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Ethyl nitrite regeneration technological method and device used in diethyl oxalate production process

A technology of ethyl nitrite and diethyl oxalate, which is applied to the preparation of nitrite, separation methods, chemical instruments and methods, etc., can solve the problem of affecting the ratio of materials, low mass transfer and reaction efficiency, and long fluid residence time etc. to achieve the effect of high reaction efficiency, simple structure and easy operation

Active Publication Date: 2011-04-20
ZHONGBEI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0026] However, the above-mentioned regeneration reactions are usually carried out in bubble towers and packed towers at present, and there are following problems in using these devices: due to the long residence time and uneven mixing of fluids in these devices, N 2 o 4 The formation of by-products such as nitric acid and acetaldehyde leads to a low utilization rate of NO, so that the system needs to add a certain amount of NO in the coupling reaction, which directly affects the ratio of materials in the coupling and regeneration reactions. relationship, and the mass transfer and reaction efficiency in traditional tower equipment is low, so that a large amount of ethanol is required, resulting in problems such as increased side reactions and large rectification load

Method used

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  • Ethyl nitrite regeneration technological method and device used in diethyl oxalate production process
  • Ethyl nitrite regeneration technological method and device used in diethyl oxalate production process
  • Ethyl nitrite regeneration technological method and device used in diethyl oxalate production process

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Embodiment 1

[0043] Treatment of ethyl nitrite regeneration process in a chemical plant: mixed gas volume of nitric oxide, nitrogen and oxygen is 50000m 3 / h, the molar fraction ratio of each component is 4: 5: 1, the mol ratio that enters ethanol in the rotating packed bed: NO is 1.2, and the rotating speed of rotating packed bed is 200r / min, and filler is stainless steel wire mesh filler, gas-liquid The temperature in the rotating packed bed is 30°C, the temperature of the rectifying tower is 95°C, and the concentration of ethanol after rectification is 94%. The ester selectivity was 99.3%.

Embodiment 2

[0045] Treatment of ethyl nitrite regeneration process in a chemical plant: 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, enters the ethanol in the rotating packed bed: the mol ratio of NO is 1.8, and the rotating speed of the rotating 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 85°C, and the ethanol concentration after rectification is 90%. After the gas-liquid reacts in the rotating packed bed, the NO mole fraction of the gas outlet is 0.0010, and the ethyl nitrite The ester selectivity was 99.9%.

Embodiment 3

[0047] Treatment of ethyl nitrite regeneration process in a chemical plant: mixed gas volume of nitric oxide, nitrogen and oxygen is 50000m 3 / h, the molar fraction ratio of each component is 5: 3.76: 1.24, enters the ethanol in the rotating packed bed: the mol ratio of NO is 1.3, and the rotating speed of the rotating packed bed is 1800r / min, and the packing is stainless steel wire mesh packing, gas-liquid The temperature in the rotating packed bed is 35°C, the temperature of the rectifying tower is 90°C, and the ethanol concentration after rectification is 92%. After the gas-liquid reacts in the rotating packed bed, the NO mole fraction at the gas outlet is 0.0003, and the ethyl nitrite The ester selectivity was 99.4%.

[0048] In the foregoing embodiment, the amount of oxygen kept is relatively insufficient, and both NO and ethanol are excessive. Therefore, the selectivity of ethyl nitrite is used as an index, and the yield is expressed as: selectivity of ethyl nitrite=unit...

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Abstract

The invention belongs to the technical field of diethyl oxalate production and specifically relates to an ethyl nitrite regeneration technological method and device used in a diethyl oxalate production process, which improve nitric oxide utilization rate in the regeneration process and reduce ethanol usage quantity. The device comprises a rotating packed bed, the gas inlet of the rotating packed bed is respectively connected with a nitrogen source, an oxygen source and a nitric oxide source, the liquid inlet is connected with an ethanol storage tank, the liquid outlet is connected with the inlet of an ethanol and water mixture storage tank, and the gas outlet is connected with a condenser I. The technological process comprises the following steps of: starting the rotating packed bed, carrying out contact reaction on nitric oxide, nitrogen, oxygen and absolute ethyl alcohol in the rotating packed bed to generate a gas phase and a liquid phase, condensing discharged gas phase and makingthe liquid phase flow into the ethanol and water mixture storage tank. The technological method has the advantages of high reaction efficiency, efficient utilization of all NO (nitric oxide) and little investment, and the device has the advantages of compact and simple structure, small size, convenience for operation, little energy consumption, simple processes, convenience for starting and stopping and the like.

Description

technical field [0001] The invention belongs to the technical field of diethyl oxalate production, in particular to a process and device for regeneration of ethyl nitrite in the production process of diethyl oxalate, in particular to the recycling of nitric oxide. Background technique [0002] Diethyl oxalate is an important organic chemical raw material and intermediate, widely used in the fine chemical industry to prepare various dyes, medicines, pesticides and other industries, and is also an important solvent and extractant. Diethyl 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 diethyl oxalate. Ethylene glycol is also an important chemical raw material. It is widely used in the production of synthetic fibers...

Claims

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Application Information

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IPC IPC(8): B01J19/18B01D5/00C07C203/00C07C201/04
Inventor 刘有智焦纬洲袁志国祁贵生申红艳
Owner ZHONGBEI UNIV
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