Iron-based cyanogroup-containing anion imidazole ionic liquid catalyst, and preparation method and applications thereof

The technology of imidazole ionic liquid and catalyst is applied in the field of catalysis, which can solve the problems of unrecyclable catalyst, unstable storage and high catalyst cost, and achieve the effects of low cost of preparing raw materials, good product distribution and high utilization rate of raw materials

Active Publication Date: 2018-02-09
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems of high catalyst cost, unstable storage and unrecyclable catalyst in the current olefin hydrosilylation reaction, the invention provides an iron-based cyano-containing anion imidazolium ionic liquid catalyst and a preparation method thereof, and uses the catalyst It is used to catalyze the hydrosilylation reaction of olefins. Using this catalyst for addition reaction has mild conditions, high conversion rate of raw materials, and good selectivity of addition products.

Method used

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  • Iron-based cyanogroup-containing anion imidazole ionic liquid catalyst, and preparation method and applications thereof
  • Iron-based cyanogroup-containing anion imidazole ionic liquid catalyst, and preparation method and applications thereof
  • Iron-based cyanogroup-containing anion imidazole ionic liquid catalyst, and preparation method and applications thereof

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Experimental program
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Effect test

Embodiment 1

[0035] Iron-based cyano-containing anion imidazole ionic liquid catalyst A (0.2mmol), join in the there-necked flask with magnetic stirring heating device and condensation device, under the protection of nitrogen, drop 1-hexene (0.6mol) successively through dropping funnel ), slowly warming up to a reaction temperature of 65°C. Then add trimethoxyhydrogensilane (0.8mol) dropwise to the liquid catalyst system, turn on condensing reflux, keep the reaction temperature at 65°C, continue to stir the reaction for 6h, stop the reaction, let the ionic liquid stand to cool below room temperature to solidify, separate the product and ionic liquid. Corresponding fractions were collected by distillation under reduced pressure. The conversion rate of 1-hexene was determined by GC-MS to be 98.9%, and the yield of β-addition product (hexyltrimethoxysilane) was 97.5%.

Embodiment 2

[0037] Iron-based cyano-containing anion imidazole ionic liquid B (0.2mmol), was added to a three-necked flask with a magnetic stirring heating device and a condensation device, and under nitrogen protection, 1-heptene (0.6mol) was sequentially added dropwise through a dropping funnel , slowly warming up to 85°C. Then add trimethoxyhydrogensilane (0.7mol) dropwise to the liquid catalyst system, keep the reaction temperature at 85°C, turn on the condensing reflux, continue to stir the reaction for 6h, stop the reaction, let it cool down to below room temperature and the ionic liquid solidifies, separate the product and ionic liquid. Corresponding fractions were collected by distillation under reduced pressure. The conversion rate of 1-heptene was determined by GC-MS to be 96.9%, and the yield of β-addition product (heptyltrimethoxysilane) was 94.5%.

Embodiment 3

[0039]Iron-based cyano-containing anion imidazole ionic liquid C (0.1mmol), was added to a three-necked flask with a magnetic stirring heating device and a condensation device, and under nitrogen protection, 1-undecene (0.3mol ), slowly warming up to a reaction temperature of 85°C. Then add trimethoxyhydrogensilane (0.5mol) dropwise to the liquid catalyst system, keep the reaction temperature at 85°C, turn on the condensing reflux, continue to stir the reaction for 6h, stop the reaction, let the ionic liquid stand to cool below room temperature to solidify, separate the product and ionic liquid. Corresponding fractions were collected by distillation under reduced pressure, and the conversion rate of 1-undecene was determined to be 88.9% by GC-MS, and the yield of β-addition product (undecyltrimethoxysilane) was 85.5%.

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Abstract

The invention belongs to the field of catalyst, and provides a preparation method of an iron-based cyanogroup-containing anion imidazole ionic liquid catalyst, and an application method of the iron-based cyanogroup-containing anion imidazole ionic liquid catalyst in catalyzing hydrosilylation of olefins with hydrogen-containing alkoxy silane. Problems in the prior art that in hydrosilylation, catalyst cost is high, a catalyst is unstable to store, and recovery of the catalyst is impossible to realize. The reaction conditions of the iron-based cyanogroup-containing anion imidazole ionic liquidcatalyst are mild; raw material conversion rate is high; catalytic activity is high; automatic phase separation of the products and the iron-based cyanogroup-containing anion imidazole ionic liquid catalyst can be realized after reaction; and catalyst recovery is realized.

Description

technical field [0001] The invention belongs to the field of catalysis, and in particular relates to a preparation method of an iron-based cyano group-containing anion imidazolium ionic liquid catalyst and a method for catalyzing the hydrosilylation reaction of olefins and alkoxysilanes. Background technique [0002] Catalytic olefin hydrosilylation plays an important role in synthetic organic chemistry, and is one of the most important ways to synthesize organosilicon coupling agents, functional organosilicon compounds and organosilicon polymers. Alkene hydrosilylation usually directly uses chloroplatinic acid as a catalyst. Speier catalyst (isopropanol solution of chloroplatinic acid) and Karstedt catalyst ([(ViMe 2 Si) 2 0] PtCl 2 ) has a certain catalytic activity and has been widely used in the production of organosilicon. Although the platinum catalyst system has high activity, the reaction often needs to be carried out under high temperature and high pressure cond...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07F7/18
CPCB01J31/0284B01J2231/32C07F7/1804C07F7/1876
Inventor 李为民连坤波宋广智王福周陈昶乐
Owner CHANGZHOU UNIV
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