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Metal-free one-pot method for preparing 5-methyl furfural from biomass resource

A biomass resource, methyl furfural technology, applied in the direction of organic chemistry, etc., can solve the problems of expensive catalyst and complicated process, and achieve the effect of avoiding material loss and simplifying the operation process.

Active Publication Date: 2019-06-28
NANCHANG UNIV
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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 shortcomings of expensive catalysts and complex processes in the existing technology for preparing 5-methylfurfural. The present invention provides a method for preparing 5-methylfurfural from biomass without metal participation.

Method used

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  • Metal-free one-pot method for preparing 5-methyl furfural from biomass resource

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 100mg of starch, 2mmol of sodium iodide, 2ml of water, 0.18mmol of HCl (37wt%), 5ml of 2-methyltetrahydrofuran in a 50mL high-temperature and high-pressure reactor, seal the reactor, fill it with hydrogen (300psi), stir and rapidly heat to 160 ℃, keep 2h. Reactor ice water bath is cooled to room temperature, collects organic phase and detects that the productive rate of 2-methylfuran in its product is 4.9%, the productive rate of furfural is 1.9%, the productive rate of 5-methylfurfural is 37.7%, total The yield was 44.5%.

[0020] The detection and calculation of 5-methylfurfural productive rate are carried out according to the following method:

[0021] Quantitative analysis adopts gas chromatograph Agilent 7820A series (FID detector, AgilentHP-5 chromatographic column: 30m*32um*0.25um). Qualitative analysis was carried out using a gas phase mass spectrometer ThermoscientificTRACE1310 (HP-5 capillary column 30m*320μm*0.25μm).

[0022] 5-Methylfurfural yield cal...

Embodiment 2

[0025] Add 100mg starch, 4mmol sodium iodide, 2ml water, 0.18mmolH 2 SO 4 , 3ml of furan, stirred and rapidly heated to 160°C for 2h. Reactor ice water bath is cooled to room temperature, collects organic phase and detects that the productive rate of 2-methylfuran in its product is 4.8%, the productive rate of furfural is 2.1%, the productive rate of 5-methylfurfural is 34.3%, total The yield was 41.2%.

Embodiment 3

[0027] Add 100mg starch, 2mmol sodium iodide, 2ml water, 0.18mmol CF 3 SO 3 H. 3ml of 2-methyltetrahydrofuran, sealed the reaction vessel, filled with hydrogen (300psi), stirred and rapidly heated to 160°C, and kept for 2h. Reactor ice-water bath is cooled to room temperature, collects organic phase and detects through gas chromatography, and the productive rate of 2-methylfuran in its product is 1.9%, the productive rate of furfural is 1.6%, and the productive rate of 5-methylfurfural is 29.0%. %, the total yield is 31.5%.

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Abstract

The invention relates to the technical field of catalysis and particularly relates to a metal-free one-pot method for preparing a 5-methyl furfural from biomass resource. The method comprises the steps of sequentially adding biomass or a derivative and iodide of the biomass, a solvent and acid into a high-temperature high-pressure reaction kettle, introducing a certain amount of hydrogen into thereaction kettle, reacting for a certain period of time, after the reaction is finished, collecting an organic phase, and carrying out fractional distillation, so as to obtain 5-methyl furfural, wherein the yield of 5-methyl furfural reaches up to 51.9%. The method has a low requirement on production equipment under low-temperature and low-pressure conditions and is accordant with a safety production principle; and 5-methyl furfural is converted through the selective hydrogenolysis of the biomass or the derivative of the biomass without metals, the regeneration cost of the raw material is low,the cycle performance is good, the process is simple, the conditions are mild, the product is easily separated, and the loss of the materials in an intermediate step is avoided, so that the maximum utilization of the resources is realized.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and relates to a metal-free method for preparing 5-methylfurfural from biomass resources in one pot. Background technique [0002] Biomass is currently the only sustainable source of organic carbon on Earth and is an ideal petroleum substitute for the production of fuels, chemicals and materials. However, the complex structure and chemistry of most bio-based raw materials restrict their large-scale application. Biomass cellulose and starch are both macromolecular polysaccharides composed of glucose, which are widely distributed in nature and account for more than 50% of the carbon content in the plant kingdom. Starch is abundant in nature and exists in staple foods such as potatoes, wheat, corn, rice and cassava, and is the most common bio-based raw material in the human diet. Glucose and fructose are the most common hexoses in nature, and their downstream derivatives, 5-hydroxymethylfurfural...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/46
CPCY02P20/584
Inventor 杨维冉彭阳高天李香花施鹤贤李腾
Owner NANCHANG UNIV