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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 catalytic system of previous studies, such as cost, catalyst and solvent recycling, and product separation and purification. Therefore, it is important to develop a large-scale, economical, sustainable, and green HMF production process. The first problem to be solved in its industrial application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0061] (2) The white solid crude product obtained in step (1) was stirred and dispersed in 30 mL of dichloromethane, and then an appropriate amount of sulfuric acid was added dropwise (the amount of sulfuric acid was 0.11 mol), and the reaction was refluxed and stirred at 50° C. for 24 h....

Embodiment 2

[0064] (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 0.1mol 1,3-propane sultone to the solution obtained from the above reaction, stir at 40°C for 24 hours to obtain precursor II; disperse 3g of SBA-15 in 50ml of toluene, and add 1.5g of the above-obtained precursor Compound II was stirred at 100°C for 24 hours, filtered with suction, and the obtained white powder solid was washed three times with ethanol to obtain SBA-15 molecular sieves loaded with 1-siloxane-3-propanesulfoimidazolium chloride ionic liquid;

[0065] (2) the SBA-15 molecular sieve that has loaded 1-siloxane-3-propanesulfonate imidazolium chloride ionic liquid is ultrasonically dispersed in 50ml ethanol, and an appropriate amount of concentrated sulfuric acid (conc. The mass concentration of sulfuric acid is 98%, and the consumption is 0.11mol), then at 50°C, reflux and stir for 24h...

Embodiment 3

[0069] (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; after that Add 0.1 mol of chloropropionic acid to the solution obtained from the above reaction, and stir at 60° C. for 24 hours to obtain an ionic liquid;

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

[0071] Accurately weigh 0.18g of fructose, 0.025g of immobilized ionic liquid C, 10ml of isopropanol, and react for 2 hours at 100°C. After the reaction, cool and filter the filtrate ...

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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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