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Method for preparing gamma-valerolactone by levulinic acid ester without solvents

A technology of levulinic acid ester and valerolactone, applied in the direction of organic chemistry, etc., can solve the problem of high energy consumption, and achieve the effects of simplified separation and purification steps, excellent cycle performance, and efficient recovery

Inactive Publication Date: 2015-08-19
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in existing reports, the catalyst needs to be activated by hydrogenation pre-reduction before it is used in the catalytic hydrogenation reaction, and this step consumes a lot of energy.

Method used

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  • Method for preparing gamma-valerolactone by levulinic acid ester without solvents
  • Method for preparing gamma-valerolactone by levulinic acid ester without solvents

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 0.1 g of copper chromite without hydrogenation pretreatment to 20 g of ethyl levulinate raw material liquid as a catalyst, reduce in situ at 225 °C and 4 MPa hydrogen pressure and react for 4 h, then filter under reduced pressure to obtain colorless Clear liquid. After the ethanol was distilled off under reduced pressure, the crude product of γ-valerolactone was obtained with a yield of 57.5%.

Embodiment 2

[0023] Add 0.2 g of copper chromite without hydrogenation pretreatment to 20 g of butyl levulinate raw material liquid as a catalyst, reduce in situ at 250 °C and 2 MPa hydrogen pressure and react for 4 h, then filter under reduced pressure to obtain colorless Clear liquid. After the ethanol was distilled off under reduced pressure, the crude product of γ-valerolactone was obtained with a yield of 46.9%.

Embodiment 3

[0025] Add 0.2 g of copper chromite without hydrogenation pretreatment to 20 g of methyl levulinate raw material liquid as a catalyst, reduce in situ at 275 °C and 4 MPa hydrogen pressure and react for 4 h, then filter under reduced pressure to obtain colorless Clear liquid. After the ethanol was removed by distillation under reduced pressure, the crude product of gamma-valerolactone was obtained, and the productive rate was 85.6% (as figure 1 ).

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Abstract

The invention discloses a method for preparing gamma-valerolactone by levulinic acid ester without solvents, and relates to gamma-valerolactone. A copper chromite catalyst is added into the levulinic acid ester and reacts in hydrogen atmosphere to obtain solid-liquid mixture, pressure is reduced, suction filtration is performed to obtain binary liquid mixture containing gamma-valerolactone and corresponding alcohols, and the alcohols are recovered by distillation to obtain the gamma-valerolactone. Cheap and easily separated copper chromite serving as the catalyst is added into the levulinic acid ester from biomass, and the gamma-valerolactone is prepared at one step in a solvent-free system. The copper chromite catalyst is activated in situ in the system, so that a traditional catalyst pre-hydrogenation step is omitted. The method is simple and efficient, and an effective way is provided for large-scale preparation of biomass-based gamma-valerolactone.

Description

technical field [0001] The invention relates to gamma-valerolactone, in particular to a method for preparing gamma-valerolactone from levulinic acid ester without solvent. Background technique [0002] Levulinate esters such as methyl levulinate, ethyl levulinate, butyl levulinate, etc. are a class of platform compounds that can be prepared by degrading lignocellulose in alcohols. Using it as a raw material, a novel biomass-based platform compound γ-valerolactone can be prepared. Due to its high calorific value, good solubility and reactivity, this substance has received extensive attention and research in recent years. [0003] Chinese patent CN200810195942.4 discloses a method for preparing γ-valerolactone from levulinic acid, which includes using formic acid as a solvent and a hydrogen source to synthesize γ-valerolactone under the action of a ruthenium catalyst and a small amount of alkali. This method requires the introduction of formic acid and ruthenium catalysts, w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33
CPCC07D307/33
Inventor 曾宪海李铮蒋叶涛孙勇林鹿
Owner XIAMEN UNIV
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