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A kind of method that metal salt catalyzes cellulose to prepare levulinic acid ester

A technology of levulinate and cellulose, which is applied in the field of catalyzing the direct alcoholysis of cellulose to prepare levulinate, can solve the problems of low catalytic efficiency, corrosion of liquid inorganic acid, reduced reaction activity, etc., and achieves good reusability, The effect of mild reaction conditions and short reaction times

Active Publication Date: 2021-02-19
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, liquid inorganic acid has the disadvantages of corroding equipment and being difficult to recycle, which does not meet the development requirements of green chemistry.
The acidity of solid acid catalysts is often much worse than that of inorganic acids, and the catalytic efficiency is low.
In addition, the surface of the solid acid catalyst is easy to attach humus, which leads to a decrease in the reactivity, and the presence of water will have a greater impact on the catalyst activity.

Method used

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  • A kind of method that metal salt catalyzes cellulose to prepare levulinic acid ester
  • A kind of method that metal salt catalyzes cellulose to prepare levulinic acid ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 500mg microcrystalline cellulose (mass concentration in alcohol is 4.5%), 0.6mL water, 14mL methanol and 0.6mmol Al 2 (SO 4 ) 3 18H 2 O(Al 3+ 1.2 mmol) was added into a polytetrafluoroethylene reactor, and heated with 800W microwave power for 2 minutes to 180° C. under air atmosphere, and reacted for 4 minutes. The reaction product was analyzed by GC-MS and compared with the standard product of methyl levulinate to confirm that the main product was indeed methyl levulinate. Using naphthalene as an internal standard, the yield of methyl levulinate was 70.6% through quantitative analysis by gas chromatography.

Embodiment 2

[0028] Substantially the same as Example 1, the difference is: adopt 1.2mmol AlCl 3 Instead of 0.6mmolAl in Example 1 2 (SO 4 ) 3 18H 2 O, the detection result is that the yield of methyl levulinate obtained in the embodiment of the present invention is 8.2%.

Embodiment 3

[0030] Basically the same as Example 1, the difference is: adopt 1.2mmolAl (NO 3 ) 3 9H 2 O replaces 0.6mmol Al in Example 1 2 (SO 4 ) 3 18H 2 O, the detection result is that the yield of methyl levulinate obtained in the embodiment of the present invention is 12.6%.

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Abstract

The invention provides a method for directly preparing levulinate from cellulose, the main steps of which are: under the action of a metal salt catalyst, cellulose is subjected to alcoholysis in a mixed solvent of alcohol and water to directly obtain levulinic acid ester. The metal cation of the metal salt used in this method is Al 3+ , Sn 4+ or Fe 3+ At least one of them; the heating methods involved in the method include microwave heating and oil bath heating. The method provided by the invention can efficiently and selectively convert cellulose into levulinate, not only has mild reaction conditions, short reaction time, and easy recovery of the catalyst, but also avoids the use of liquid acid or solid acid catalysts, and has few side reactions. Low cost and friendly to the environment.

Description

technical field [0001] The invention relates to the field of organic compound synthesis, in particular to a method for preparing levulinate by catalyzing the direct alcoholysis of cellulose. Background technique [0002] Levulinate is a new type of biomass-based chemical product with high application prospects. It can be used as spices, solvents, plasticizers, oil additives and important chemical intermediates. Further transformation can also produce other downstream functions sex molecule. Its molecular structure contains two unsaturated groups, carbonyl and ester. The existence of these two active groups makes levulinic acid esters have higher reactivity, and reactions such as oxidation, reduction, addition, substitution, transesterification, and hydrolysis can occur. [0003] The direct alcoholysis of cellulose has the advantages of simple production process and easy control of process conditions, and is currently a research hotspot in the conversion and preparation of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/00C07C67/08C07C69/716
CPCC07C67/00C07C67/08C07C69/716
Inventor 黄耀兵杨涛潘晖
Owner NANJING FORESTRY UNIV
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