Process method and method for regenerating methyl nitrite in production of dimethyl oxalate

A technology of methyl nitrite and dimethyl oxalate, applied in the field of dimethyl oxalate production, can solve the problems of low mass transfer and reaction efficiency, affecting the ratio of materials, long fluid residence time, etc. Efficient and easy to operate

Inactive Publication Date: 2011-04-13
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0026] And at present, the above-mentioned regeneration reaction is usually carried out in a bubble column and a packed column, and there are following problems in using these equipment: due to the long residence time and uneven mixing of the fluid in these equipment, the N 2 o 4 The generation of by-products such as nitric acid and formaldehyde leads to a low utilization rate of NO, so tha...

Method used

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  • Process method and method for regenerating methyl nitrite in production of dimethyl oxalate
  • Process method and method for regenerating methyl nitrite in production of dimethyl oxalate
  • Process method and method for regenerating methyl nitrite in production of dimethyl oxalate

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Embodiment 1

[0043] Dealing with the regeneration process of methyl nitrite in a chemical plant: the mixed gas volume of nitric oxide, nitrogen and oxygen is 50000m 3 / h, the molar fraction ratio of each component is 4: 5: 1, and the mol ratio that enters methanol in the rotating packed bed: NO is 1.2, and the rotating speed of the rotating packed bed is 200r / min, and the packing is stainless steel wire mesh packing, gas-liquid The temperature in the rotating packed bed is 30°C, the temperature of the rectifying tower is 80°C, and the concentration of methanol after rectification is 94%. The ester selectivity was 99.2%.

Embodiment 2

[0045] Dealing with the regeneration process of methyl nitrite in a chemical plant: the mixed gas volume of nitric oxide, nitrogen and oxygen is 50000m 3 / h, the molar fraction ratio of each component is 6: 2.5: 1.5, and the mol ratio that enters methanol in the rotary packed bed: NO is 1.8, and the rotating speed of the rotary packed bed is 2800r / min, and the filler is a plastic mesh filler, gas-liquid The temperature in the rotating packed bed is 40°C, the temperature of the rectifying tower is 70°C, and the concentration of methanol after rectification is 91%. The selectivity of ester is 99.9%.

Embodiment 3

[0047] Dealing with the regeneration process of methyl nitrite in a chemical plant: the mixed gas volume of nitric oxide, nitrogen and oxygen is 50000m 3 / h, the molar fraction ratio of each component is 5: 3.77: 1.23, and the mol ratio of methyl alcohol: NO in the rotating packed bed is 1.3, and the rotating speed of the rotating packed bed is 1800r / min, and the packing is stainless steel mesh packing, gas-liquid The temperature in the rotating packed bed is 35°C, the temperature of the rectifying tower is 75°C, and the concentration of methanol after rectification is 93%. The ester selectivity was 99.5%.

[0048] In the above-described embodiment, the amount of oxygen kept is relatively insufficient, and both NO and methanol are excessive. Therefore, the selectivity of methyl nitrite is used as an index, and the yield is expressed as: the selectivity of methyl nitrite=unit time to generate methyl nitrite The amount of oxygen species consumed × 100% / the amount of oxygen spec...

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Abstract

The invention belongs to the technical field of the production of dimethyl oxalate, and particularly relates to a process method and a device for regenerating methyl nitrite in the production of the dimethyl oxalate. In the method, the utilization rate of nitric oxide in the regenerative process is improved, and the using amount of methanol is reduced. The device comprises a rotary filler bed, wherein a gas inlet of the rotary filler bed is connected with sources of nitrogen, oxygen and nitric oxide respectively, a liquid inlet is connected with a methanol storage tank, a liquid outlet is connected with an inlet of a methanol-water mixture storage tank, and a gas outlet is connected with a condenser I. The process method comprises the following steps of: opening the rotary filler bed, so that the nitric oxide, the nitrogen and the oxygen are contacted and reacted with absolute methanol in the rotary filler bed to form a gas phase and a liquid phase; and discharging the gas phase, condensing, and allowing the liquid phase to flow into the methanol-water mixture storage tank. The process method has the advantages that: the process reaction efficiency is high; all NO is used efficiently; and the equipment has a compact structure and small volume and requires a small investment. The equipment has the advantages of making operation easy, along with simple structure, small energy consumption, simple flow, convenience for starting and stopping and the like.

Description

technical field [0001] The invention belongs to the technical field of dimethyl oxalate production, and in particular relates to a process and device for regeneration of methyl nitrite in the production process of dimethyl oxalate, in particular to the recycling of nitric oxide. Background technique [0002] Dimethyl oxalate is an important organic chemical raw material and intermediate. It is widely used in the fine chemical industry to prepare various dyes, medicines, and pesticides. It is also an important solvent and extraction agent. Dimethyl oxalate is hydrolyzed to produce oxalic acid, which can be used to produce high value-added special chemicals for electronic information and national defense atomic energy industries. Organic chemical products such as ammonium oxalate can be obtained by ammoniation. Ethylene glycol is produced by hydrogenation of dimethyl oxalate. Ethylene glycol is also an important chemical raw material. It is widely used in the production of synt...

Claims

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Application Information

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IPC IPC(8): B01J8/10C07C203/00C07C201/04
Inventor 刘有智焦纬洲申红艳祁贵生袁志国
Owner ZHONGBEI UNIV
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