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Method for preparing diethyl oxalate by coupling CO

A technology of diethyl oxalate and ethyl nitrite, applied in chemical instruments and methods, carbon monoxide or formate reaction preparation, metal/metal oxide/metal hydroxide catalyst, etc., to achieve high efficiency and good industrialization prospects Effect

Active Publication Date: 2008-03-19
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But, the deficiency of this invention is, has just completed small-scale research, for large-scale production with industrial production as the background, its production method also needs further improvement

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  • Method for preparing diethyl oxalate by coupling CO
  • Method for preparing diethyl oxalate by coupling CO

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Experimental program
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Effect test

Embodiment 1

[0035] The CO gas produced by the industrial gas generator is purified and treated to obtain the CO raw material gas composition (volume %) required by the process: CO 96% to 98%, and a small amount of impurities should meet the process requirements. 2 ≤100ppm, S≤1ppm, H 2 O≤100ppm, H 2 ≤100ppm, the rest is N 2 gas. The CO purified feed gas enters the reaction system with an operating pressure (gauge pressure) of 0.12MPa-0.2MPa (see Figure 1 for the device). The flow rate of CO raw material gas is 170L / h and the ethyl nitrite cycle gas from the cycle gas storage tank 7 enters the preheater 1 for mixing and preheating (60°C-70°C), and then enters the coupling reactor 2 after preheating. The coupling reactor is a fixed-bed tubular reactor, 3 meters long, a stainless steel jacketed reactor with a diameter of Φ32×2.5 mm, and 1 kg of Pd-Fe / Al is placed in the tube 2 o 3 For bimetallic supported catalysts, the temperature of the reaction bed is adjusted by circulating hot oil i...

Embodiment 2

[0041] The CO gas produced by the industrial gas generator is purified by water washing, alkali washing, desulfurization, deoxidation, and drying. 2 ≤100ppm, S≤lppm, H 2 O≤100ppm, H 2 ≤100ppm, the rest is N 2 gas. The CO cleans the feed gas to 16M 3 The feed flow rate of / h enters the reaction system (see Figure 1 for the device). The process operating pressure (gauge pressure) is 0.16MPa~0.2MPa. The feed gas is mixed with the ethyl nitrite recycle gas obtained from the regeneration reaction in the recycle gas storage tank 7 in a ratio of 8 to 10:1 (the recycle ratio is the ratio of the feed volume of the recycle gas to the feed gas) ratio) into the preheater 1 together, and the mixed gas enters the coupling reactor 2 after preheating. The coupling reactor is a fixed bed tubular reactor, and there are 96 tubes in total, each tube is 3 meters long and has a diameter of Φ32×2.5mm stainless steel tubes, 1.25kg of catalyst is placed in each tube, and the reactor is filled wit...

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Abstract

The invention discloses a method for preparing diethyl oxalate by CO coupling reaction. By applying a gas phase method, CO is coordinated with ethyl nitrite and is catalyzed by bimetallic supported catalyzer to couplingly generate crude diethyl oxalate, the reaction is a self-sealing circulation process, the CO gas mixed with the ethyl nitrite coming from a regeneration reactor is preheated and then enters into a coupling reactor, after the reaction, the gas is separated by condensation, so that the colorless and transparent condensed diethyl oxalate liquid is produced, and the uncondensed gas containing NO enters into the regeneration reactor to react with ethanol and oxygen in order to generate ethyl nitrite which is again circulated back to the coupling reactor for continuous use. The invention is carried out on the basis of previous laboratory research and under the background of industrial production and fulfils the continuous run examination of the bench scale test and pilot magnification under the condition of industrial operation, the temperature of the coupling reaction is low, and the concentration of products is increased. The method has the advantages of more energy saving, no pollution and high benefit. The total conversion rate of the CO generated by reaction is one hundred percent, and the selectivity of diethyl oxalate is over ninety six percent.

Description

technical field [0001] The invention belongs to the application of one-carbon chemical technology in organic chemical industry, in particular to a method for preparing diethyl oxalate with CO. Background technique [0002] The production of diethyl oxalate by CO gas-phase coupling catalysis is currently the focus of international "C1 chemical industry" new process research, and it is also one of the research topics for the sustainable development of non-petroleum routes that are key projects in my country's "Eleventh Five-Year Plan" , CO raw materials have a wide range of sources and are cheap. They can be produced from coal or natural gas, and CO or CO2 in industrial waste gas can also be used as raw materials. If we make full use of my country's rich coal and natural gas resources, it is the most economical to use CO to produce oxides. A reasonable route can open up a new way for the comprehensive utilization of energy and the development of new technologies in our country. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/36C07C67/36B01J23/89
Inventor 许根慧马新宾王保伟李振花张毅民
Owner TIANJIN UNIV
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