Method for preparing levulinic acid by catalyzing microcrystalline cellulose with heteropolyacid

A technology of microcrystalline cellulose and levulinic acid is applied in the preparation of carboxylates, chemical instruments and methods, preparation of organic compounds, etc., which can solve the problems of environmental pollution and high reaction energy consumption, achieve low environmental pollution damage and obtain high efficiency. High rate, mild response effect

Inactive Publication Date: 2019-11-22
TIANJIN UNIV OF SCI & TECH
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  • Summary
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AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems of environmental pollution and high reaction energy consumption, the invention provides a method for preparing levulinic acid from microcrystalline cellulose catalyzed by heteropolyacids. The purpose is to make full use of agricultural and forestry straw microcrystalline cellulose biomass resources and reduce energy consumption, reduce pollution, increase productivity and save costs, and increase economic, ecological and social benefits

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) adding corn stalk microcrystalline cellulose and loaded titanium dioxide-zirconia composite metal oxide phosphomolybdic acid into the reaction kettle according to the mass ratio of 1:1;

[0021] (2) Add 25 times of corn stalk microcrystalline cellulose γ-valerolactone-water mixed solution in the reactor, wherein the volume ratio of γ-valerolactone and water is 1: 10, and then the reactor containing the reactant React at 150°C for 4 hours under stirring at 300 rpm;

[0022] (3) After the reaction, cool to 20° C., and separate the solid and liquid by high-speed centrifugation. After separation, the solution is purified by vacuum distillation, and the yield of levulinic acid product is 62%.

Embodiment 2

[0024] (1) adding wheat straw microcrystalline cellulose and loaded titanium dioxide-zirconia composite metal oxide phosphomolybdic acid into the reaction kettle according to the mass ratio of 2:1;

[0025] (2) Add 15 times of corn stalk microcrystalline cellulose γ-valerolactone-water mixed solution in the reactor, wherein the volume ratio of γ-valerolactone and water is 5: 1, and then the reactor containing the reactant React at 180°C for 2 hours under stirring at 400 rpm;

[0026] (3) After the reaction, cool to 20° C., and separate the solid and liquid by high-speed centrifugation. After separation, the solution is purified by vacuum distillation, and the yield of levulinic acid product is 72%.

Embodiment 3

[0028] (1) adding rice straw microcrystalline cellulose and loaded titanium dioxide-zirconia composite metal oxide phosphomolybdic acid into the reaction kettle according to the mass ratio of 5:1;

[0029] (2) Add 50 times of corn stalk microcrystalline cellulose gamma-valerolactone-water mixed solution in the reactor, wherein the volume ratio of gamma-valerolactone and water is 10:1, then the reactor filled with reactant React at 175°C for 4 hours under stirring at 400 rpm;

[0030] (3) After the reaction was completed, it was cooled to 20° C., and the solid and liquid were separated by vacuum filtration. After separation, the solution was purified by vacuum distillation, and the yield of levulinic acid product was 67%.

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Abstract

The invention discloses a method for preparing levulinic acid by catalyzing microcrystalline cellulose with heteropolyacid, and belongs to the field of biomass chemical industry. According to the method, microcrystalline cellulose is used as a raw material, a gamma-valerolactone-water mixed solution is used as a reaction medium, and the heteropolyacid is used for a catalytic reaction; after solid-liquid separation and purification, the product levulinic acid is obtained. The method is wide in raw material source, low in price, high in catalyst activity, stable in property, mild in whole reaction process, simple in reaction process flow, easy to implement, high in product yield and wide in industrialized application prospect.

Description

technical field [0001] The invention belongs to the field of biomass chemical industry, and relates to a method for preparing levulinic acid from microcrystalline cellulose catalyzed by heteropolyacids. Background technique [0002] Levulinic acid is an important platform compound, which has the properties of carboxylic acid and ketone, so it has good chemical reactivity, and can perform chlorination, esterification, hydrogenation, substitution, polymerization, redox and other reactions, and is widely used It is used in the synthesis of compounds such as resins, pharmaceuticals, rubber and plastic additives, fuel additives, herbicides, fragrances, surfactants, and new polymers. At present, the main process for the production of levulinic acid is the direct hydrolysis of biomass. The principle of this method is to use biomass as raw material. Methylfurfural continues to decarboxylate to levulinic acid. The method has the advantages of wide sources of raw materials and low p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/00C07C59/185
CPCC07C51/00C07C59/185
Inventor 梁敏司传领李晓云吕乐福李光壁张晨阳蒋利杰李颖
Owner TIANJIN UNIV OF SCI & TECH
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