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Preparation method and application of iron-based pyrrolidone ionic liquid catalyst

An iron-based pyrrolidone and ionic liquid technology, applied in the field of catalysis, can solve the problems of unrecyclable catalysts and high catalyst costs, and achieve the effects of good product distribution, high raw material utilization and good selectivity

Active Publication Date: 2018-01-19
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem that the catalyst cost is high and the catalyst cannot be recycled in the current hydrosilylation reaction, and also to improve the selectivity of the β-position product, the invention provides a method for preparing an iron-based pyrrolidone ionic liquid catalyst, and the The catalyst is used to catalyze the hydrosilylation reaction of olefins and alkoxyhydrosilanes. The catalytic method has mild reaction conditions, high conversion rate of raw materials, and good selectivity of addition products.

Method used

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  • Preparation method and application of iron-based pyrrolidone ionic liquid catalyst
  • Preparation method and application of iron-based pyrrolidone ionic liquid catalyst
  • Preparation method and application of iron-based pyrrolidone ionic liquid catalyst

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Effect test

Embodiment 1

[0026] Pyridine diimide iron compound 1 (0.2mmol), pyrrolidone ionic liquid A (3mmol), was added to a 500ml three-necked flask equipped with a magnetic stirring heating device and a condensation device, and under nitrogen protection, the temperature was slowly raised to 60°C. Keeping warm and stirring for 3 hours, cooling down to room temperature, and drying in a vacuum oven to obtain an iron compound / ionic liquid catalyst. Then add 1-hexene (0.6mol) and trimethoxyhydrogensilane (0.8mol) dropwise to the liquid catalyst system through the dropping funnel, keep the reaction temperature at 65°C, turn on the condensing reflux, continue to stir the reaction for 6h, and stop the reaction , standing and cooling to below room temperature, the ionic liquid is solidified, and the product and the ionic liquid are separated. Corresponding fractions were collected by distillation under reduced pressure. The conversion rate of 1-hexene was determined by GC-MS to be 96.9%, and the yield of β...

Embodiment 2

[0028] Add pyridinediimide iron compound 1 (0.2mmol) and pyrrolidone ionic liquid B (4mmol) to a 500ml three-neck flask equipped with a magnetic stirring heating device and a condensation device, and slowly raise the temperature to 120°C under the protection of helium , keep stirring for 3 hours, cool down to room temperature, and dry in a vacuum oven to obtain an iron compound / ionic liquid catalyst. Then add 1-heptene (0.6mol) and trimethoxyhydrogensilane (0.7mol) dropwise to the liquid catalyst system through the dropping funnel, keep the reaction temperature at 90°C, turn on the condensing reflux, continue to stir the reaction for 6h, and stop the reaction , standing and cooling to below room temperature, the ionic liquid is solidified, and the product and the ionic liquid are separated. 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 (hep...

Embodiment 3

[0030] Pyridine diimide iron compound 2 (2mmol), pyrrolidone ionic liquid C (10mmol), was added to a 500 ml three-necked flask equipped with a magnetic stirring heating device and a condensation device, and under the protection of nitrogen, the temperature was slowly raised to 90 ° C, and the temperature was kept Stirring was continued for 3 hours, the temperature was lowered to room temperature, and dried in a vacuum oven to obtain an iron compound / ionic liquid catalyst. Then add 1-undecene (0.3mol) and triethoxyhydrogensilane (0.5mol) dropwise to the liquid catalyst system through the dropping funnel, keep the reaction temperature at 120°C, turn on the condensing reflux, and continue to stir for 6h. Stop the reaction, let it cool down to below room temperature and the ionic liquid solidifies, and separate the product and the ionic liquid. Corresponding fractions were collected by distillation under reduced pressure. The conversion rate of 1-undecene was determined by GC-MS t...

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Abstract

Belonging to the catalysis field, the invention provides a preparation method of an iron-based pyrrolidone ionic liquid catalyst and a method for catalysis of olefin hydrosilylation reaction with thecatalyst in order to solve the problems of high catalyst cost and non-recyclability of catalyst in current hydrosilylation reaction. The catalyst prepared by the method provided by the invention can be used for catalyzing hydrosilylation reaction of olefin and hydrogen-containing alkoxy silane, the reaction conditions are mild, the raw material conversion rate is high, and the catalyst is convenient for recycling.

Description

technical field [0001] The invention belongs to the field of catalysis, and in particular relates to a preparation method and application of an iron-based pyrrolidone ionic liquid catalyst. Background technique [0002] Catalytic hydrosilylation reaction plays an important role in organosilicon synthesis chemistry, and is one of the most important ways to synthesize functional organosilicon monomers, silane coupling agents, functional organosilicon compounds and polymers. Alkoxysilanes are very important intermediates in the silicone industry. The usual method for preparing alkoxysilanes is the addition reaction of unsaturated olefins and hydrosilanes. The most critical technology in the hydrosilylation reaction is the selection and preparation of the catalyst. In the past, chloroplatinic acid was generally used as the catalyst for the hydrosilylation of olefins. Homogeneous catalysts have the characteristics of high activity and short reaction cycle. The most widely used c...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J31/22C07F7/18
CPCY02P20/584
Inventor 李为民连坤波宋广智陈昶乐王福周
Owner CHANGZHOU UNIV