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Silicon-hydrogen additive reaction method

A technology of hydrosilylation reaction and hydrosilane, which is applied in the direction of chemical instruments and methods, silicon organic compounds, organic compounds/hydrides/coordination complex catalysts, etc., which can solve the problems of difficult separation, recovery and reuse, and catalytic reactivity It is not high, it is difficult to apply to problems such as industrialization, to achieve high thermal and chemical stability, simple operation of reaction and product separation, and the effect of improving activity and selectivity

Inactive Publication Date: 2007-09-12
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

But for certain types of hydrosilylation reactions, such as the hydrosilylation of olefins and alkoxysilanes, transition metals (Pt, Rh, Ru, etc.) are used as catalysts, and the catalytic activity is not high (Bogdan Marciniec, and Jacek Gulinski, J. Organomet. Chem., 1983, 253, 349-362)
At the same time, the catalytic system is also difficult to separate, recover and reuse from the reaction system.
Since then, Chen Yuanyin et al. (Meng Lingzhi, Ke Aiqing, Chen Yuanyin, Applied Chemistry, 1997, 14, 1, 107-109; Liu Ying, Chen Yuanyin, Sheng Rongsheng, Molecular Catalysis, 1997, 11, 5, 394-400; Dai Yanfeng, Xiao Bin, Li Fengyi, Ru Xiang, Chemical Reagents, 2005, 27, 12, 707-709) studied the application of Pt on polymer compounds for hydrosilylation reaction, but the preparation of the catalyst is complicated and the reaction activity is not high , it is difficult to apply to industrialization

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0023] In a 250 ml three-necked flask, triphenylphosphine rhodium chloride (1.25 mmol) and 1-butyl-3-methylimidazolium hexafluorophosphate (BMImPF 6 ) (25mL), under the protection of nitrogen, the temperature was slowly raised to 70°C, the reaction was stirred for 0.5 hours, the condensing reflux was opened, and hexene (1.25mol) and triethoxyhydrogensilane (1.25mol) were successively added dropwise through the dropping funnel, keeping Reaction temperature, continue to stir and react for 5 hours, let stand, cool to room temperature, decant to separate the upper layer product, measure the conversion rate of hexene by GC-MS 100%, β adduct 1-triethoxysilyl Hexane (CH 3 (CH 2 ) 5 Si(OCH 2 CH 3 ) 3 ) The yield is 97.3%.

Embodiment 2

[0025] In Example 1, triphenylphosphine rhodium chloride (6.25mmol) was added, and the conversion rate of hexene measured by GC-MS after the reaction was 100%, and the yield of β-adduct 1-triethoxysilyl hexane The rate is 99.6%.

Embodiment 3

[0027] In Example 1, triphenylphosphine rhodium chloride (3.12mmol) was added, and the conversion rate of hexene measured by GC-MS after the reaction was 100%, and the yield of β-adduct 1-triethoxysilyl hexane The rate is 98.0%.

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Abstract

This invention relates to a method of using hydrosilylation reaction to synthesize silicon compound. It needs to solve the technical problem that provides a hydrosilylation reaction method taking ionic liquids of room temperature as the reaction medium and transition metal complexes Rh (PPh3) 3Cl as the main catalyst. The greatest strength is that it can improve the catalytic activity of Rh (PPh3) 3Cl and increase selectivity of beta adduct in the ionic liquid at room temperature. At the same time, when the reaction ends, cooling and settling make the catalyst / ionic liquid and products separate, and the catalyst / ionic liquid can be recycled.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a method for carrying out hydrosilylation reaction using a rhodium complex / room temperature ionic liquid as a catalyst and a reaction medium. Background technique [0002] Olefin-catalyzed hydrosilylation reaction occupies an important position in synthetic organic chemistry, and is one of the most important ways to synthesize organosilicon coupling agents and functional organosilicon compounds and polymers (Leslie D. Field, Antony J. Ward, J Organomet. Chem, 2003, 681, 91-97). Before the present invention, usually use chloroplatinic acid / organic solvent as the catalyzer of this type of reaction, although this catalytic system has higher activity, it is difficult to separate and recover from the reaction system, and the reaction cost is higher (Chisso Corp.JP ., 8204995, 1982). Later, through the study of various transition metal complexes, it was found that transition metals (...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08B01J31/24B01J31/30
Inventor 彭家建厉嘉云来国桥邱化玉倪勇吴连斌
Owner HANGZHOU NORMAL UNIVERSITY
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