Method for preparing methyl levulinate from cellulose under mild conditions of mechanical force chemocatalysis

A technology of methyl levulinate and mechanochemistry, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of low acid concentration, few by-products, strong corrosion, etc., and achieve low reaction temperature , high synthesis yield, and the effect of deepening the degree of depolymerization

Inactive Publication Date: 2017-07-07
CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of this invention is to provide a kind of method that mechanochemically catalyzed cellulose mild condition prepares methyl levulinate, the present invention uses cellulose as raw material, carries out alcoholysis reaction after impregnating cellulose with sulfuric acid and carries out ball milling, solves the problem of The problem of high pressure and strong corrosion caused by high temperature and high acid concentration in the prior art is solved, and the acid concentration used is low, the by-products are few, and the reaction conditions are relatively mild, but the yield of methyl levulinate can reach 50mol%~ 67mol%

Method used

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  • Method for preparing methyl levulinate from cellulose under mild conditions of mechanical force chemocatalysis
  • Method for preparing methyl levulinate from cellulose under mild conditions of mechanical force chemocatalysis
  • Method for preparing methyl levulinate from cellulose under mild conditions of mechanical force chemocatalysis

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Experimental program
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Effect test

Embodiment 1

[0036](1) Disperse 30g of cellulose in 150ml of diethyl ether (3g of 98wt% sulfuric acid has been added to the diethyl ether) solvent, mix well and then stir with magnetic force for 30min (speed 300r / min), place the solvent diethyl ether in a fume hood at normal temperature and pressure to dry naturally (about 24h) to obtain sulfuric acid impregnated cellulose. The obtained sulfuric acid impregnated cellulose was ball milled with CJM-SY-B type high-energy nano-impact mill (tank volume is 2L) for 60min, and the ball milling medium (the ball milling medium was zirconia balls, the zirconia balls with diameters of 6mm, 8mm and 10mm) mixed use) the filling rate is 30%, and the temperature of the tank body during the ball milling process is below 30° C. to obtain ball-milled cellulose impregnated with sulfuric acid, wherein the mass fraction of sulfuric acid in the cellulose is 10%.

[0037] (2) Add 1.1g sulfuric acid impregnated ball-milled cellulose, 20g methyl alcohol, 0.1g sulfu...

Embodiment 2

[0039] (1) The specific steps are the same as the step (1) in Example 1.

[0040] (2) Add 1.1g sulfuric acid impregnated ball-milled cellulose, 20g methyl alcohol, 0.1g sulfuric acid in polytetrafluoroethylene tank, make sulfuric acid account for the mass concentration of methanol to be 1wt%, liquid-solid ratio (the mass ratio of methanol and cellulose) 20:1, add a stirrer, put it into the microwave reaction chamber after installation, first use the microwave instrument magnetic stirring system to pre-stir for 1min, set the heating program: 2min to 160°C, microwave power 800w; 160°C for 120min, microwave The power is 600w; the reaction process keeps stirring at a constant speed. After the reaction was completed, cool in an ice-water bath, lower the temperature to below 15°C, and then open the can to take out the entire reaction mixture. The reaction mixture was taken and analyzed by gas chromatography to calculate that the yield of methyl levulinate was 55.70 mol%.

Embodiment 3

[0042] (1) Concrete steps are identical with step (1) in embodiment 1;

[0043] (2) Add 1.1g sulfuric acid-impregnated ball-milled cellulose and 20g methyl alcohol in the polytetrafluoroethylene tank, so that the mass concentration of sulfuric acid in methanol is 0.5wt%, and the liquid-solid ratio (the mass ratio of methanol to cellulose) is 20: 1. Add a stirrer, put it into the microwave reaction chamber after installation, pre-stir with the magnetic stirring system of the microwave instrument for 1min, set the heating program: 2min to 170°C, microwave power 800w; 170°C for 120min, microwave power 600w; The reaction process was kept stirring at a constant speed. After the reaction was completed, cool in an ice-water bath, lower the temperature to below 15°C, and then open the can to take out the entire reaction mixture. The reaction mixture was taken and analyzed by gas chromatography to calculate that the yield of methyl levulinate was 49.61mol%.

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Abstract

The invention discloses a method for preparing methyl levulinate from cellulose under mild conditions of mechanical force chemocatalysis. The method comprises the steps of carrying out ball milling on sulfuric acid dipped cellulose, and enabling the cellulose to react with methanol, so as to obtain methyl levulinate. By utilizing a technique of combining the sulfuric acid dipped cellulose with ball milling, the depolymerization degree of the cellulose is increased, and the crystallinity degree of the cellulose is greatly decreased. Compared with cellulose which is not processed by the technique, the method has the advantage that the molar yield of methyl levulinate is greatly increased. The method has the advantages that a production process is simple, process conditions are easily controlled, the reaction temperature is low, the use amount of a catalyst is low, the requirements on high temperature resistance, high pressure resistance and corrosion resistance of reaction equipment are relatively low, and the synthetic yield is high. The technique has positive significances to the guidance of the development and utilization of biomass resources in China and the protection of ecological environments.

Description

technical field [0001] The invention relates to the field of mechanochemical catalysis and preparation of methyl levulinate, in particular to a method for preparing methyl levulinate from cellulose under mild conditions of mechanochemical catalysis. Background technique [0002] At present, the depletion of traditional non-renewable fossil energy sources such as coal, oil, and natural gas has attracted more and more attention. Energy is the foundation of my country's sustainable development strategy and one of the key factors to promote social progress and improve people's living standards. In this context, with the massive consumption of non-renewable resources, the conversion and utilization of renewable resources has become the focus of global attention. Biomass is the most potential renewable resource on earth, and its main components are cellulose, hemicellulose and lignin. Methyl levulinate, which is produced by the esterification reaction of cellulose and methanol u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/716C07C67/00
CPCC07C67/00C07C69/716
Inventor 肖卫华侯涛韩鲁佳赵婷婷刘欢张宇轩
Owner CHINA AGRI UNIV
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