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Preparation method of solid acid catalyst for preparing 5-hydroxymethylfurfural from biomass

A solid acid catalyst, a technology of hydroxymethyl furfural, which is applied in the fields of catalytic chemistry and biomass resource utilization, can solve the problems of poor catalyst stability, decreased reaction activity, and is not suitable for large-scale production, and achieves stable structure and good water resistance. Effect

Active Publication Date: 2017-05-17
EAST CHINA UNIV OF SCI & TECH
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  • Abstract
  • Description
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Problems solved by technology

For example, Antonio Jiménez-López et al. used Al-MCM-41 to catalyze glucose to prepare HMF, and the yield could reach 63%, but the catalyst had poor stability, and after three times of use, the reaction activity dropped significantly (Appl.Catal., B, 2015 , 164, 70–76.)
Du Yuguang's research group used WO 3 -Ta 2 o 5 Catalytic conversion of carbohydrates to prepare HMF to obtain HMF with high yield and high stability (patent number: CN201110435929.3), but the tantalum source (tantalum chloride, tantalum ethoxide, etc.) in the material preparation process is expensive and not suitable for industrialization mass production

Method used

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  • Preparation method of solid acid catalyst for preparing 5-hydroxymethylfurfural from biomass
  • Preparation method of solid acid catalyst for preparing 5-hydroxymethylfurfural from biomass
  • Preparation method of solid acid catalyst for preparing 5-hydroxymethylfurfural from biomass

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Experimental program
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Effect test

Embodiment 1-18

[0030] Weigh a certain amount of carbon source and 2 grams of niobium source into a beaker, add it to 20mL acidic solution, stir continuously for 2 hours, transfer the obtained solution to a stainless steel autoclave lined with polytetrafluoroethylene, and crystallize at a certain temperature After some time a dark brown solid was obtained. After washing with deionized water, drying, and then placing in a tube furnace, carbonizing for a certain period of time in a nitrogen atmosphere and at a certain temperature, the required niobium-carbon solid acid catalyst (carbon source, niobium source, mass ratio , synthesis solvent, and carbonization temperature are shown in Table 1, and the physicochemical parameter characterization results of each solid acid catalyst are shown in Table 2).

[0031] Add 0.2 g of catalyst, 0.2 g of cellulose, 6 mL of tetrahydrofuran, and 2 mL of saturated aqueous sodium chloride into a high-pressure magnetic stirring batch reactor, fill with 0.5 MPa nit...

Embodiment 34-48

[0033] Add 0.2 g of the catalyst in the above example, 0.2 g of biomass raw material, 6 mL of tetrahydrofuran, 2 mL of saturated aqueous sodium chloride solution into a high-pressure magnetic stirring batch reaction kettle, fill with 0.5 MPa nitrogen, heat to 180 ° C, and react at constant temperature for 8 hours , the reaction system was cooled to room temperature (25°C), and the catalyst was separated by centrifugation. The reaction solution was analyzed by high performance liquid chromatography, and the yield of 5-hydroxymethylfurfural was calculated, as shown in Table 3.

Embodiment 49

[0035] Add 0.2 g of the catalyst of Example 1, 0.2 g of cellulose, 6 ml of tetrahydrofuran, and 2 ml of saturated aqueous sodium chloride into a high-pressure magnetic stirring batch reactor, fill with 0.5 MPa nitrogen, heat to 180 ° C, and react at a constant temperature for 8 hours. The reaction system was cooled to room temperature (25°C), and the catalyst was separated by centrifugation. The reaction solution was analyzed by high performance liquid chromatography, and the yield of 5-hydroxymethylfurfural was calculated. The catalyst was put into the next reaction after being washed with deionized water, and a total of 8 reactions were used in a cycle. The results of each reaction are shown in the attached figure 2 , it can be seen that the niobium-carbon solid acid catalyst exhibits good cycle stability.

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Abstract

The invention relates to a preparation method of a solid acid catalyst for preparing 5-hydroxymethylfurfural from biomass. The solid acid catalyst is a compound of charcoal and niobium pentoxide and has an amorphous structure. The preparation method comprises the steps that with carbohydrate compounds as a carbon source, tartaric acid, niobium oxalate, niobium citrate, niobium pentachloride or other niobium salts as a niobium source as well as inorganic or organic acid as a catalyst, the compound is prepared by virtue of a hydrothermal or solvothermal method, and high temperature carbonization is implemented under nitrogen, so as to obtain the niobium-charcoal solid acid catalyst. The solid acid catalyst is applied to dehydration reaction of saccharides and cellulose, the yield of the product 5-hydroxymethylfurfural is high, and the cycle use performance of the catalyst is good; and the solid acid catalyst is a very good catalyst for preparing 5-hydroxymethylfurfural through biomass catalytic conversion.

Description

technical field [0001] The invention relates to a method for preparing a solid acid catalyst for preparing 5-hydroxymethylfurfural from biomass, and relates to the fields of catalytic chemistry and utilization of biomass resources. Background technique [0002] With the rapid growth of the world economy, fossil fuel (especially oil) resources are becoming increasingly scarce, and their use has brought a series of social and environmental problems to human society. Therefore, from one of the renewable energy sources The research on the synthesis of fuels and fine chemicals from substances and their derivatives has become one of the hotspots of scientists at home and abroad. Because biomass has the advantages of sustainability and wide sources, and 5-hydroxymethylfurfural is an important class of furan compounds, it can be used to prepare liquid fuel 2,5-dimethylfuran, long-chain alkanes, pharmaceutical intermediates 2,5-diformylfuran, polyester monomer 2,5-furandicarboxylic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/20B01J31/02C07D307/46
CPCB01J23/20B01J31/02C07D307/46
Inventor 王艳芹李相呈刘晓晖夏启能
Owner EAST CHINA UNIV OF SCI & TECH
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