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

Active Publication Date: 2018-04-13
XIAMEN UNIV
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Problems solved by technology

[0003] In the prior art, the catalysts for preparing 5-hydroxymethylfurfural from glucose can be simply divided into homogeneous acid catalysts and solid acid catalysts. Due to the shortcomings of homogeneous acid catalysts such as corrosion equipment, dangerous operation, and difficult recovery, solid acid catalysts has become mainstream
Among many solid acid catalysts, chromium-based solid acid catalysts show good catalytic activity in the process of catalyzing glu

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  • Method for preparing 5-hydroxymethyl furfural from glucose

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preparation example Construction

[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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Abstract

The invention discloses a method for preparing 5-hydroxymethyl furfural from glucose. The method comprises the following steps: (1) adding glucose, a solid acid catalyst, a NaCl aqueous solution and ethyl acetate into a high-pressure reaction kettle, and heating to 180-200 DEG C at a stirring speed of 400-600 rpm to react, thereby obtaining a reaction phase and an extraction phase; and (2) separating the reaction phase from the extraction phase obtained in step (1), adding glucose and ethyl acetate into the reaction phase in proportion, and continuously reacting by utilizing the solid acid catalyst in the reaction phase under conditions of the step (1). The method is simple to operate, adopts cheap and easily available raw materials, adopts the green and environment-friendly catalyst, adopts ethyl acetate with a low boiling point as an extraction solvent, so that the separating and purifying of 5-hydroxymethyl furfural from glucose is facilitated, and an industrial value is realized.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for preparing 5-hydroxymethylfurfural from glucose. Background technique [0002] 5-Hydroxymethylfurfural is an important biomass-based platform compound. The molecule contains a furan ring, an aldehyde group and a hydroxymethyl group, so it can undergo hydrogenation, oxidative dehydrogenation, esterification, halogenation, polymerization, A variety of high value-added derivatives can be prepared through hydrolysis and other reactions, such as levulinic acid, furandicarboxylic acid, furandimethanol, furandicarbaldehyde and dimethylfuran, which can be used in polymers, biofuels and other fields. 5-Hydroxymethylfurfural is mainly produced by dehydration of glucose and fructose under acidic conditions. Using fructose as raw material can often get higher yield of 5-hydroxymethylfurfural, but using glucose as raw material to prepare 5-hydroxymethylfurfu...

Claims

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Application Information

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IPC IPC(8): C07D307/46B01J29/40
CPCB01J29/405B01J2229/18C07D307/46
Inventor 曾宪海冯云超左淼孙勇唐兴林鹿
Owner XIAMEN UNIV
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