Immobilized ionic liquid catalyst used for preparing 5-hydroxymethylfurfural and preparation of immobilized ionic liquid catalyst

A technology of hydroxymethyl furfural and ionic liquid is applied in the application field of catalytic conversion of biomass to prepare 5-hydroxymethyl furfural, which can solve the problems of difficult recovery, low substrate conversion rate, corrosion of equipment and the like, and achieves improved catalytic efficiency, The effect of improving dispersion effect and high recovery rate

Inactive Publication Date: 2017-03-08
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of this series of catalysts is more or less difficult to recover, corroded equipment, environmental pollution, low substrate conversion rate, poor thermal stability, low catalytic activity and complex catalyst preparation process, etc.
[0004] There are serious problems in the ca

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0059] Example 1

[0060] (1) Add 0.10mol of N-methylimidazole to 30mL of ethanol, add 5g of ZSM-5 molecular sieve under vigorous stirring (the stirring speed is 300rpm), and stir for 10h at room temperature so that the N-methylimidazole can be fully contained in the molecular sieve. After dispersion, add 0.2mol of 1,3-propane sultone in ethanol solution, stir and react for 12h at 50℃, filter with suction, and wash with ethanol 3 times to remove unreacted N-methylimidazole, The 1,3-propane sultone and the reaction product of the two attached to the surface of the molecular sieve are thoroughly washed and removed, thereby obtaining a white solid crude product, which is ZMS loaded with 1-propanesulfonate-3-methylimidazole -5 molecular sieve;

[0061] (2) The crude white solid obtained in step (1) is stirred and dispersed in 30 mL of dichloromethane, and then an appropriate amount of sulfuric acid (the amount of sulfuric acid is 0.11 mol) is added dropwise, and the reaction is reflux...

Example Embodiment

[0063] Example 2

[0064] (1) Add 0.10 mol of imidazole to 30 ml of absolute ethanol, and add 0.11 mol of 3-chloropropyltriethoxysilane, and stir at 100°C (stirring time is 24h) to obtain precursor I; 0.1mol 1,3-propane sultone was added to the solution obtained by the above reaction, and stirred at 40°C for 24h to obtain precursor II; 3g of SBA-15 was dispersed in 50ml of toluene, and 1.5g of the precursor obtained above was added Body II, stirred at 100°C for 24 hours, filtered with suction, and the obtained white powder solid was washed with ethanol 3 times to obtain SBA-15 molecular sieve loaded with 1-siloxane-3-propanesulfonyl imidazole chloride ionic liquid;

[0065] (2) The SBA-15 molecular sieve loaded with 1-siloxane-3-propanesulfonic acid imidazolium chloride ionic liquid was ultrasonically dispersed in 50ml of ethanol, and then an appropriate amount of concentrated sulfuric acid (concentrated) was gradually added dropwise under ice bath conditions. The mass concentrati...

Example Embodiment

[0068] Example 3

[0069] (1) Add 0.10mol of imidazole to 30ml of absolute ethanol, and add 0.11mol of 3-chloropropyltriethoxysilane, and stir at 100°C (stirring time is 24h) to obtain precursor I; Add 0.1 mol of chloropropionic acid to the solution obtained by the above reaction, and stir at 60°C for 24 hours to obtain an ionic liquid;

[0070] (2) Disperse 3g of MCM-22 in 50ml of toluene, add the above ionic liquid, stir at 100°C for 24h, and filter with suction. The white powder solid obtained is washed with ethanol 3 times and dried (the drying temperature is 80 ℃, the time is 12h), the MCM-22 molecular sieve loaded with 1-siloxane-3-acetic acid imidazole chloride ionic liquid is obtained, which is the prepared immobilized ionic liquid C. The loading rate of the ionic liquid is 15%.

[0071] Accurately weigh 0.18g of fructose, 0.025g of immobilized ionic liquid C, 10ml of isopropanol, 100°C, react for 2h, after the reaction is over, cool, the filtrate obtained after filtration ...

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Abstract

The invention belongs to the technical fields of catalyst preparation method and efficient-conversion of biomass and discloses immobilized ionic liquid catalyst used for preparing 5-hydroxymethylfurfural and preparation of the immobilized ionic liquid catalyst. The catalyst is obtained by immobilizing acidic functional ionic liquid on a carrier, wherein load of the ionic liquid on the carrier is 5%-30%; the catalyst is used for preparing 5-hydroxymethylfurfural. By the arrangement, mild conditions are achieved, operation cost is low, catalytic effect of the catalyst is good, problems about loss of the catalyst and solvent loss and the like during reaction can be effectively solved, regeneration of the catalyst is facilitated, and recycling effect is good.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation methods and high-efficiency conversion of biomass, and specifically relates to a new in-situ preparation method of immobilized ionic liquid and its application in the catalytic conversion of biomass to prepare 5-hydroxymethylfurfural. Background technique [0002] As we all know, non-renewable resources such as coal and oil are the basis for the rapid development of human society. However, with the continuous progress of social civilization, traditional fossil energy is increasingly exhausted, so people have to find a renewable energy as a substitute for fossil resources. Biomass refers to various organisms produced through photosynthesis using the atmosphere, water, and land. It is the fourth largest energy source after oil, coal, and natural gas, and is the most common renewable resource on earth. Currently, biomass utilization and conversion technologies are mainly divided into dir...

Claims

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Application Information

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IPC IPC(8): B01J31/26C07D307/46
CPCY02P20/584B01J31/26B01J31/0292C07D307/46
Inventor 李雪辉汤洛龙金星刘思洁张雄宋畅华
Owner SOUTH CHINA UNIV OF TECH
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