Method for producing nitric oxide and synthesizing dimethyl oxalate through carbonylation

A technology of dimethyl oxalate and nitric oxide, which is applied in the direction of carbon monoxide or formate reaction preparation, nitric oxide, nitrogen oxides/oxyacids, etc., can solve the problems of production and storage safety hazards, and achieve low cost Low, good market value, effect of equipment operation safety

Active Publication Date: 2013-03-13
久泰能源(鄂尔多斯)有限公司
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Problems solved by technology

[0011] The purpose of the present invention is to overcome the current safety hazards in the preparation and storage of nitrous ester methyl esters, the shortcomings of the carbonylation synthesis of dimethyl oxalate and the process, and provide a method suitable for large-scale production of dimethyl oxalate, which supports the synthesis of dimethyl oxalate. Gas as raw material to produce ethylene glycol process route

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  • Method for producing nitric oxide and synthesizing dimethyl oxalate through carbonylation

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: annual production scale of 2000 tons of dimethyl oxalate

[0030] The specifications of the reaction raw materials are as follows:

[0031] The concentration of dilute nitric acid is 50%, the concentration of sodium nitrite solution is 45%, the purity of CO is 98.5%, the purity of methanol is 99.8%, and the purity of oxygen is 99.5%.

[0032] The reaction feed is as follows:

[0033] CO: 109Nm 3 / h,

[0034] o 2 : 27Nm 3 / h,

[0035] Methanol: 770Kg / h,

[0036] Nitric acid: 38Kg / h,

[0037] Sodium nitrite: 46Kg / h.

[0038] The main control indicators of carbonylation reaction are as follows:

[0039] Into the reactor gas components: NO 2.5%, CO 15%, methyl nitrite 10%, methanol 15%, the rest is N 2 .

[0040] Reaction pressure: 0.3MPa.

[0041] Reaction temperature: 140°C.

[0042] Products and methanol consumption are as follows:

[0043] The amount of dimethyl oxalate in the product is: 280K g / h,

[0044] Dimethyl oxalate purity: ≥99.5%, ...

Embodiment 2

[0047] Embodiment 2: annual production scale of 5000 tons of dimethyl oxalate

[0048] The specifications of the reaction raw materials are as follows:

[0049] The concentration of dilute nitric acid is 50%, the concentration of sodium nitrite solution is 45%, the purity of CO is 98.5%, the purity of methanol is 99.8%, and the purity of oxygen is 99.5%.

[0050] The reaction feed is as follows:

[0051] CO: 270Nm 3 / h,

[0052] o 2 : 67.5Nm 3 / h,

[0053] Methanol: 1850Kg / h,

[0054] Nitric acid: 93Kg / h,

[0055] Sodium nitrite: 109Kg / h.

[0056] The main control indicators of carbonylation reaction are as follows:

[0057] Into the reactor gas components: NO 3.0%, CO 18%, methyl nitrite 10%, methanol 16%, the rest is N 2 .

[0058] Reaction pressure: 0.4MPa.

[0059] Reaction temperature: 140°C.

[0060] Products and methanol consumption are as follows:

[0061] The amount of dimethyl oxalate in the product is: 700K g / h,

[0062] Dimethyl oxalate purity: ≥99.5%,...

Embodiment 3

[0065] Embodiment 3: annual production scale of 10000 tons of dimethyl oxalate

[0066] The specifications of the reaction raw materials are as follows:

[0067] The concentration of dilute nitric acid is 50%, the concentration of sodium nitrite solution is 45%, the purity of CO is 98.5%, the purity of methanol is 99.8%, and the purity of oxygen is 99.5%.

[0068] The reaction feed is as follows:

[0069] CO: 561Nm 3 / h,

[0070] o 2 : 138Nm 3 / h,

[0071] Methanol: 3980Kg / h,

[0072] Nitric acid: 92Kg / h,

[0073] Sodium nitrite: 370Kg / h.

[0074] The main control indicators of carbonylation reaction are as follows:

[0075] Into the reactor gas components: NO 2.0%, CO 15%, methyl nitrite 12%, methanol 15%, the rest is N 2 .

[0076] Reaction pressure: 0.35MPa.

[0077] Reaction temperature: 135°C.

[0078] Products and methanol consumption are as follows:

[0079] The amount of dimethyl oxalate in the product is: 1460K g / h,

[0080] Dimethyl oxalate purity: ≥99...

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Abstract

The invention discloses a method for producing nitric oxide and synthesizing dimethyl oxalate through carbonylation and relates to the technical field of dimethyl oxalate. According to the method disclosed by the invention, nitric oxide production and synthetic process of dimethyl oxalate through carbonylation are combined, so that the safety in a nitric oxide producing process is improved and utilization rate of raw material is increased. In the method disclosed by the invention, the nitric oxide is produced by reacting sodium nitrite with dilute nitric acid, and a raw material of carbonylation reaction, namely carbonic oxide, is taken as gas for stirring, so that the sodium nitrite and the dilute nitric acid fully react in a reactor to obtain the nitric oxide; then the nitric oxide is supplemented to a dimethyl oxalate circulating system along with the carbonic oxide to be esterified and carbonylated; and finally the dimethyl oxalate product is synthesized. The method disclosed by the invention can be used for avoiding the phenomenon that a potential safety hazard exists in the existing production and storage process of dimethyl oxalate and also overcoming the defects of the existing synthetic process of dimethyl oxalate through carbonylation.

Description

technical field [0001] The invention relates to a method for the industrial preparation and carbonylation of nitric oxide to synthesize dimethyl oxalate, more specifically a method for large-scale nitric oxide preparation and carbonylation to synthesize dimethyl oxalate. Background technique [0002] Dimethyl oxalate is mainly used in organic synthesis, and can also be used in plasticizers, pharmaceuticals, pesticides and other industries. Gas-phase catalytic coupling of carbon monoxide to synthesize dimethyl oxalate, as a part of synthesis gas to ethylene glycol technology, has become an important research topic in the field of carbon-chemistry and organic chemical industry in China. Successively, there are Chengdu Institute of Organic Chemistry, Chinese Academy of Sciences, Fujian Institute of Material Structure, Chinese Academy of Sciences, Southwest Chemical Industry Research Institute, Zhejiang University, Tianjin University, East China University of Science and Technol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/36C07C67/36C01B21/24
Inventor 李奇宋少兵丁兆华郑敏武玉晓刘长宇
Owner 久泰能源(鄂尔多斯)有限公司
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