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Method for preparing HMF (5-hydroxymethylfurfural) from glucose by lower-temperature catalysis with boehmite

A technology of hydroxymethyl furfural and boehmite, applied in chemical recovery, organic chemistry and other directions, can solve problems such as high reaction temperature and complicated catalyst preparation, achieve simple preparation method, good industrial application prospect, and avoid a large number of side reactions Effect

Active Publication Date: 2018-10-02
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the technical problem that the reaction temperature is too high or the preparation of the catalyst is complicated in the high-efficiency preparation of HMF from glucose by heterogeneous catalysis, and to provide a new method for the preparation of HMF from glucose with one-step low-temperature and high-efficiency catalysis of boehmite (γ-AlOOH) Method, the catalyst boehmite (γ-AlOOH) that this method adopts is stable in property

Method used

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  • Method for preparing HMF (5-hydroxymethylfurfural) from glucose by lower-temperature catalysis with boehmite
  • Method for preparing HMF (5-hydroxymethylfurfural) from glucose by lower-temperature catalysis with boehmite
  • Method for preparing HMF (5-hydroxymethylfurfural) from glucose by lower-temperature catalysis with boehmite

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Experimental program
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Effect test

Embodiment 1

[0032] 30mmol NH 4 HCO 3 and 15mmol Al(NO 3 ) 3was added to 50 mL of deionized water with vigorous stirring. After it became a clear and transparent homogeneous solution, 25% concentrated ammonia solution was slowly added dropwise to adjust the pH to 9. After it became a homogeneous mixed solution, it was transferred to a 100 mL Teflon-lined reaction kettle, and reacted at 150° C. for 12 h. When the reaction time reaches the set time, take out the reactor. After being naturally cooled to room temperature, the reactor was opened to separate and wash the catalyst to obtain a solid product. Finally, the solid product was dried at 150° C. for 12 h to obtain the solid catalyst γ-AlOOH. This solid catalyst was subjected to XRD analysis. like figure 2 shown, from figure 2 It can be seen that all the diffraction peaks of the sample are consistent with the diffraction peaks of the orthogonal γ-AlOOH (JCPDS 021-1307) marker, and no diffraction peaks of other substances are ob...

Embodiment 2

[0036] The preparation method of γ-AlOOH is the same as that of Example 1. The experimental process of glucose conversion to prepare HMF is also the same as in Example 1.

[0037] The amount of dimethyl sulfoxide (DMSO) was increased to 2.0 g during the preparation of 5-hydroxymethylfurfural. The specific process is as follows: 0.1 g of glucose and 0.1 g of solid catalyst γ-AlOOH were added to 2.0 g of dimethyl sulfoxide, and after stirring evenly, the above solution was transferred to an oil bath at 130 °C, and the reaction was conducted under magnetic stirring for 3 h. After the reaction was completed, 20 mL of cold deionized water was immediately added to the reaction solution for quenching treatment. The centrifuge was then used for separation at a speed of 10,000 rpm for 5 min, and the upper layer liquid was collected to obtain a degradation solution containing HMF. Take out a small amount of this degradation solution, dilute it 300 times with deionized water, and then ...

Embodiment 3

[0039] The preparation method of γ-AlOOH is the same as that of Example 1. The experimental process of glucose conversion to prepare HMF is also the same as in Example 1.

[0040] The amount of dimethyl sulfoxide (DMSO) was reduced to 0.5 g during the preparation of 5-hydroxymethylfurfural. The specific process is as follows: 0.1 g of glucose and 0.1 g of solid catalyst γ-AlOOH were added to 0.5 g of dimethyl sulfoxide, and after stirring evenly, the above solution was transferred to a 130 °C oil bath pot, and the reaction was conducted under magnetic stirring for 3 h. After the reaction was completed, 20 mL of cold deionized water was immediately added to the reaction solution for quenching treatment. The centrifuge was then used for separation at a speed of 10,000 rpm for 5 min, and the upper layer liquid was collected to obtain a degradation solution containing 5-hydroxymethylfurfural. Take out a little of this degradation solution, dilute it 200 times with deionized wate...

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Abstract

The invention discloses a method for preparing HMF (5-hydroxymethylfurfural) from glucose by lower-temperature catalysis with boehmite. The method specifically comprises the following steps: boehmitegamma-AlOOH and glucose are added to dimethyl sulfoxide, the substances are mixed and transferred to a position at 80-180 DEG C for a stirring reaction, deionized water is added to a reaction liquid after the reaction for quenching treatment, then centrifugation is performed, an upper liquid is collected, and a degradation liquid containing HMF is obtained. When HMF is prepared from glucose by catalysis with the method, the method has the characteristics of low temperature, high efficiency (high HMF yield and high selectivity), easily separable and recyclable catalyst, low energy consumption and the like, and has quite high application value; a large quantity of side effects can be avoided, product selectivity can be improved, and product separation cost can be reduced.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a method for preparing 5-hydroxymethylfurfural (HMF) from boehmite (γ-AlOOH) by catalyzing glucose in one step with low temperature and high efficiency. Background technique [0002] 5-Hydroxymethylfurfural (HMF) is an important biomass platform compound with the ability to synthesize a variety of high value-added chemicals, such as 2,5-diformylfuran (DFF), 2,5-furandi Carboxylic acid (FDA), 2,5-dimethylolfuran (BHMF), 2,5-dimethylfuran (DMF), levulinic acid (LA), etc., have very important research and industrial application value. At present, the synthesis of HMF is mainly obtained from two common monosaccharides, glucose and fructose, in a certain catalyst system. However, compared with fructose, glucose is more abundant in nature, more readily available and cheaper, and it is a more ideal raw material for the preparation of HMF. [0003] At present, there are m...

Claims

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Application Information

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IPC IPC(8): C07D307/46
CPCC07D307/46Y02P20/584
Inventor 唐喆苏建辉姜瑞雨仓辉韩粉女许琦
Owner YANCHENG INST OF TECH
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