Method for preparing 5-hydroxymethylfurfural by solid acid catalysis
A hydroxymethylfurfural, solid acid catalysis technology, applied in chemical instruments and methods, catalyst carriers, physical/chemical process catalysts and other directions, can solve the problems of waste of resources, physical and chemical properties and processing performance obstacles, etc. Reaction activation energy, effect of lowering reaction temperature
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Embodiment 1
[0021] The residual lignin sample was dried at 105°C, and 10g of dry lignin was carbonized at 400°C for 10h under the protection of an inert gas to obtain a black solid Powder, porous carbon carrier:concentrated sulfuric acid mass ratio 1:5, black solid powder washed with deionized water and dried to obtain lignin-based solid acid.
[0022] Add 10mL deionized water to the autoclave, preheat to 80°C, then add 0.5g lignin-based solid acid and 2g fructose, stir, heat to 150°C within 10min, and react at constant temperature for 300min. After the reaction, samples were taken and cooled with cold water at 0-20° C., diluted with ultrapure water, and analyzed by liquid chromatography for the content of fructose and 5-hydroxymethylfurfural. The conversion rate of fructose was 100%, and the yield of 5-hydroxymethylfurfural was 16%.
Embodiment 2
[0024] The residual lignin sample was dried at 105°C, and 10g of dry lignin was carbonized at 400°C for 5 hours under the protection of an inert gas to form a porous carbon carrier, and the porous carbon carrier was sulfonated with 98% concentrated sulfuric acid at 200°C for 10 hours to obtain a black solid Powder, porous carbon carrier:concentrated sulfuric acid mass ratio 1:10, washed with deionized water and dried to obtain lignin-based solid acid.
[0025] Add 20mL of deionized water to the autoclave, preheat to 80°C, then add 1g of lignin-based solid acid and 4g of fructose, stir, heat to 150°C within 5min, and react at constant temperature for 60min. After the reaction, samples were taken and cooled with cold water at 0-20° C., diluted with ultrapure water, and analyzed by liquid chromatography for the content of fructose and 5-hydroxymethylfurfural. The conversion rate of fructose was 100%, and the yield of 5-hydroxymethylfurfural was 39%.
Embodiment 3
[0027] The residual lignin sample was dried at 105°C, and 10g of dry lignin was carbonized at 400°C for 5 hours under the protection of an inert gas to form a porous carbon carrier, and the porous carbon carrier was sulfonated with 98% concentrated sulfuric acid at 200°C for 5 hours to obtain a black solid Powder, porous carbon carrier:concentrated sulfuric acid mass ratio 1:10, washed with deionized water and dried to obtain lignin-based solid acid.
[0028] Add 2g of [Bmim]Cl into the microwave reactor, heat to 120°C within 5min, then add 0.2g of lignin-based solid acid and 0.2g of fructose, stir, and react at constant temperature for 30min. After the reaction, samples were taken and cooled with cold water at 0-20° C., diluted with ultrapure water, and analyzed by liquid chromatography for the content of fructose and 5-hydroxymethylfurfural. The conversion rate of fructose was 85%, and the yield of 5-hydroxymethylfurfural was 71%.
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