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Method for preparing furfural, hydroxymethylfurfural and levulinic acid by means of microchannel reaction device

A technology of hydroxymethylfurfural and microchannel reaction, which is applied in the preparation of carboxylate salts, chemical instruments and methods, and the preparation of organic compounds, can solve problems such as high energy consumption, reduced product yield, and large equipment investment, and achieve energy efficiency. Low energy consumption, improved utilization efficiency, and short processing time

Active Publication Date: 2016-07-20
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The physical method mainly uses means such as mechanical crushing and grinding, microwave radiation, steam explosion (CN1952162A) to improve the enzymatic hydrolysis efficiency of cellulase.
At the same time, because the whole process is fluid during the reaction process, the agglomeration of compounds is reduced to a large extent to form humus, which reduces the product yield.

Method used

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  • Method for preparing furfural, hydroxymethylfurfural and levulinic acid by means of microchannel reaction device
  • Method for preparing furfural, hydroxymethylfurfural and levulinic acid by means of microchannel reaction device
  • Method for preparing furfural, hydroxymethylfurfural and levulinic acid by means of microchannel reaction device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043]Dissolve 9.2 mmol of concentrated sulfuric acid in 100 ml of diethyl ether, take 10.0 g of corn stalks (60 mesh) and disperse them into the diethyl ether sulfuric acid solution, stir at 300 rpm for 1 h, distill off the diethyl ether under reduced pressure. The acid-impregnated corn stalks were put into a ball mill for ball milling (500rpm / min). Note that the temperature should not exceed 45°C for intermittent ball milling. Then the ground corn stalk powder was taken out and weighed to obtain soluble lignocellulose. Take 1g of soluble lignocellulose and disperse it into 10ml of water, shake it for 5 minutes, and filter out the insoluble matter to obtain soluble oligosaccharides and lignin. The yield of soluble oligosaccharides is above 95%.

[0044] The productive rate of soluble oligosaccharides is calculated according to the following formula:

[0045]

[0046] m 0 : the mass of soluble lignocellulose before dissolving;

[0047] m: the mass of the remaining resi...

Embodiment 2

[0050] Dissolve 9.2 mmol of acetic acid in 100 ml of diethyl ether, take 10.0 g of corn stalks (60 mesh) and disperse into the diethyl ether acetic acid solution, stir at 300 rpm for 1 h, distill off the diethyl ether under reduced pressure. The acid-impregnated corn stalks were put into a ball mill for ball milling (500rpm / min). Note that the temperature should not exceed 45°C for intermittent ball milling. Then the ground corn stalk powder was taken out and weighed to obtain soluble lignocellulose. Take 1g of soluble lignocellulose and disperse it into 10ml of water, shake it for 5 minutes, and filter out the insoluble matter to obtain soluble oligosaccharides and lignin. The yield of soluble oligosaccharides is more than 85%.

Embodiment 3～5

[0052] Using the same conditions as in Example 1, the difference is that in Example 3, acetone is used to replace ether; in Example 4, MIBK is used to replace ether; in Example 5, n-butanol is used to replace ether; the yield is shown in Table 1.

[0053] Table 1 embodiment 3~5 detection result

[0054] Example number

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Abstract

The invention discloses a method for preparing furfural, hydroxymethylfurfural and levulinic acid by means of a microchannel reaction device.The method is characterized by comprising the following steps that 1, lignocellulose is utilized for preparing a soluble oligosaccharide solution; 2, oligosaccharide in the soluble oligosaccharide solution is catalyzed by HCl to be converted into furfural or hydroxymethylfurfural or levulinic acid in the microchannel reaction device, wherein during the catalysis process, the molar ratio of soluble oligosaccharide to HCl is 1:(1-3), the temperature of the catalytic reaction ranges from 140 DEG C to 210 DEG C, the flow velocity of the catalytic reaction ranges from 1 ml / min to 6 ml / min, and the retention time of the catalytic reaction ranges from 2 min to 10 min; 3, after the reaction is completed, the reaction fluid is cooled, and furfural, hydroxymethylfurfural and levulinic acid in the reaction fluid are extracted.By means of the method, the conversion rate of pentose is 90%-97%, the highest yield of furfural reaches 92%, the conversion rate of hexose is 83%-92%, the highest yield of 5-HMF is 85%, and the height yield of levulinic acid is 87%.

Description

technical field [0001] The invention belongs to the technical field of biochemical industry, and specifically relates to a new technology for high-value utilization of lignocellulose combined with microchannel reaction devices Background technique [0002] In response to the increasingly severe energy crisis, countries all over the world have attached great importance to the development and utilization of biomass resources in recent years. Lignocellulose is the most abundant renewable biomass resource on the earth. Compared with other biomass resources such as starch and oil, lignocellulose has the unique advantage of not competing with people for food or land. Preparation of biomass energy and bio-based chemicals from lignocellulosic resources and the gradual establishment of a biorefinery economic model can alleviate dependence on the petroleum industry and reduce environmental pollution. In the conversion process of lignocellulose, the bioconversion technology based on s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/50C07D307/46C07C51/00C07C59/185
CPCC07C51/00C07D307/46C07D307/50C07C59/185
Inventor 朱晨杰郭凯唐成伦应汉杰刘铖陈彦君欧阳平凯
Owner NANJING UNIV OF TECH
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