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Silica-supported bis-acid functionalized ionic liquid and its preparation method and application

A technology of ionic liquid and silica, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problems of less research on biomass hydrolysis, etc. Achieve the effect of overcoming difficulty in separation, low price and stable structure

Active Publication Date: 2019-03-29
LANZHOU INST OF CHEM PHYSICS 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 immobilization of ionic liquids has been successfully applied to a variety of catalytic reactions and separations, but less research has been done on biomass hydrolysis.

Method used

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  • Silica-supported bis-acid functionalized ionic liquid and its preparation method and application
  • Silica-supported bis-acid functionalized ionic liquid and its preparation method and application
  • Silica-supported bis-acid functionalized ionic liquid and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1 Preparation and characterization of catalyst

[0028] The preparation process is outlined as follows: under magnetic stirring at 110°C, add 2.78 g of imidazole to the flask, and after it melts into a liquid, add 9.5 mL of 3-chloropropyltriethoxysilane, N 2 Protect and continue to stir for 24h to obtain a clear viscous solution. After repeated washing with ether, spin evaporate to obtain N-(3-propyltriethoxysilane) imidazolium chloride salt; ethanol dissolves the above-mentioned ionic liquid (the molar ratio is 100:1 ), add 100-200 mesh silica (the molar ratio of silica to ionic liquid is 4:1), reflux with magnetic stirring at 85°C for 24h, wash with 10mL ethanol for 5 times, and dry at 100°C to obtain immobilized ion Liquid (SiO 2 / IL-1). The catalyst is characterized by TEM, FT-IR, TG, BET and elemental analysis, and it can be concluded that the ionic liquid is successfully bonded to silicon dioxide.

Embodiment 2

[0029] Example 2 Preparation and Characterization of Catalyst

[0030] The preparation process is outlined as follows: under magnetic stirring at 110°C, add 2.78 g of imidazole to the flask, and after it melts into a liquid, add 9.5 mL of 3-chloropropyltriethoxysilane, N 2 Protect and continue to stir for 24h to obtain a clear viscous solution. After repeated washing with ether, spin evaporate to obtain N-(3-propyltriethoxysilane) imidazole chloride salt; equimolar amounts of 1,4-butanesulfonate Acid lactone at 15°C, N 2 Slowly add dropwise to the ethanol solution of N-(3-propyltriethoxysilane)imidazolium chloride salt (the mass ratio of ionic liquid to ethanol is 1:3) under the atmosphere, N 2 Reaction at 45°C for 24 hours under the atmosphere, rotary evaporation, repeated washing with ether, and rotary evaporation to obtain a light yellow and clear ionic liquid 3-(4-sulfobutyl)-1-(3-propyltriethoxysilane)imidazole Chloride salt; Dissolve the above ionic liquid in ethanol (...

Embodiment 3

[0031] Preparation and characterization of embodiment 3 catalyst

[0032] The preparation process is outlined as follows: under magnetic stirring at 110°C, add 2.78 g of imidazole to the flask, and after it melts into a liquid, add 9.5 mL of 3-chloropropyltriethoxysilane, N 2 Protect and continue to stir for 24h to obtain a clear viscous solution. After repeated washing with ether, spin evaporate to obtain N-(3-propyltriethoxysilane) imidazolium chloride salt; ethanol dissolves the above-mentioned ionic liquid (the molar ratio is 100:1 ), add 100-200 mesh silica (the molar ratio of silica to ionic liquid is 4:1), reflux with magnetic stirring at 85°C for 24h, wash with 10mL ethanol for 5 times, and dry at 100°C to obtain immobilized ion Liquid: Weigh 1.4g of the above product and disperse it in 7mL of ethanol, add excess concentrated sulfuric acid (350mL) dropwise, stir and reflux with magnetic force at 80°C for 24h, wash with ethanol repeatedly until the filtrate is neutral, ...

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Abstract

The invention discloses a silica immobilized double-acid functionalized ionic liquid. The structural formula of the immobilized ionic liquid is shown as the specification. As a catalyst, the immobilized ionic liquid not only inherits the advantages of high activity and high selectivity of homogeneous ionic liquid, can efficiently converts carbohydrates to prepare high value-added chemicals, but also overcomes the disadvantages of difficult separation, large consumption and the like of homogeneous ionic liquid, realizes regeneration and recycling of catalyst, and lays a good foundation for industrial application. The invention also discloses a preparation method of the silica immobilized ionic liquid and application of the silica immobilized ionic liquid as a catalyst in carbohydrate hydrolysis for preparation of furfural compounds (furfural and 5-hydroxymethylfurfural).

Description

technical field [0001] The invention relates to a silicon dioxide immobilized bis-acid functionalized ionic liquid and a preparation method and application thereof. Background technique [0002] Biomass energy, as a kind of renewable energy, has a wide range of sources, low price, and abundant reserves. It has become an ideal alternative resource and has attracted widespread attention (Lin, Y. C.; Huber, G. W., Energy & EnvironmentalScience ,2009, 2, 68.). The current research focus of biomass energy is the synthesis of biomass platform compounds from carbohydrates, among which furfural compounds (5-hydroxymethylfurfural, furfural, etc.) are widely used in medicine, plastics, rubber and other fields (Dutta, S. ; De, S.; Saha, B., Chempluschem , 2012, 77, 259.), has been recognized as the most promising and representative new platform compound in recent years. The preparation of furfural compounds from carbohydrates is regarded as "a key link of great significance connect...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18B01J31/02C07D307/48C07D307/46
CPCY02P20/584
Inventor 丑凌军许海梅宋焕玲杨建赵军赵华华梁宁
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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