Dimethyl oxalate production method with byproduct (dimethyl carbonate)

A technology of dimethyl oxalate and dimethyl carbonate, applied in the purification/separation of carbonate/haloformate, preparation of carbonate/haloformate, separation/purification of carboxylate, etc., capable of Solve the problems of complicated separation process of methanol and dimethyl carbonate, large amount of methanol consumption, complicated process, etc., and achieve the effects of saving equipment investment and floor area, reducing steam consumption, and simplifying equipment

Active Publication Date: 2017-03-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem of complex process and high energy consumption in the separation process of methanol and dimethyl carbonate has not been solved
[0016] In short, in the existing technology, for the separation method of dimethyl carbonate, whether it is pressu

Method used

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  • Dimethyl oxalate production method with byproduct (dimethyl carbonate)
  • Dimethyl oxalate production method with byproduct (dimethyl carbonate)
  • Dimethyl oxalate production method with byproduct (dimethyl carbonate)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] The gas phase raw material containing CO and methyl nitrite enters the coupling reactor 21 through the pipeline 25, and the output of the coupling reactor enters between the extraction section 22b and the stripping section 22c of the ester separation tower 22 through the pipeline 26, and is connected with the pipeline 33 The dimethyl oxalate absorbing liquid that enters the ester separation tower extraction section 22b top and flows down is countercurrently contacted, and the absorption liquid obtained at the bottom of the extraction section 22b of the ester separation tower flows to the ester separation tower stripping section 22c, and passes through the stripping section 22c After the stripping, the mixture of dimethyl oxalate and dimethyl carbonate obtained by separating from the bottom of the stripping section 22c of the ester separation tower enters the refining tower 23 through a pipeline 29 . The gas phase stream obtained at the top of the extraction section 22b a...

Embodiment 2

[0062] It is the same as [Example 1], except that the equipment parameters and operating conditions of the tower are different.

[0063]The reaction temperature of the coupling reactor is 120°C, and the reaction pressure is 0.3Mpa.

[0064] The ratio of the absorption section to the extraction section of the ester separation tower is 1:1.5, and the number of theoretical plates in the stripping section is 25; the operating pressure is 0.16Mpa; the operating temperature at the top of the tower is 38°C, and the operating temperature at the bottom of the tower is 180°C; The volume ratio of the dimethyl ester) stream to the absorbent (methanol) stream was 2.2:1.

[0065] Dimethyl oxalate refining tower has 40 theoretical plates, reflux ratio 8.5; operating pressure 0.12Mpa; tower top operating temperature 96°C, tower bottom operating temperature 176°C; dimethyl oxalate extractant and dimethyl oxalate product The ratio is 2.3:1; the dimethyl oxalate extractant is cooled to 100°C by...

Embodiment 3

[0071] The implementation is the same as [Example 1], except that the feed composition, reaction conditions, and tower equipment parameters and operating conditions are different.

[0072] The reaction temperature of the coupling reactor is 130°C, and the reaction pressure is 0.4Mpa.

[0073] The ratio of the absorption section to the extraction section of the ester separation tower is 1:2, and the number of theoretical plates in the stripping section is 15; the operating pressure is 0.2Mpa; the operating temperature at the top of the tower is 42°C, and the operating temperature at the bottom of the tower is 186°C; the extractant (oxalic acid The volume ratio of the dimethyl ester) stream to the absorbent (methanol) stream was 1.8:1.

[0074] Dimethyl oxalate refining tower has 30 theoretical plates, reflux ratio 8.8; operating pressure 0.20Mpa; tower top operating temperature 113°C, tower bottom operating temperature 193°C; dimethyl oxalate extractant and dimethyl oxalate pro...

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Abstract

The invention provides a dimethyl oxalate production method with a byproduct (dimethyl carbonate). The method comprises the following steps: (a) introducing reaction materials containing CO and methyl nitrite into a coupling reactor, and carrying out reactions in the presence of a platinum family metal catalyst to obtain a gas phase material flow containing dimethyl oxalate and dimethyl carbonate; (b) introducing the gas phase material flow containing dimethyl oxalate and dimethyl carbonate into an ester separation tower to contact with a methanol material flow from the top of the ester separation tower and an extracting agent material flow containing oxalic acid from the middle of the ester separation tower in a countercurrent contact mode, obtaining crude methanol from the top of the ester separation tower, and obtaining a mixture containing dimethyl oxalate and dimethyl carbonate from the bottom of the ester separation tower; and (c) introducing the mixture into a dimethyl oxalate refining tower, obtaining a dimethyl carbonate product from the top of the dimethyl oxalate refining tower, and obtaining a dimethyl oxalate product from the bottom of the dimethyl oxalate refining tower; wherein the gas phase material flow containing dimethyl oxalate and dimethyl carbonate is not cooled after being introduced into the ester separation tower.

Description

technical field [0001] The present invention relates to a kind of production method of dimethyl oxalate, also relate to a kind of method of producing dimethyl oxalate and simultaneously by-product dimethyl carbonate. Background technique [0002] Dimethyl oxalate (DMO) is an important intermediate product, which can be hydrolyzed to produce oxalic acid, and can also be hydrogenated to produce ethylene glycol. It has important uses in the chemical industry. The synthetic route of dimethyl oxalate mainly contains two: the first route is to adopt methanol and oxalic acid esterification reaction to synthesize, and this route has the shortcoming that discharges waste water amount is big, and environmental pollution is serious; Another route is by carbon monoxide and suboxide Methyl nitrate is synthesized by coupling reaction under platinum group catalyst. Due to the rapid development of the coal chemical industry in recent years, the second route has attracted widespread attenti...

Claims

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Application Information

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IPC IPC(8): C07C67/36C07C67/48C07C69/36C07C68/00C07C68/08C07C69/96
CPCC07C67/36C07C67/48C07C68/00C07C68/08C07C69/36C07C69/96
Inventor 杨卫胜贺来宾施德胡松
Owner CHINA PETROLEUM & CHEM CORP
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