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Methyl nitrite regeneration method

A technology of methyl nitrite and methanol, applied in nitrite preparation, chemical recovery, organic chemistry and other directions, can solve the problems of complex process, poor economy, poor operation safety, etc., to simplify the follow-up process, reduce equipment investment, improve Effect of regeneration rate

Active Publication Date: 2014-07-23
WUHUAN ENG +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, none of the above-mentioned reactor types and methods can really solve the problem of nitric acid generated by side reactions, and some methods still have problems such as complicated process, poor operation safety, and poor economy.

Method used

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  • Methyl nitrite regeneration method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The circulating gas 1 containing nitric oxide, whose specific composition (volume percentage) is 12% nitric oxide, 2% methyl nitrite, 8% methanol, 12% carbon monoxide and 66% nitrogen, enters the regeneration reactor 12 in two streams, The regeneration reactor 12 has a pressure of 0.5Mpa, and a stream accounting for 20% (volume percentage) of the total gas volume enters the lower section 3 of the regeneration reactor 12 from the bottom of the tower, reacts with nitric acid in the lower section 3 to generate nitrogen dioxide and rises to the upper section 4, and the remaining 80% (percentage by volume) enters the upper section 4 of the regeneration reactor 12 from the middle, and supplementary oxygen 2 is added to the circulating gas in the middle of the regeneration reactor, and fresh methanol 8 is sprayed on the top of the tower. In the upper section 4, nitric oxide and oxygen , methanol reaction regeneration methyl nitrite, the obtained gas containing methyl nitrite is...

Embodiment 2

[0050] The circulating gas 1 containing nitric oxide, whose specific composition (volume percentage) is 5% nitric oxide, 5% methyl nitrite, 7% methanol, 17% carbon monoxide and 66% nitrogen, enters the regeneration reactor 12 in two streams, The regeneration reactor 12 pressure is 0.40Mpa, accounts for 25% (volume percent) of the total gas volume and enters the lower section 3 of the regeneration reactor 12 from the bottom of the tower, reacts with nitric acid in the lower section 3 to generate nitrogen dioxide and rises to the upper section 4, and the remaining 75% (percentage by volume) enters the upper section 4 of the regeneration reactor 12 from the middle, and the supplementary oxygen 2 is added into the recycle gas in the middle of the regeneration reactor 12, and fresh methanol 8 is sprayed on the top of the tower. In the upper section 4, nitric oxide and Oxygen and methanol react to regenerate methyl nitrite, and the obtained gas containing methyl nitrite is discharged...

Embodiment 3

[0055] The circulating gas 1 containing nitric oxide, whose specific composition (volume percentage) is 15% nitric oxide, 1% methyl nitrite, 12% methanol, 15% carbon monoxide and 57% nitrogen, enters the regeneration reactor 12 in two streams, The regeneration reactor 12 has a pressure of 0.35Mpa, and one stream accounting for 5% (volume percentage) of the total gas volume enters the lower section 3 of the regeneration reactor 12 from the bottom of the tower, reacts with nitric acid in the lower section 3 to generate nitrogen dioxide and rises to the upper section 4, and the remaining 95% (percentage by volume) enters the upper section 4 of the regeneration reactor 12 from the middle, and the supplementary oxygen 2 is added into the recycle gas in the middle of the regeneration reactor 12, and fresh methanol 8 is sprayed on the top of the tower. In the upper section 4, nitric oxide and Oxygen and methanol react to regenerate methyl nitrite, and the obtained gas containing methy...

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Abstract

The invention discloses a methyl nitrite regeneration method, and is used for solving the problems of low regeneration rate of methyl nitrite, poor operational stability of a system caused by improper side reaction control, increase of operating cost and the like. The methyl nitrite regeneration method comprises the following steps: forming recycled gas containing 5-20% of nitric oxide after synthesis of methyl nitrite and carbon monoxide carbonyl, and entering the recycled gas to a methyl nitrite regeneration reactor in two parts, wherein a small part of recycled gas enters the lower section of the regeneration reactor from the bottom, the rest part of recycled gas and supplementing oxygen gas enter the upper section of the regeneration reactor from the middle part together; spraying fresh methyl alcohol into the tower top of the regeneration reactor, discharging methyl nitrite-containing gas from the tower top, pressurizing tower bottoms led out from the tower by using a pump and entering the tower bottoms to the lower section of the regeneration reactor from the middle part of the regeneration reactor; arranging a reboiler on the tower of the regeneration reactor, filling the lower section of the regeneration reactor with a catalyst, and arranging stuffing and / or a tower plate on the upper section of the regeneration reactor. The methyl nitrite regeneration method is simple in process, low in equipment investment and operating cost and high in regeneration rate of methyl nitrite and can be used for effectively solving the side reaction problem.

Description

technical field [0001] The invention relates to a regeneration method of methyl nitrite. Background technique [0002] In methyl nitrite (CH 3 ONO) and carbon monoxide (CO) carbonylation dimethyl oxalate (DMO) or dimethyl carbonate (DMC) industrial plant, the carbonylation product gas contains a certain amount of nitric oxide (NO), the NO needs to be regenerated converted to CH 3 ONO, the reaction equation is as follows: [0003] NO+1 / 2O 2 →NO 2 [0004] NO 2 +NO→N 2 o 3 [0005] 2CH 3 OH+N 2 o 3 →2CH 3 ONO+H 2 o [0006] above CH 3 In the ONO regeneration reaction, there are also the following side reactions: [0007] 3NO 2 +H 2 O→2HNO 3 +NO [0008] NO+HNO 3 →NO 2 +HNO 2 [0009] 3HNO 2 →HNO 3 +2NO+H 2 o [0010] generate HNO 3 The side reaction will lead to CH at the outlet of the regeneration reactor 3 The content of ONO is gradually reduced, and the effective raw material NO in the system is also lost X , which requires that NO must be ad...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C203/00C07C201/04
CPCY02P20/584
Inventor 陈伟建孔渝华闫常群张国建钱胜涛王保山王志峰刘华伟双建永王先厚马高飞肖二飞吕仪军刘应杰雷军吕明
Owner WUHUAN ENG
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