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Method for preparing catalyst for addition reaction of hydrogen and silicon

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 the problem of low reaction activity and low catalytic activity High, difficult to separate, recycle and reuse problems, to achieve the effect of mild addition reaction conditions, simple separation operation, and high selectivity

Inactive Publication Date: 2009-09-09
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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 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
Comparison scheme
Effect test

Embodiment 1

[0025] Catalyst preparation: Add 0.1mol 1-bromo-2-chloroethane and 50mL tetrahydrofuran into a three-necked flask, stir and control the temperature at 60°C, gradually add 0.1mol N-methylimidazole dropwise, react overnight, white precipitates appear, filter, and use Tetrahydrofuran was washed several times to obtain the white intermediate 1-(2-chloroethyl)-3-methylimidazolium bromide.

[0026] Add 100mL of tetrahydrofuran and 0.05mol of triphenylphosphine into a three-neck flask, stir and dissolve, cut into 0.8g of lithium flakes, react at 20°C for 4 hours, remove unreacted lithium, add 5mL of tert-chlorobutane, and react for 30min. filter. Add 0.05 mol of the white crystalline product obtained in the first step to the reaction solution, the orange color of the solution fades, vacuum filter after 1 hour, and vacuum dry to obtain 1-(diphenylphosphinoethyl)-3-methylimidazolium hexafluorophosphate .

[0027] In a 25 ml round bottom flask, add 0.03 mol of 1-(diphenylphosphinoethy...

Embodiment 2

[0029] Catalyst preparation: In Example 1, replace N-methylimidazole with 0.1mol N-butylimidazole, and synthesize three [1-(diphenylphosphinoethyl)-3-butylimidazole hexafluorophosphate] chloride in the same steps rhodium.

[0030] The reaction process of the hydrosilylation reaction: in embodiment 1, add three [1-(diphenylphosphine ethyl)-3-butyl hexafluorophosphate] rhodium chloride instead of three [1-(diphenylphosphine Ethyl)-3-methyl imidazole Hexafluorophosphate] rhodium chloride, the conversion rate of styrene measured by GC-MS at the end of the reaction is 97.5%, and the β adduct 1-triethoxysilyl-2-phenylethane (PhCH 2 CH 2 Si(OCH 2 CH 3 ) 3 ) yield was 91.1%, and the α-adduct 1-triethoxysilyl-1-phenylethane (PhCH(CH 3 )Si(OCH 2 CH 3 ) 3 ) The yield is 6.8%.

Embodiment 3

[0032] Catalyst preparation: replace N-methylimidazole with 0.1mol N-hexylimidazole in embodiment 1, three [1-(diphenylphosphine ethyl)-3-hexylimidazole hexafluorophosphate] rhodium chloride are synthesized in the same steps .

[0033] The reaction process of the hydrosilylation reaction: add three [1-(diphenylphosphine ethyl)-3-hexyl imidazolium hexafluorophosphate] rhodium chloride instead of three [1-(diphenylphosphine Ethyl)-3-methyl imidazole Hexafluorophosphate] rhodium chloride, the conversion rate of styrene measured by GC-MS at the end of the reaction is 98.8%, and the β adduct 1-triethoxysilyl-2-phenylethane (PhCH 2 CH 2 Si(OCH 2 CH 3 ) 3 ) yield was 92.2%, and the α-adduct 1-triethoxysilyl-1-phenylethane (PhCH(CH 3 )Si(OCH 2 CH 3 ) 3 ) The yield is 5.7%.

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Abstract

The invention relates to a method for preparing rhodiumm chloride (1-(diphenylphosphine alkyl)-3-alkyl imidazole hexafluorophosphate), and aims to solve the technical problems that a series of catalyst for addition reaction of hydrogen and silicon is provided; the reaction is easy to carry out; the selectivity of a beta addition product in a product can be improved; and the catalyst can be recovered and reutilized. The method for preparing the catalyst is characterized in that 1-(diphenylphosphine alkyl)-3-alkyl imidazole hexafluorophosphate and rhodium chloride with the mol ratio of 3:1 are taken as a raw material, reflowed in ethanol, and are cooled to the room temperature; solid materials are filtered out; ethanol washing is carried out; and the rhodium chloride (1-(diphenylphosphine alkyl)-3-alkyl imidazole hexafluorophosphate) complex is obtained after vacuum drying.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a method for preparing a hydrosilylation reaction catalyst tris[1-(diphenylphosphinoalkyl)-3-alkylimidazolium hexafluorophosphate]rhodium chloride. 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 me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07F7/18C07F7/14
Inventor 来国桥彭家建厉嘉云白赢胡应乾蒋剑雄邱化玉
Owner HANGZHOU NORMAL UNIVERSITY
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