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A method for preparing 5-hydroxymethylfurfural from glucose catalyzed by boehmite at low temperature

A technology of hydroxymethyl furfural and boehmite, applied in the directions of organic chemistry, chemical recovery, etc., can solve the problems of high reaction temperature, complicated catalyst preparation, etc., achieves simple preparation method, good industrial application prospect, and avoids a large number of side reactions Effect

Active Publication Date: 2021-12-10
YANCHENG INST OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A method for preparing 5-hydroxymethylfurfural from glucose catalyzed by boehmite at low temperature
  • A method for preparing 5-hydroxymethylfurfural from glucose catalyzed by boehmite at low temperature
  • A method for preparing 5-hydroxymethylfurfural from glucose catalyzed by boehmite at low temperature

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Embodiment 1

[0032] The 30mmol NH 4 HCO 3 And 15mmol Al (NO 3 ) 3The addition of 50 ml of deionized water in strong agitation. After it turns into a clear transparent homogeneous solution, 25% of the concentrated aqueous solution is slowly added to adjust the pH to 9. After it turned into a uniform mixture, it was transferred to 100 mL of the reactor of the inner lining polytetrafluoroethylene, and at 150 ° C for 12 h. When the reaction time reaches the set time, the reactor is removed. Naturally, after cooling to room temperature, the reactor is opened, and the separation of the catalyst and washing work is performed, and the solid product is obtained. Finally, the solid product was dried at 150 ° C for 12 h, i.e., obtained solid catalyst γ-Alooh. This solid catalyst was analyzed by XRD. like figure 2 As shown, from figure 2 It can be seen that all diffraction peaks of the sample are consistent with the orthogonal γ-AlOOH (JCPDS 021-1307) marker diffraction peak, and no other substance diffra...

Embodiment 2

[0036] The γ-AlOOH preparation method and Example 1 were identical. Glucose conversion is also the same as in Example 1.

[0037] Dimethyl sulfoxide (DMSO) was increased to 2.0 g during the preparation of 5-hydroxymethylfurifer. 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 the above solution was transferred to a 130 ° C oil bath, and the magnetic force was stirred. After the reaction was completed, 20 ml of cold deionized water was added to the reaction mixture for quenching treatment. The re-use centrifuge was separated at a speed of 10000 rpm, and the upper liquid was collected, and the degradation of HMF was obtained. The little degradation solution was taken, 300 times diluted with deionized water, and then analyzed using the product in the degradation liquid using high performance liquid chromatography, and the HMF yield of the reaction was 60% and HMF selectivity of 63%, glucose conver...

Embodiment 3

[0039] The γ-AlOOH preparation method and Example 1 were identical. Glucose conversion 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-hydroxymethyl furfural. 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 the above solution was transferred to a 130 ° C oil bath, and the magnetic force was stirred. 3 h. After the reaction was completed, 20 ml of cold deionized water was added to the reaction mixture for quenching treatment. After the centrifuge was separated at a speed of 10000 rpm, the upper liquid was collected, and the degradation of 5-hydroxyhydehydehyde was obtained. The little degradation solution was taken out, diluted with deionized water, and then analyzed the product in the degradation liquid using high performance liquid chromatography, calculated that the HMF yield of the reaction was 45% and HMF se...

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Abstract

The invention discloses a method for preparing 5-hydroxymethylfurfural from glucose catalyzed by boehmite at low temperature. Specifically, adding boehmite γ-AlOOH and glucose to dimethyl sulfoxide and transferring to 80~ The reaction was stirred at 180° C., and after the reaction was completed, deionized water was added to the reaction liquid for quenching treatment, centrifuged, and the upper liquid was collected to obtain a degradation liquid containing 5-hydroxymethylfurfural. When the method of the present invention is used to catalyze glucose to produce HMF, it has the characteristics of low temperature, high efficiency (high HMF yield and selectivity), easy separation of the catalyst, reusable use, and low energy consumption, which can avoid a large number of side reactions and improve product selectivity , reduce the cost of product separation, and have extremely high application value.

Description

Technical field [0001] The present invention belongs to the technical field of catalyst, particularly a process for preparing 5-hydroxymethylfurfural (of HMF) A boehmite (γ-AlOOH) allows high-temperature step catalytic glucose. Background technique [0002] 5-hydroxymethyl furfural (of HMF) is an important biomass platform chemical, the ability to synthesize a variety of high value added chemicals, such as 2,5-diformylfuran (the DFF), 2,5-furandicarboxylic carboxylic acid (FDA), 2,5- bis (hydroxymethyl) furan (BHMF), 2,5- dimethylfuran (DMF), levulinic acid (LA) and the like, having a value very important research and industrial applications. Currently HMF synthesis mainly glucose, fructose two common monosaccharides in a certain catalyst system. However, compared with fructose, glucose nature, content richer, more readily available, more affordable, is more desirable raw material preparation of HMF. [0003] Currently more Glucose HMF preparation methods, including homogeneous c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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