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Novel method for preparing 5-hydroxymethylfurfural and furfural by adopting biomass raw material

A biomass raw material, the technology of hydroxymethyl furfural, applied in the direction of organic chemistry and the like, can solve the problems of complex catalyst preparation, high price and the like, and achieve the effects of good industrialization prospects, low cost and environmental friendliness

Inactive Publication Date: 2014-10-01
湖南清欣绿色环保有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation of the catalyst is too complicated and expensive to be the biggest obstacle to its industrialization (A.H. Jadhav et al. Chemical Engineering Journal 243 (2014) 92–98)

Method used

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  • Novel method for preparing 5-hydroxymethylfurfural and furfural by adopting biomass raw material
  • Novel method for preparing 5-hydroxymethylfurfural and furfural by adopting biomass raw material
  • Novel method for preparing 5-hydroxymethylfurfural and furfural by adopting biomass raw material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 0.2 g of fructose, 0.2 g of iron phosphate, 10 mL of high-purity water, and 50 mL of THF into a 100 mL autoclave, and react at a speed of 350 r / min and a temperature of 140 °C for 15 min. The product is separated into an aqueous phase and an organic phase using a separatory funnel , the content of reducing sugar in the aqueous phase was measured by DNS method, and the content of 5-HMF in the organic phase was determined by high performance liquid chromatography. The conversion rate of fructose was >99%, the yield of HMF was 71.49%, and the selectivity was 71.58%.

Embodiment 2-4

[0033] Add 0.2 g of fructose, 0.05 g of iron phosphate, 10 mL of high-purity water, and 30 mL of THF into a 100 mL autoclave, and react at a speed of 350 r / min and a temperature of 140 °C for 5, 15, and 30 min respectively, and separate the products using a separatory funnel It is an aqueous phase and an organic phase, the content of reducing sugar in the aqueous phase is measured by DNS method, and the content of 5-HMF in the organic phase is determined by high performance liquid chromatography. The specific reaction results are listed in Table 1.

[0034] Table 1 The conversion rate of fructose at different reaction times, the yield and selectivity of 5-HMF.

[0035]

Embodiment 5-8

[0037] Add 0.2 g of fructose, 0.05 g of iron phosphate, 10 mL of high-purity water, and 30 mL of THF into a 100 mL autoclave, and react at 120, 140, 160, and 180 °C for 15 min at a speed of 350 r / min. The separating funnel was separated into water phase and organic phase, the content of reducing sugar in the water phase was measured by DNS method, and the content of 5-HMF in the organic phase was determined by high performance liquid chromatography. The specific reaction results are listed in Table 2.

[0038] Table 2 The conversion rate of fructose, the yield and selectivity of 5-HMF under different reaction temperatures.

[0039]

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Abstract

The invention relates to a method for preparing 5-hydroxymethylfurfural and furfural by adopting a biomass raw material. The method comprises the following steps: adding the biomass raw material, solvent, solid phosphate catalyst and soluble inorganic salt into a reactor to form a reaction system; carrying out the dehydration reaction for 0 to 100h under the protection of inert gases at the temperature of 20 to 400 DEG C to obtain products 5-hydroxymethylfurfural and furfural with high yield. The novel method has the advantages that the weaknesses of the prior art that the toxicity of catalyst is large, equipment is likely to corrode, the price is high, the preparation method is complicated, recycling is difficult to realize and the like can be overcome. The solid catalyst has the characteristics of high catalytic activity, high selectivity, high efficiency, environmental friendliness, less byproducts, recyclability and the like, and is easy to separate and recycle.

Description

technical field [0001] The invention relates to a new method for preparing 5-hydroxymethylfurfural (5-HMF) and furfural by converting biomass raw materials, belonging to the field of biomass conversion and synthesis of important chemicals. Background technique [0002] Most of the energy and organic chemicals needed in the world today come from petroleum, coal and natural gas. However, with the gradual depletion of these non-renewable fossil energy sources and in order to achieve the purpose of sustainable development of human beings, making full use of renewable and degradable resources and making them an important industrial raw material through chemical synthesis has become a solution to resource depletion and the environment. effective means of pollution. Glucose, fructose, sucrose, hemicellulose, cellulose, lignin and other biomass raw materials are abundant in nature and low in price. They are important biomass resources. They can be synthesized into high value-added ...

Claims

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Application Information

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IPC IPC(8): C07D307/50C07D307/46
CPCC07D307/46C07D307/50
Inventor 夏海岸闫晓沛陈皓左宋林
Owner 湖南清欣绿色环保有限公司
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