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Method for preparing dimethyl oxalate from syngas and by-product dimethyl carbonate

A technology of dimethyl oxalate and dimethyl carbonate, applied in the purification/separation of carbonate/haloformate, preparation of organic compounds, preparation of carboxylate, etc., can solve the problem of high energy consumption and product loss high, short operating cycle and other problems, to achieve the effect of reducing operating energy consumption, reducing energy consumption, and avoiding coking

Active Publication Date: 2019-01-11
SINOPEC SHANGHAI ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0024] The technical problem to be solved by the present invention is the problem of high energy consumption, short operation period and high product loss in the prior art, and a new synthesis gas is provided to prepare dimethyl oxalate and by-product dimethyl carbonate method

Method used

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  • Method for preparing dimethyl oxalate from syngas and by-product dimethyl carbonate
  • Method for preparing dimethyl oxalate from syngas and by-product dimethyl carbonate
  • Method for preparing dimethyl oxalate from syngas and by-product dimethyl carbonate

Examples

Experimental program
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Effect test

Embodiment 1

[0039] A kind of synthesis gas prepares the method for dimethyl oxalate and by-product dimethyl carbonate, such as figure 1 Shown, methanol (01), the fresh methyl nitrite (02) and oxygen (03) that need to be replenished due to the consumption loss due to side reactions, and the oxalate recovery tower (105) overhead flow containing nitrogen monoxide and other light The circulating return gas (09) of the components is sent to the corresponding positions of the oxidative esterification reaction rectification tower (101) respectively, and the oxidative esterification reaction takes place in the oxidative esterification reaction rectification tower (101) to obtain methyl nitrite and other components. Methyl nitrite and other light components (04) are separated and flowed from the top of the oxidative esterification reaction rectification tower (101), and enter the coupling reactor (104) together with carbon monoxide (05). , Carry out gas-phase catalytic coupling reaction to genera...

Embodiment 2

[0046] According to the conditions and steps described in Example 1, only the production scale was changed to a 20,000-ton / year syngas to prepare ethylene glycol industrial production device, and the inner diameter of the reaction tube of the coupling reactor 104 was changed to 25 mm. Using the technical method of the present invention to prepare dimethyl oxalate and by-product dimethyl carbonate, no coking phenomenon occurs in the industrial production device during normal full-load operation for one year; at the same time, the nitrogen monoxide cycle return gas does not contain carbonic acid Dimethyl ester reduces the flow rate of circulating return air, and reduces the energy consumption of operation by 7.72%; moreover, dimethyl carbonate does not undergo hydrolysis reaction, the equipment does not corrode, and the service life reaches 20 years; finally, dimethyl oxalate product and dicarbonate There is also no loss of methyl ester by-product.

Embodiment 3

[0048] According to the conditions and steps described in Example 1, only the production scale was changed to 200,000 tons / year synthesis gas to prepare ethylene glycol industrial production equipment, and the inner diameter of the reaction tube of the coupling reactor 104 was changed to 32 mm. Using the technical method of the present invention to prepare dimethyl oxalate and by-product dimethyl carbonate, no coking phenomenon occurs in the industrial production device during normal full-load operation for one year; at the same time, the nitrogen monoxide cycle return gas does not contain carbonic acid Dimethyl ester reduces the flow rate of circulating return air, and reduces the energy consumption of operation by 8.36%; moreover, dimethyl carbonate does not undergo hydrolysis reaction, the equipment does not corrode, and the service life reaches 20 years; finally, dimethyl oxalate product and dicarbonate There is also no loss of methyl ester by-product.

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Abstract

The invention relates to a method for preparing dimethyl oxalate and producing dimethyl carbonate as a by-product from a synthetic gas. The problems that the energy consumption is higher, the operational cycle is shorter and the amount of loss of a product is higher in the prior art are mainly solved. Through adopting the method for preparing the dimethyl oxalate and producing the dimethyl carbonate as the by-product from the synthetic gas, a material in coupling reaction of the synthetic gas is sent into an oxalate recovery tower; the dimethyl carbonate is not contained at a tower top to reduce a gas return amount; a material in a tower kettle is sent into an oxalate product tower; at lower operational temperature, the dimethyl oxalate is obtained in the tower kettle. By using the technical scheme, the problems are solved better; the method for preparing the dimethyl oxalate and producing the dimethyl carbonate as the by-product from the synthetic gas can be used in the preparation of the dimethyl oxalate from the synthetic gas.

Description

technical field [0001] The invention relates to a method for preparing dimethyl oxalate from synthesis gas and producing dimethyl carbonate by-product. Background technique [0002] Dimethyl oxalate (COOCH 3 ) 2 It is an important chemical raw material, which can generate ethylene glycol through hydrogenation reduction reaction. The traditional synthetic method of dimethyl oxalate is obtained by esterification reaction of oxalic acid and methanol. However, this method has problems such as large energy consumption, serious pollution and low utilization rate of raw materials. Therefore, nowadays, dimethyl oxalate is prepared by a two-step method of oxidative esterification of synthesis gas and coupling reaction. First with methanol CH 3 OH and oxygen O 2 As a raw material, the nitrogen monoxide NO returned by the cycle and the fresh methyl nitrite CH that needs to be replenished due to the consumption loss due to side reactions 3 ONO together undergoes an oxidative ester...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/36C07C67/54C07C69/36C07C68/00C07C68/08C07C69/96
CPCC07C67/36C07C67/54C07C68/00C07C68/08C07C69/36C07C69/96
Inventor 王江义何琨沙鑫佚胡亚敏钟亮李真泽张斌李勇
Owner SINOPEC SHANGHAI ENG