Method for preparing 5-hydroxymethyl furfural from glucose
A technology of hydroxymethylfurfural and glucose, which is applied in the field of preparing 5-hydroxymethylfurfural from glucose, can solve the problems of unfriendly environment, high energy consumption for separation, high price, etc., and achieve low toxicity, environmental friendliness, simple preparation process, The effect of cheap and easy-to-obtain raw materials
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[0024] The preparation method of solid acid catalyst in following embodiment comprises the steps:
[0025] a. ZrOCl 2 ·8H 2 Dissolve O in deionized water, add HZSM-5 and stir to suspend, in which ZrOCl 2 ·8H 2 The ratio of O to deionized water is 1g: 100mL;
[0026] b. Add ammonia water dropwise to the material obtained in step a to stabilize the pH at 8 to 9, then age for 8 to 12 hours and filter to remove Cl - ;
[0027] c. Dry the material obtained in step b at 100-120° C. for 7-9 hours;
[0028] d, use the material obtained in step c with 0.5~1M H 2 SO 4 Vulcanize for 2 to 3 hours;
[0029] e. Calcining the material obtained in step d at 500-600°C for 2.5-3.5 hours to obtain the solid acid catalyst, expressed as S / Z x -HZSM, where S means SO 4 2- , Z means ZrO 2 , x is ZrO 2 Ratio to mass ratio of HZSM-5.
Embodiment 1
[0031] 0.15g glucose, 0.05gS / Z 0.05 -HZSM, 1.5mL 25%wt NaCl aqueous solution and 3.5mL ethyl acetate were added to the autoclave, heated to 195°C at a stirring speed of 450rpm and reacted for 2h to obtain a reaction phase and an extraction phase, and the extraction phase was taken for detection. According to gas chromatography analysis, the calculated yield of 5-hydroxymethylfurfural was 36.61%.
Embodiment 2
[0033] 0.3g glucose, 0.1gS / Z 0.05 -HZSM, 3mL 25%wt NaCl aqueous solution and 7mL ethyl acetate were added to the autoclave, heated to 195°C at a stirring speed of 450rpm and reacted for 2h to obtain the reaction phase and the extract phase. Analysis, the calculated yield of 5-hydroxymethylfurfural was 38.13%.
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