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Method of one-step hydrogenation esterification between ketone and carboxylic acid in electrochemical hydrogen pump reactor

An electrochemical and reactor technology, applied in the field of electrochemical engineering, to achieve the effect of improving the uniformity of dispersion, increasing the reaction interface, increasing the reaction rate and conversion rate

Active Publication Date: 2018-10-19
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the one-step hydroesterification reaction reported in the literature still needs to be operated under high pressure conditions, and there is no report on the use of electrochemical hydrogen pump reactors for one-step hydroesterification of keto acids

Method used

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  • Method of one-step hydrogenation esterification between ketone and carboxylic acid in electrochemical hydrogen pump reactor
  • Method of one-step hydrogenation esterification between ketone and carboxylic acid in electrochemical hydrogen pump reactor
  • Method of one-step hydrogenation esterification between ketone and carboxylic acid in electrochemical hydrogen pump reactor

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Experimental program
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Effect test

Embodiment 1

[0026] In the electrochemical hydrogen pump reactor, the anode hydrogen is fed, and the feed amount is 20sccm; the cathode ethyl ketone and acetic acid mixture is fed, the feed liquid temperature is 40°C, the circulation flow rate is 10ml / min, and the pH value is 1.8, wherein The volume ratio of butanone to acetic acid is 1:1. When the electrochemical hydrogen pump reactor with a constant current of 18.9mA / cm 2 , After operating at 40°C for 3 hours, the reactor voltage was 0.47V, the reaction rate of hydrogenation of butanone to butanol was 117.6mmol / (cm s), and the current efficiency was 96.1%. Compared with only hydrogenation of butanone at the cathode, the conversion rate of butanone is increased by about 25%, and the hydrogenation rate and current efficiency are increased by about 30%. The conversion rate of butanol and acetic acid to generate sec-butyl acetate is 85.6%, which is about 1.09 times that when the alkyd esterification reaction is simply carried out at the cat...

Embodiment 2

[0028] In the electrochemical hydrogen pump reactor, the anode hydrogen is fed, and the feed amount is 10 sccm; the cathode butanone and acetic acid mixture is fed, the feed liquid temperature is 60 ° C, the circulation flow rate is 20 mL / min, and the pH value is 1.0, where The volume ratio of butanone to acetic acid is 1:1. When the electrochemical hydrogen pump reactor with a constant current of 18.9mA / cm 2 , After operating at 60°C for 3 hours, the reactor voltage was 0.55V, the reaction rate of hydrogenation of butanone to butanol was 82.9mmol / (cm s), and the current efficiency was 83.6%. Compared with only hydrogenation of butanone at the cathode, the conversion rate of butanone is increased by about 20%, and the hydrogenation rate and current efficiency are increased by about 30%. The conversion rate of butanol and acetic acid to generate sec-butyl acetate is 82.3%.

Embodiment 3

[0030]In the electrochemical hydrogen pump reactor, the anode hydrogen is fed, and the feed amount is 25 sccm; the cathode butanone and acetic acid mixture is fed, the temperature of the feed liquid is 40°C, the circulation flow rate is 30mL / min, and the pH value is 3.0, where The volume ratio of butanone to acetic acid is 1:1. When the electrochemical hydrogen pump reactor with a constant current of 18.9mA / cm 2 , After running at 40°C for 10 hours, the reactor voltage is 0.66V, the reaction rate of hydrogenation of butanone to butanol is 51.3mmol / (cm s), the current efficiency is 52.4%, and the reaction rate of butanol and acetic acid to generate sec-butyl acetate The conversion rate was 75.0%.

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Abstract

The invention belongs to the technical field of electrochemical engineering, and relates to a method of one-step hydrogenation esterification between ketone and carboxylic acid in an electrochemical hydrogen pump reactor. In an electrochemical hydrogen pump reactor, when electrical power is applied, an electrochemical window with extremely low hydrogen is utilized to dissociate hydrogen in the anode, then hydrogen is delivered to the catalysis layer of the cathode to generate in-situ adsorption hydrogen, in-situ adsorption hydrogen and ketone in the cathode circulation liquid carry out hydrogenation reactions directly, the generated alcohols further carry out esterification reactions with carboxylic acids in the cathode circulation liquid; hydrogenation and esterification are carried out in one reactor under a normal pressure, and a synergistic effect is generated.

Description

technical field [0001] The invention belongs to the technical field of electrochemical engineering, and relates to a method for one-step hydrogenation esterification of ketone and carboxylic acid in an electrochemical hydrogen pump reactor. Background technique [0002] Energy is the material basis of human activities and restricts social and economic development. Bio-oil is called "green oil", which originates from plant photosynthesis, has abundant reserves, is environmentally friendly, is compatible with infrastructure, and can also be used as a raw material for many chemicals, so it has received more and more attention. Bio-oil is a complex oxygen-containing mixture composed of alcohols, ethers, aldehydes, ketones, acids and their derivatives. It needs hydrogenation to remove its unsaturated components and esterification to remove organic carboxylic acids, thereby improving the stability and combustion of oil products. performance and reduce its corrosiveness. Hydrogen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/00C07C69/14
CPCC07C69/14C25B3/00
Inventor 吴雪梅贺高红宋雪黄诗琪肖武阮雪华郑文姬范姝艾王云晴孙嵩岚于喆淼
Owner DALIAN UNIV OF TECH
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