flask, add 2.0 g of the functional group compound undecylenic acid and 100 mL of water, heat up to 80 °C, stir to completely dissolve the undecylenic acid, add 6.0 g of the undecylenic acid in step 1 ) primary modified silica, keep the temperature and continue to stir for 3 h, filter and wash to obtain a ...

Embodiment 2

[0025] 1) Modify the surface of the support with a coupling agent: In a 500 mL reactor with a feeding port and a stirring device, add 20.0 g of silica gel and 250 mL of toluene, stir at room temperature for 10 min, add 6.0 g of γ-aminopropyl tris Ethoxysilane, stirred for 20 min, added dropwise a mixed solution of 10 mL of water and 30 mL of ethanol at room temperature, stirred for 2 h, heated to reflux at 100 °C and stirred for 2 h. Toluene and ethanol were removed to obtain a white powder, which was dried under vacuum at 80 °C for 24 h to obtain a modified carrier.

[0026] 2) Modify the surface of the carrier with functional groups: In a 250mL three-necked flask, add 2.0 g of undecylenic acid and 100 mL of water, heat up to 80°C, stir to completely dissolve the undecylenic acid, and add 6.0 g of the product obtained in step 1) , keep the temperature and continue to stir for 3 h, filter and wash to obtain a light yellow powder, which is dried at 80 °C for 24 h under vacuum t...

Embodiment 3

[0029] 1) Modify the surface of the carrier with a coupling agent: In a 500 mL reactor with a feeding port and a stirring device, add 20.0 g of silica gel and 250 mL of toluene, stir at room temperature for 10 min, add 5.0 g of γ-aminopropyl trimethyl Oxysilane, stirred for 20 min, added dropwise a mixed solution of 10 mL of water and 30 mL of ethanol at room temperature, stirred for 2 h, heated to reflux at 100 °C and stirred for 2 h. Toluene and ethanol were removed to obtain a white powder, which was dried under vacuum at 80 °C for 24 h to obtain a modified carrier.

[0030] 2) Modify the surface of the carrier with functional groups: In a 250mL three-necked flask, add 2.0 g of undecylenic acid and 100 mL of water, heat up to 80°C, stir to completely dissolve the undecylenic acid, and add 6.0 g of the product obtained in step 1) , keep the temperature and continue to stir for 3 h, filter and wash to obtain a light yellow powder, which is dried at 80 °C for 24 h under vacuum...

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Abstract

The invention relates to a supported hydrosilylation catalyst and a preparation method thereof, and aims to provide a heterogeneous catalyst suitable for hydrosilylation and a preparation method thereof. When the catalyst is used, the reaction conditions are mild; and the catalyst is safe and effective and conveniently separated from the product, and can be recycled. The catalyst provided by the invention has the structural formula shown in the specification. The preparation method provided by the invention comprises the following steps: 1) modifying the carrier surface with a coupling agent;2) modifying the carrier surface with a functional group compound; and 3) preparing the catalyst through coordination complexing with a platinum compound.

Description

technical field [0001] The invention relates to a catalyst in the field of organic chemistry and a preparation method thereof, in particular to a supported hydrosilylation reaction catalyst and a preparation method thereof. Background technique [0002] Catalytic olefin hydrosilylation plays an important role in organic synthetic chemistry, and is one of the most important ways to synthesize organosilicon coupling agents and functional organosilicon compounds and polymers. Usually directly use chloroplatinic acid as catalyzer, experiment and industrial production use most are Speier's catalyst (chloroplatinic acid isopropanol solution) and Karstedt's catalyst (chloroplatinic acid and containing vinyl silane or siloxane complex). Although these two catalysts have high activity, the product selectivity is not high; and as a homogeneous catalyst, it is difficult to separate the catalyst from the reaction system after the reaction, which is undoubtedly a waste for the use of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07F7/18C07F7/14C07F7/08
CPCY02P20/50Y02P20/584
Inventor 来国桥白赢彭家建厉嘉云蒋剑雄
Owner HANGZHOU NORMAL UNIVERSITY
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