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

A high-selectivity, valerolactone technology, applied in organic chemistry and other directions, can solve problems such as high energy consumption, environmental pollution, and long reaction time

Active Publication Date: 2013-04-03
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 disadvan

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 an inert gas N 2 Add 10mmol ethyl levulinate and 20ml isopropanol under protection, then add homemade or commercially available wet weight 1g Raney Ni catalyst under inert gas (Raney Ni can be purchased from reagent companies such as Aldrich), all operations are 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 through gas chromatography detection, and a transparent and clear GVL liquid product was obtained through vacuum distillation, with a total yield of 99%.

Embodiment 2

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

Embodiment 3

[0067] Use a dry round-bottomed flask with a branch tube under an inert gas N 2 Add 10mmol ethyl levulinate and 20ml isopropanol under protection, then add homemade or commercially available catalyst with a wet weight of 0.5g Raney Ni under inert gas, all operations are 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 through gas chromatography detection, and a transparent and clear GVL liquid product was obtained through vacuum distillation, with a total yield of 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 highly selective preparation of γ-valerolactone under mild conditions, in particular to a method for highly selective preparation of γ-valerolactone from lignocellulose derivatives under mild reaction conditions (GVL) approach. Background technique [0002] Lignocellulose is an important organic compound that exists most in nature and is widely distributed. It is mainly composed of carbon, hydrogen and oxygen, and is a renewable carbon source. With the increasing depletion of petroleum resources and serious pollution problems, it is more and more urgent to find a renewable and clean energy source to replace conventional petroleum resources, so as to reduce the dependence of social development on petroleum. Compared with fossil energy, lignocellulosic energy has the characteristics of wide distribution, large amount, no pollution and renewable. Lignocellulosi...

Claims

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Application Information

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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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