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Method for synthesizing oxalate by CO gas-phase coupling

An oxalate ester and gas phase technology, applied in the field of regeneration technology, can solve the problems of difficult gas separation and purification, discharge pollution of nitric acid-containing wastewater, and low yield of nitrite, achieving high utilization rate, reduced investment, and short process Effect

Active Publication Date: 2013-03-13
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Abstract
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Problems solved by technology

[0027] The purpose of the present invention is to provide a kind of method for the synthesis of oxalate by CO gas-phase coupling in view of the demand for the regeneration process in the production process of CO gas-phase coupling synthesis of oxalate above, this method mainly solves the problem in the regeneration reaction in the prior art. The low yield of nitrite caused by the generation of nitric acid and the pollution of wastewater containing nitric acid discharge solve the problem of high cost and gas separation and purification when supplementing NO gas through ammonia oxidation method, nitrite oxidation method, nitric acid tail gas, etc. in the previous technology It has the advantages of high nitrogen oxide utilization rate, simple process, low energy consumption, and no pollution.

Method used

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  • Method for synthesizing oxalate by CO gas-phase coupling

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Effect test

Embodiment 1

[0056] With CO and ethyl nitrite as raw materials, N 2 As a dilution gas, the raw material first enters the coupling reactor I, reacts under the action of the Pd catalyst, and generates effluent A containing diethyl oxalate, NO, unreacted ethyl nitrite and unreacted CO, and effluent A After gas-liquid separation in the condenser, the gas phase effluent B containing NO, ethyl nitrite and CO and the liquid phase effluent C containing diethyl oxalate are obtained respectively. The gas phase effluent B is divided into two streams, namely gas phase effluent D and gas phase effluent E, gas phase effluent D reacts with 68% nitric acid solution in reactor II, and the reaction temperature is 30 o C, the reaction pressure is normal pressure, and the residence time of the gas phase effluent D during the reaction is 1 second. NO 2 The tail gas F and the still liquid G containing nitric acid are mixed, and the tail gas F is mixed with the gas phase effluent E to obtain the gas phase effl...

Embodiment 2

[0059] Using CO and methyl nitrite as raw materials, N 2 As a dilution gas, the raw material first enters the coupling reactor I, reacts under the action of the Pd catalyst, and generates effluent A containing dimethyl oxalate, NO, unreacted methyl nitrite, and unreacted CO, and effluent A After gas-liquid separation in the condenser, the gas phase effluent B containing NO, methyl nitrite and CO and the liquid phase effluent C containing dimethyl oxalate are obtained respectively. The gas phase effluent B is divided into two streams, namely gas phase effluent D and gas phase effluent E, gas phase effluent D is reacted with 30% nitric acid solution in reactor II, and the reaction temperature is 90 o C, the reaction pressure is normal pressure, and the residence time of the gas phase effluent D during the reaction is 50 seconds. NO 2 The tail gas F and the still liquid G containing nitric acid are mixed, and the tail gas F is mixed with the gas phase effluent E to obtain the g...

Embodiment 3

[0062] With CO and isopropyl nitrite as raw materials, N 2 As a dilution gas, the raw material first enters the coupling reactor I, and reacts under the action of the Pd catalyst to generate effluent A containing diisopropyl oxalate, NO, unreacted isopropyl nitrite, and unreacted CO, and flows out After the product A is separated from the gas and liquid by the condenser, the gas phase effluent B containing NO, isopropyl nitrite and CO and the liquid phase effluent C containing diisopropyl oxalate are respectively obtained. Divide gaseous phase effluent B into two streams, namely gaseous phase effluent D and gaseous phase effluent E, gaseous phase effluent D reacts with 55% nitric acid solution in reactor II, the reaction temperature is 65 o C, the reaction pressure is normal pressure, and the residence time of the gas phase effluent D during the reaction is 30 seconds. NO 2 The tail gas F and the still liquid G containing nitric acid are mixed, and the tail gas F is mixed wi...

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Abstract

The invention discloses a method for synthesizing oxalate by CO gas-phase coupling. The regeneration technique in the invention is used for solving the problem that extra NO gas needs to be supplemented due to nitrogen loss caused by nitric acid generated in regeneration reaction. In the invention, NO and nitric acid react to provide NO2 gas to supplement nitrogen loss due to nitric acid generated by the regeneration reaction. The method can recycle the nitric acid generated in the regeneration reaction, so that the utilization ratio of NO is kept at 98% above; and meanwhile, the invention solves the problem of pollution of discharge of nitric-acid-containing wastewater generated by the regeneration reaction.

Description

technical field [0001] The present invention relates to a method for CO gas-phase coupling synthesis of oxalate, in particular to the regeneration process in the production process of CO gas-phase coupling synthesis of oxalate, which is used to solve the loss of nitrogen caused by the generation of nitric acid in the regeneration reaction and requires additional The problem of supplementing NO gas. Background technique [0002] As a degradable and environmentally friendly engineering plastic monomer, oxalate has attracted more and more international attention, and it is also an important organic chemical raw material, widely used in the production of various dyes, medicines, important solvents, extractants and other fields. In addition, with the depletion of petroleum resources, the non-petroleum route of synthesizing ethylene glycol from oxalate esters using syngas as raw material is becoming more and more popular. my country is a big consumer of ethylene glycol. In 2010, ...

Claims

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Application Information

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IPC IPC(8): C07C69/36C07C67/36
Inventor 王科李扬胡玉容范鑫袁小金许红云胡文励谢光全
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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