Method for preparing gamma-valerolactone with high selectivity under mild condition

A high-selectivity, valerolactone-based technology, applied in organic chemistry and other fields, can solve problems such as expensive catalysts, long reaction time, and high energy consumption

Active Publication Date: 2015-05-27
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The technical problem to be solved in the present invention is to provide a method for preparing gamma-valerolactone by hydrogen transfer reaction in view of the disadvantages of environmental pollution, high energy consumption, expensive catalyst, and long reaction time in the existing technology for preparing gamma-valerolactone. ester method

Method used

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  • Method for preparing gamma-valerolactone with high selectivity under mild condition
  • Method for preparing gamma-valerolactone with high selectivity under mild condition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Use a dry round-bottomed flask with a branch tube under inert gas N 2 Add 10 mmol of ethyl levulinate and 20 ml of isopropanol under protection, and then add a self-made or commercially available 1 g Raney Ni catalyst (Raney Ni can be purchased from Aldrich and other reagent companies) under inert gas. All operations are performed under inert gas. N 2 Under a protective atmosphere, the flask was closed and reacted at room temperature for 9 hours, and the GVL product was obtained by gas chromatography detection, and a transparent and clear GVL liquid product was obtained by vacuum distillation, and the total yield was 99%.

Embodiment 2

[0065] Put 10 mmol of ethyl levulinate and 20 ml of isopropanol into a dry round-bottomed flask with a branch tube, and then add a homemade or commercially available 1 g Raney Ni catalyst (wet weight), all operations without inert gas protection. , reacted at room temperature for 9 hours, detected by gas chromatography, obtained GVL product, and obtained transparent and clear GVL liquid product through reduced pressure distillation, and the total yield was 70%.

Embodiment 3

[0067] Use a dry round-bottomed flask with a branch tube under inert gas N 2 Add 10 mmol of ethyl levulinate and 20 ml of isopropanol under protection, and then add a homemade or commercially available Raney Ni catalyst with a wet weight of 0.5 g under an inert gas. All operations are performed under an inert gas N 2 Under the protective atmosphere, the flask was closed and reacted at room temperature for 9 hours, and the GVL product was obtained by gas chromatography detection, and the transparent and clear GVL liquid product was obtained by vacuum distillation, and the total yield was 95%.

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Abstract

The invention relates to a method for preparing gamma-valerolactone with high selectivity under the mild condition. The method comprises the following steps of: under the conditions of optimal room temperature and inert gas, with secondary alcohol as a hydrogen source and active Raney nickel as a catalyst, carrying out hydrogen transfer reaction on a levulinic acid ester compound to obtain the gamma-valerolactone. The invention particularly relates to a method of preparing gamma-valerolactone by a lignocellulose derivative with high selectivity under the mild condition, which comprises the following steps of: carrying out alcoholysis reaction on the lignocellulose derivative such as fructose, 5-hydroxymethylfurfural or furfuryl alcohol by a solid acid catalyst in the presence of an alcohol solvent at certain temperature, filtering solid acid, collecting liquid, and obtaining levulinic acid esters through reduced pressure distillation; and with the secondary alcohol as the hydrogen source, catalyzing the obtained esters by Raney Ni as a non-noble metal catalyst at the room temperature to obtain the gamma-valerolactone with high yield.

Description

technical field [0001] The invention belongs to the field of organic matter preparation, and relates to a method for preparing γ-valerolactone with high selectivity under mild conditions, in particular to a method for preparing γ-valerolactone with high selectivity from lignocellulose derivatives through mild reaction conditions (GVL) method. Background technique [0002] Lignocellulose is the most abundant and widely distributed type of important organic compounds in nature, mainly composed of carbon, hydrogen and oxygen, and is a renewable carbon source. With the increasing depletion of oil resources and serious pollution problems, the need to find a renewable and clean energy source is becoming more and more urgent to replace conventional oil resources, so as to reduce the dependence of social development on oil. Compared with fossil energy, lignocellulose energy has the characteristics of wide distribution, large amount, non-polluting and renewable. Lignocellulosic res...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/33
Inventor 傅尧黄耀兵杨珍郭庆祥
Owner UNIV OF SCI & TECH OF CHINA
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