Method for preparing 5-hydroxymethylfurfural through directed liquefaction of wood fiber

A technology of hydroxymethylfurfural and lignocellulosic, applied in the field of preparing 5-hydroxymethylfurfural, which can solve the problems of high corrosiveness of liquid inorganic acid catalysts, difficulty in converting lignocellulosic raw materials, harsh reaction conditions, etc., and achieve high pretreatment efficiency Easy to operate, excellent thermal and chemical stability, simple pretreatment effect

Pending Publication Date: 2019-03-29
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) The liquid inorganic acid catalyst is highly corrosive, difficult to recycle, and the process cost is high
[0006] (2) Conventional solid acid catalysts have low catalytic activity, long reaction time and high reaction temperature
[0007] (3) New catalysts such as ionic liquids and supercritical fluids have high costs and harsh reaction conditions
[0008] (4) cellulose, glucose or fructose are mostly used as raw materials, and the cost of raw materials is high, so it is difficult to apply in the conversion of lignocellulosic raw materials

Method used

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  • Method for preparing 5-hydroxymethylfurfural through directed liquefaction of wood fiber
  • Method for preparing 5-hydroxymethylfurfural through directed liquefaction of wood fiber
  • Method for preparing 5-hydroxymethylfurfural through directed liquefaction of wood fiber

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Experimental program
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Effect test

Embodiment 1

[0045] The first step: pretreatment of lignocellulosic raw materials: firstly, the lignocellulosic raw material willow is washed with deionized water and dried, and then crushed to about 200 mesh by a high-speed pulverizer, and the mass ratio of lignocellulosic raw material powder and sulfolane is 1:1 / water composite solvent (wherein the mass ratio of sulfolane to water is 90:10) is mixed with a mass fraction of 1% solid acid catalyst and placed in a pre-mixing tank, stirred at room temperature to a slurry state, ready for use.

[0046] Step 2: Preparation of solid acid: Put the purchased granular activated carbon in a three-necked flask, dissolve tin chloride in deionized water as a solvent, then pour it into the three-necked flask, heat to 120°C under magnetic stirring, reflux for 0.1h, and filter The resulting filter cake was thoroughly washed with the above-mentioned solvent and dried in vacuum before use.

[0047] Step 3: Hydrolysis of lignocellulosic raw materials: Add ...

Embodiment 2

[0050] The first step: pretreatment of lignocellulosic raw materials: first, the lignocellulosic raw material poplar is washed with deionized water and then dried, then crushed to about 200 mesh by a high-speed pulverizer, and the mass ratio is 1:5 lignocellulosic raw material powder and The γ-valerolactone / water composite solvent (the mass ratio of sulfolane to water is 90:10) is mixed with a solid acid catalyst with a mass fraction of 10% and placed in a premixing tank, stirred at room temperature until it reaches a slurry state, and is ready for use.

[0051] Step 2: Preparation of solid acid: Put the purchased granular activated carbon in a three-necked flask, dissolve zinc chloride in the solvent anhydrous methanol and pour it into the three-necked flask, heat to 70°C under magnetic stirring and reflux for 0.2h, Filter and thoroughly wash the obtained filter cake with the above-mentioned solvent and dry it in vacuum before use.

[0052] Step 3: Hydrolysis of lignocellulos...

Embodiment 3

[0055] The first step: pretreatment of lignocellulosic raw materials: first, the lignocellulosic raw material poplar is washed with deionized water and then dried, then crushed to about 200 mesh by a high-speed pulverizer, and the mass ratio is 1:10 lignocellulosic raw material powder and N,N-dimethylformamide / water composite solvent (wherein the mass ratio of sulfolane to water is 90:30) is mixed with a mass fraction of 5% solid acid catalyst and placed in a pre-mixing kettle, stirred at room temperature to a slurry state, ready for use .

[0056] Step 2: Preparation of solid acid: Place the purchased granular activated carbon in a three-necked flask, dissolve magnesium chloride in the solvent absolute ethanol and pour it into the three-necked flask, heat to 80°C under magnetic stirring for 0.3h, filter and use The obtained filter cake was thoroughly cleaned with the above solvent and dried in vacuum before use.

[0057] Step 3: Hydrolysis of lignocellulosic raw materials: A...

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Abstract

The invention provides a method for preparing 5-hydroxymethylfurfural through directed liquefaction of wood fiber. The method comprises the steps: adopting wood fiber as a raw material, mixing the wood fiber with a self-made solid acid catalyst and a composite solvent of a polar aprotic solvent and water firstly, pretreating the obtained wood fiber raw material by using a slurry-state method at room temperature, raising the temperature so as to achieve directed catalytic liquefaction and prepare 5-hydroxymethylfurfural; performing filtration, preparing the solid acid catalyst by using the solid residues, and performing fractional reduced pressure distillation on the filtrate so as to isolate water and the target product 5-hydroxymethylfurfural and by-products including furfural and levulinic acid and obtain the remaining aprotic solvent. The renewable wood fiber with a wide source is adopted as the raw material, and thus environmental protection and low cost are achieved; and in the composite solvent system of the polar aprotic solvent and water, a good selectivity to the target product 5-hydroxymethylfurfural, high yield, easy separation, efficient recycling utilization of the solvents, the catalyst and other matter and environmental protection can be achieved, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technology of preparing 5-hydroxymethylfurfural, in particular to the method of pretreating lignocellulosic raw materials by slurry method and then directional liquefaction to prepare 5-hydroxymethylfurfural. Background technique [0002] In recent years, with the depletion of non-renewable fossil oil resources on the earth and the increasing environmental pollution worldwide, people are paying more and more attention to the use of renewable resources to produce energy or chemicals to meet the needs of human society. Biomass is rich in reserves and is a renewable and cheap resource. Biomass resources are playing an increasingly important role in the progress of human society. It is considered to be the most effective resource to partially replace petroleum resources. Lignocellulosic is an abundant biomass resource that can be directly converted into liquid fuels and fine chemicals, and thus is considered an ideal substitute...

Claims

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Application Information

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IPC IPC(8): C07D307/46
CPCC07D307/46Y02P20/584
Inventor 王奎蒋剑春刘超卫民徐俊明李静夏海虹刘朋叶俊周铭昊王霏
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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