Method for preparing levulinic acid and co-producing gamma-valerolactone from biomass

A technology of levulinic acid and biomass, which is applied in the preparation of organic compounds, carboxylate preparation, chemical instruments and methods, etc., can solve the problems of solid acid catalyst deactivation, acid site loss, increased cost, etc., to improve the reaction Efficiency and product yield, increased contact area, and the effect of avoiding waste acid discharge

Inactive Publication Date: 2013-12-11
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The two-step method increases the cost of the whole process and limits the development of the process, and the presence of a large amount of water will cause the acid site of the solid acid to be lost, resulting in the deactivation of the solid acid catalyst

Method used

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  • Method for preparing levulinic acid and co-producing gamma-valerolactone from biomass
  • Method for preparing levulinic acid and co-producing gamma-valerolactone from biomass

Examples

Experimental program
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Effect test

Embodiment 1

[0030] This example is a process for preparing levulinic acid. Corn stalks are mixed with an aqueous solution with a content of 90% γ-valerolactone. The mixing ratio is 1:20 according to the weight ratio of corn stalks to γ-valerolactone. Dissolving, after the dissolution is completed, the obtained mixture is filtered, and a molecular sieve solid acid catalyst is added to the filtrate. The weight ratio of the molecular sieve solid acid catalyst to the filtrate is 1:20, and the catalytic reaction is carried out at 160 ° C. After the reaction, the obtained mixture Filtration is carried out, and the filtered molecular sieve solid acid catalyst is reused, and the filtrate is distilled to separate levulinic acid, water and γ-valerolactone. The process utilizes γ-valerolactone to dissolve corn stalks and then catalyzes the preparation of levulinic acid with a solid acid catalyst. The catalytic efficiency is high, and the yield of levulinic acid is greatly improved compared with the w...

Embodiment 2

[0032] This example is the preparation process of levulinic acid. Corncobs are mixed with an aqueous solution with a γ-valerolactone content of 95%. The mixing ratio is 1:5 according to the weight ratio of corncobs and γ-valerolactone. Dissolve, after the dissolution is completed, filter the obtained mixture, add an ion exchange resin solid acid catalyst to the filtrate, the weight ratio of the ion exchange resin solid acid catalyst to the filtrate is 1:4, carry out the catalytic reaction at 260 ° C, and the reaction ends The obtained mixture is filtered, and the filtered ion exchange resin solid acid catalyst is reused, and the filtrate is distilled to separate levulinic acid, water and gamma-valerolactone solution. In this process, the yield of levulinic acid is not less than 40%.

Embodiment 3

[0034] This example is the preparation process of levulinic acid, mixing wood chips with an aqueous solution with a content of 98% of γ-valerolactone, the mixing ratio is 1:200 by weight ratio of wood chips and γ-valerolactone, and dissolving at 100°C After the dissolution is completed, the obtained mixture is filtered, and a heteropolyacid solid acid catalyst is added to the filtrate. The weight ratio of the heteropolyacid solid acid catalyst to the filtrate is 1:100, and the catalytic reaction is carried out at 100 ° C. After the reaction, the obtained The mixture is filtered, and the filtered heteropolyacid solid acid catalyst is reused, and the filtrate is separated from levulinic acid, water and gamma-valerolactone solution by distillation. In this process, the yield of levulinic acid is not less than 50%. The filter residue in the reaction process can be used as fuel after being dried.

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Abstract

The present invention provides a method for preparing levulinic acid and co-producing gamma-valerolactone from biomass. The method comprises: mixing biomass and a gamma-valerolactone aqueous solution according to a weight ratio of the biomass to the gamma-valerolactone of 1:5-1:200, and dissolving the biomass under a heating condition; adding a solid acid catalyst to the filtrate to prepare levulinic acid; and adding a Ru, Ni or Pt base catalyst to prepare gamma-valerolactone. According to the present invention, after cellulose and hemicellulose in the biomass are dissolved in the gamma-valerolactone, the contact area with the solid acid is substantially increased so as to improve reaction efficiency and a product yield; the solid acid can be reused after recycling, such that waste acid emission can be avoided, cost can be reduced, and pollution on the environment can not be caused; the final product is the gamma-valerolactone so as to avoid separation of the product and the solvent; and difficult problems of low product yield, easy catalyst deactivation and low product separation cost due to existing of a large amounts of water during a levulinic acid and gamma-valerolactone preparation process using biomass in the prior art are solved.

Description

technical field [0001] The invention relates to a method for preparing levulinic acid or co-producing gamma-valerolactone from biomass, and belongs to the field of solid waste treatment and resource utilization. Background technique [0002] Levulinic acid and its derivative γ-valerolactone are important biomass-based platform compounds. At present, liquid acid is usually used as a catalyst in the process of preparing levulinic acid and γ-valerolactone from lignocellulose. In the water phase, there are problems of low product yield and high cost of separation of catalyst and product. The use of solid acid solves the problem of catalyst recovery. However, in the aqueous phase, since both lignocellulose and solid acid are solid, it is difficult to achieve uniform contact between the two, resulting in a greatly reduced reaction efficiency. In order to solve this problem, someone divided the reaction process into two steps. The first step is to convert cellulose into glucose th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33C07C59/185C07C51/00
Inventor 吕学斌张书廷
Owner TIANJIN UNIV
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