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Imidazole grafting-type ionic liquid catalyst and preparation method and application

A technology of ionic liquid and catalyst, which is applied in the field of imidazole-based grafted ionic liquid catalyst and its preparation, can solve the problems of low catalytic activity and selectivity, harsh reaction conditions, etc., achieve good catalytic effect, mild reaction conditions, and easy repeated use Effect

Inactive Publication Date: 2010-09-29
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the heterogeneous catalysts used in cycloaddition reactions mainly include metal oxides, supported metal complexes, and polymers; however, their catalytic activity and selectivity are low, and the reaction conditions are relatively harsh.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 1mol of methylimidazole and 1mol of chloropropyltriethoxysilane to 80mL of toluene solvent, stir and reflux until the layers are separated, and take the lower layer of viscous liquid (1-chloropropyl (triethoxysilyl)-3 - methylimidazole chloride crude product), washed 3 times with ethyl acetate and dried in vacuo. Add the obtained [Smim]Cl and 1 mol potassium hydroxide into 80 mL of anhydrous dichloromethane, stir vigorously at room temperature for 10 h, filter off the precipitate, remove the solvent by rotary evaporation, wash 3 times with ether, and dry in vacuum at 70 °C for 10 h . Add 2.3g of the obtained ionic liquid to a 0.3mol silica gel carrier uniformly dispersed in 50mL of anhydrous toluene, stir and reflux for 12h, extract with dichloromethane for 10h, and vacuum dry at 70°C for 10h to obtain the heterogeneously grafted ionic liquid Liquid Catalyst [Smim]OH / SiO 2 , the mass grafting amount of ionic liquid is 5%. Propylene oxide and imidazole-based graft...

Embodiment 2

[0019] Add 1mol of methylimidazole and 1mol of chloropropyltriethoxysilane into 100mL of toluene solvent, stir and reflux until the layers are separated, and the lower layer of viscous liquid (1-chloropropyl (triethoxysilyl)-3 - methylimidazole chloride crude product), washed 3 times with ethyl acetate and dried in vacuo. Add the obtained [Smim]Cl and 1 mol potassium hydroxide into 100 mL of anhydrous dichloromethane, stir vigorously at room temperature for 16 h, filter off the precipitate, remove the solvent by rotary evaporation, wash 3 times with ether, and dry under vacuum at 90°C for 16 h . Add 4.6g of the obtained ionic liquid to a 0.3mol silica gel carrier uniformly dispersed in 70mL of anhydrous toluene, stir and reflux for 18h, extract with dichloromethane for 16h, and vacuum dry at 90°C for 16h to obtain a heterogeneously grafted ion Liquid Catalyst [Smim]OH / SiO 2 , the mass grafting amount of ionic liquid is 10.5%. Propylene oxide and imidazole-based grafted ioni...

Embodiment 3

[0021] Add 1mol of methylimidazole and 1mol of chloropropyltriethoxysilane to 120mL of toluene solvent, stir and reflux until the layers are separated, and the lower layer of viscous liquid (1-chloropropyl (triethoxysilyl)-3 - methylimidazole chloride crude product), washed 3 times with ethyl acetate and dried in vacuo. Add the obtained substance [Smim]Cl and 1mol potassium hydroxide into 120mL of anhydrous dichloromethane, stir vigorously at room temperature for 20h, filter off the precipitate, remove the solvent by rotary evaporation, wash 3 times with ether, and dry under vacuum at 110°C 20h. Add 9.1 g of the obtained ionic liquid to a 0.3 mol silica gel carrier uniformly dispersed in 90 mL of anhydrous toluene, stir and reflux for 20 h, extract with dichloromethane for 18 h, and vacuum dry at 110 °C for 20 h to obtain a heterogeneously grafted ion Liquid Catalyst [Smim]OH / SiO 2 , the quality grafting amount of ionic liquid is 17%. Propylene oxide and imidazole-based gra...

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PUM

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Abstract

The invention relates to an imidazole grafting-type ionic liquid catalyst, which is hydroxide of 1-propyl (triethoxysilyl)-3-methylimidazole grafted on a carrier. The representation formula of the imidazole grafting-type ionic liquid catalyst is [Smim]OH / X and a mass grafting amount of ionic liquid is between 5 and 25 percent, wherein Smim represents 1-propyl (triethoxysilyl)-3-methylimidazole; and X represents the meso-porous carrier. The imidazole grafting-type ionic liquid catalyst has the advantages of good catalytic effect, high conversion rate of propylene oxide, 100 percent of selectivity of propene carbonate, mild reaction condition and capability of being recycled better.

Description

technical field [0001] The invention relates to an imidazole grafted ionic liquid catalyst, a preparation method and application. Background technique [0002] Propylene carbonate (PC) is a widely used chemical, which can be used as a high-efficiency solvent, an excellent extractant, an excellent medium for high-energy lithium batteries and capacitors, and can also be used as an auxiliary and fixing agent for synthetic fibers; PC is also a It is an extremely versatile raw material and intermediate for organic synthesis. The synthesis methods of PC mainly include phosgene method, transesterification method, chloropropanol method and propylene oxide (PO) and CO 2 Cycloaddition. Among them, the cycloaddition method is an environmentally friendly synthesis method. For PO and CO 2 Catalysts for cycloaddition reactions can be divided into two categories: homogeneous catalysts and heterogeneous catalysts. Homogeneous catalysts (such as quaternary ammonium salts, metal complexe...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07D317/36
Inventor 孙予罕魏伟张学兰王登峰赵宁阿卜杜拉赫·阿尔·阿里费塔伊比·奥克赛义德·阿卜杜拉赫·奥斯曼
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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