Process and production system for synthesizing dimethyl oxalate or diethyl oxalate and coproducing oxalic acid

A technology for synthesizing dimethyl oxalate and diethyl oxalate, which is applied in the preparation of carboxylate/lactone, the reaction preparation of carbon monoxide or formate, and organic chemistry, etc., can solve equipment corrosion, high energy consumption, and increased separation cost and other problems, to achieve the effect of large driving force, thorough absorption and reduction of separation cost

Active Publication Date: 2011-04-06
SHANGHAI HUAYI ENERGY CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The purpose of the present invention is to overcome the high energy consumption and separation cost in the process of preparing methyl oxalate or ethyl oxalate by using CO as a raw material through methyl nitrite or ethyl nitrite, and the circulation system of CO oxidation coup...

Method used

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  • Process and production system for synthesizing dimethyl oxalate or diethyl oxalate and coproducing oxalic acid
  • Process and production system for synthesizing dimethyl oxalate or diethyl oxalate and coproducing oxalic acid
  • Process and production system for synthesizing dimethyl oxalate or diethyl oxalate and coproducing oxalic acid

Examples

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Embodiment 1

[0060] This embodiment is a process for the co-production of oxalic acid from dimethyl oxalate, and the pressure of all equipment is 0.1 MPa. The reaction temperature of equipment A gas-phase coupled carbonylation reactor is 140°C, and the catalyst is Pd / a-Al 2 o 3 , the process temperature of the equipment B condenser is 20°C, the equipment C oxalate ester hydrolysis reactor is designed as a reactive distillation column in this example, the temperature of the reaction zone is 85°C, the temperature of the condenser at the top of the oxalate ester hydrolysis reactor -5°C, the esterification reactor of equipment D is also designed as a reactive distillation column, and the temperature in the reaction zone is 40°C. The following table is the present embodiment according to the instructions attached figure 1 The composition of each pipeline material, attached figure 1 Pipeline No. 13 is the relaxation point. According to the technical requirements of the circulation system, the...

Embodiment 2

[0065] This example is a flow process for the co-production of oxalic acid from dimethyl oxalate, and the pressure of all equipment is 0.1 MPa. The reaction temperature of equipment A gas-phase coupled carbonylation reactor is 140°C, and the catalyst is Pd / a-Al 2 o 3 , the process temperature of the equipment B condenser is 40°C, the equipment C oxalate ester hydrolysis reactor is designed as a reactive distillation column in this embodiment, the temperature of the reaction zone is 85°C, the condenser at the top of the oxalate ester hydrolysis reactor The temperature is -5°C, and the esterification reactor of equipment D is also designed as a reactive distillation column, and the temperature in the reaction zone is 40°C. The following table is the example attached according to the manual figure 1 The composition of each pipeline material. attached figure 1 Pipeline No. 13 is the relaxation point. According to the technical requirements of the circulation system, the circul...

Embodiment 3

[0070]Except that the reaction zone temperatures of the equipment C oxalate ester hydrolysis reactor were respectively 25° C. and 98° C., the rest were the same as in Example 1. As a result, the output of dimethyl oxalate and oxalic acid is close to that of Example 1, indicating that the temperature of the hydrolysis reactor has little influence on the production capacity.

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Abstract

The invention discloses a process and a production system for synthesizing dimethyl oxalate or diethyl oxalate and coproducing oxalic acid. The method comprises the following steps of: reacting nitrogen oxide with alcohol in an esterification reactor to form nitrite, adding the nitrite into a gas phase coupling carbonylation reactor, and connecting the gas phase coupling carbonylation reactor with a condenser and an oxalate hydrolysis reactor. After being condensed by the condenser, outlet gas of the gas phase coupling carbonylation reactor is condensed into liquid-phase or solid-phase oxalate; the oxalate in the gas phase enters the oxalate hydrolysis reactor to generate the oxalic acid and the alcohol of corresponding ester; the ester solution of the corresponding ester can enter the subsequent esterification reactor for reaction; and the amount of the oxalate which enters the gas phase can be adjusted by adjusting the temperature of the condenser so as to adjust the distribution of the synthetic amount of the oxalate and the oxalic acid. Nitrogen oxide-containing noncondensable gas which passes through the oxalate hydrolysis reactor is recycled to enter the esterification reactor so as to realize the recycling of the nitrogen oxide. The process and the production system for synthesizing the dimethyl oxalate or the diethyl oxalate and coproducing the oxalic acid have low energy consumption and high productivity and meet the industrial requirement.

Description

technical field [0001] The invention relates to a process for synthesizing dimethyl oxalate or diethyl oxalate and co-producing oxalic acid, more specifically, to a process for synthesizing dimethyl oxalate or diethyl oxalate and co-producing carbon monoxide and oxygen through nitrite esters Oxalic acid process. Background technique [0002] Oxalic acid, dimethyl oxalate and diethyl oxalate are all important organic chemical raw materials. Oxalic acid is widely used in the fields of chemical synthesis, pharmaceuticals, extraction and refining of rare earth elements, metal treatment and cleaning, and polymer synthesis, while dimethyl oxalate The low-pressure hydrogenation of esters and diethyl oxalate can produce ethylene glycol, an important chemical raw material, which has attracted widespread attention in the chemical industry. [0003] The traditional oxalic acid production methods are sodium formate method, ethylene glycol oxidation method, carbohydrate oxidation method...

Claims

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Application Information

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IPC IPC(8): C07C69/36C07C67/36C07C55/06C07C51/09
Inventor 单文波鲁文质黄斌徐长青黄飚
Owner SHANGHAI HUAYI ENERGY CHEM
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