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Producing method of catalyzer of addition reaction of silicon and hydrogen

A hydrosilylation reaction and catalyst technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve problems such as difficult separation and troublesome operation, and achieve Easy storage, easy addition, and mild reaction conditions

Inactive Publication Date: 2009-02-25
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, the catalyst and the reaction medium are separated, which brings disadvantages such as troublesome operation and difficult separation during the reaction process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1-tert-butyl-3-methylimidazolium hexafluorophosphate (sBMImPF 6 ) (50g) and three (triphenylphosphine) rhodium chloride (1.25mmol) were added in the there-necked flask with magnetic stirring heating device and condensing device, under the protection of nitrogen, the temperature was slowly raised to the melting of the carrier, and the insulation continued to stir for 3 hour, cooling down to room temperature, and drying in a vacuum oven to obtain a supported rhodium catalyst.

[0019] The reaction process of the hydrosilylation reaction: In a 250 ml three-necked flask, add the catalyst prepared above, under the protection of nitrogen, slowly raise the temperature to 90°C, stir for 0.5 hours, turn on the condensing reflux, and add benzene dropwise through the dropping funnel Ethylene (1.25mol) and triethoxyhydrogensilane (1.25mol), keep the reaction temperature, continue to stir the reaction for 2 hours, let it stand, cool to room temperature, separate the upper layer prod...

Embodiment 2

[0021] 1-Benzyl-3-methylimidazolium hexafluorophosphate (PhCH 2 MPF 6 ) (50g) and three (triphenylphosphine) rhodium chloride (1.25mmol) were added in the there-necked flask with magnetic stirring heating device and condensing device, under the protection of nitrogen, the temperature was slowly raised to the melting of the carrier, and the insulation continued to stir for 3 hour, cooling down to room temperature, and drying in a vacuum oven to obtain a supported rhodium catalyst. Applied to the addition reaction of styrene and triethoxyhydrogensilane, the conversion rate of styrene determined by GC-MS at the end of the reaction is 93.2%, and the β-adduct 1-triethoxysilyl-2-phenylethane (PhCH 2 CH 2 Si(OCH 2 CH 3 ) 3 ) yield was 86.8%, and the α-adduct 1-triethoxysilyl-1-phenylethane (PhCH(CH 3 )Si(OCH 2 CH 3 ) 3 ) The yield is 1.6%.

Embodiment 3

[0023] N-ethylpyridine hexafluorophosphate (EPyPF 6 ) (50g) and three (triphenylphosphine) rhodium chloride (1.25mmol) were added in the there-necked flask with magnetic stirring heating device and condensing device, under the protection of nitrogen, the temperature was slowly raised to the melting of the carrier, and the insulation continued to stir for 3 hour, cooling down to room temperature, and drying in a vacuum oven to obtain a supported rhodium catalyst. Applied to the addition reaction of styrene and triethoxyhydrogensilane, the conversion rate of styrene determined by GC-MS at the end of the reaction is 100%, and the β-adduct 1-triethoxysilyl-2-phenylethane (PhCH 2 CH 2Si(OCH 2 CH 3 ) 3 ) yield was 90.6%, and the α-adduct 1-triethoxysilyl-1-phenylethane (PhCH(CH 3 )Si(OCH 2 CH 3 ) 3 ) The yield is 5.3%.

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Abstract

The present invention relates to process of preparing catalyst for the addition reaction of silicon and hydrogen, and solves the technological problem of preparing catalyst with easy maintenance, easy separation and easy reuse. The catalyst has dialkyl imidazolyl hexafluorphsphate or alkyl pyridyl hexafluorphsphate as carrier and tri(triphenyl phosphine) rhodium chloride as main catalyst in the weight ratio of 1 to 0.0005-0.01, and is prepared through mixing via stirring under nitrogen protection, heating slowly for smelting the carrier, maintaining while stirring, cooling and drying to obtain the catalyst.

Description

technical field [0001] The invention relates to the field of organic catalytic chemistry, in particular to a method for preparing a catalyst for a hydrosilylation reaction. Background technique [0002] The hydrosilylation reaction is the most studied and widely used reaction in organosilicon chemistry, through which a series of functional organosilicon compounds containing Si-C bonds can be prepared (Leslie D. Field, Antony J. Ward, J Organomet. Chem, 2003, 681, 91-97). Its product forms include organosilicon monomer, silane coupling agent, silicone rubber, special silicone oil, silicone resin and many silicon-containing polymer compounds, and the reaction conditions are mild, the yield is high, and the application is wide. It is widely used in the field of organosilicon chemistry and chemical industry occupied an important position. In 1957, Speier (Speier J.L., Webster J.A., Barnes G.H., J Am.Chem.Soc., 1957, 79, 4, 974-979) discovered the homogeneous hydrosilylation re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/24B01J31/30C07F7/18
Inventor 彭家建伍川厉嘉云蒋剑雄倪勇白赢
Owner HANGZHOU NORMAL UNIVERSITY