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A kind of method and equipment for preparing methyl nitrite

A technology of methyl nitrite and dimethyl oxalate, which is applied in the preparation of nitrite, organic chemistry, etc., can solve the problems of consumption, low NO conversion rate and MN yield, and high energy consumption of esterification towers, and achieves changes in operation. The effect of complex, simple reaction equipment and short reaction time

Active Publication Date: 2022-01-04
PUJING CHEM IND SHA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] (2) In the oxidation reaction, the reaction rate of the reaction (1) increases with the decrease of the reaction temperature, while the NO in the reaction (2) 2 with N 2 o 4 There is a chemical equilibrium between them, high temperature favors N 2 o 4 converted into NO 2 , so there must be N in the oxidation reaction 2 o 4 Produce and impel the generation of reaction (4) and (5), and cause the generation of by-product nitric acid, cause nitrogen raw material to be consumed by a large amount of useless;
[0020] (1) The operating temperature of the fully mixed tower is high and the energy consumption is large;
[0021] (2) The energy consumption of the esterification tower is high under low pressure operation, and the disadvantages of mutual influence of reaction and rectification still exist;
[0022] (3) passing oxygen into the esterification tower is easy to form an explosive gas mixture with the methyl nitrite generated, increasing the operating risk of the device;
[0023] (4) NO conversion rate and MN yield are low at lower operating temperature in the nitric acid recovery tower

Method used

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  • A kind of method and equipment for preparing methyl nitrite
  • A kind of method and equipment for preparing methyl nitrite
  • A kind of method and equipment for preparing methyl nitrite

Examples

Experimental program
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Embodiment 1

[0065] This embodiment is carried out in a plug-flow isothermal reactor and catalytic esterification tower B, and the above-mentioned equipments are all made of stainless steel. The plug flow isothermal reactor has an inner diameter of 50 cm and a tube length of 0.85 m. The tail gas flow rate entering the plug flow isothermal reactor is 1Nm 3 / h, wherein the volume content of NO is 12%, the volume content of methanol is 8%, O 2 The volume content is 2%, and the rest is nitrogen. The inner diameter of the catalytic esterification tower is 30cm, the tower height is 5.3m; the catalyst bulk density is 0.7g / mL, the packing height is 3m, and the catalyst composition is Ni-Zr / Al 2 o 3 , wherein the content of the Ni component is 2wt.% of the mass of the support, and the content of the Zr component is 0.2wt.% of the mass of the support. The reaction pressures of the plug flow isothermal reactor and the catalytic esterification tower are both 0.4MPa. Before the reaction, a certain...

Embodiment 2

[0071] This example is basically the same as Example 1, the difference is that the reaction temperature of the catalytic esterification is maintained at 50°C, and the nitric acid content in the catalytic esterification tower is changed to investigate its influence on the conversion rate of NO and the molar content of MN at the outlet , the experimental data are shown in Table 2:

[0072] Table 2

[0073]

[0074] It can be seen from Table 2 that the higher the nitric acid content, the higher the conversion rate of NO and the higher the content of MN at the outlet. At a higher nitric acid content, a NO conversion rate of more than 95% can still be guaranteed. Therefore, this method is applicable to the working condition of dealing with higher nitric acid content.

Embodiment 3

[0076] This embodiment is basically the same as Example 1, except that three plug-flow isothermal reactors A1 to A3 are selected to be connected in series in this embodiment, wherein the plug-flow isothermal reactor A1 is the same as the reactor in Example 1, Plug-flow isothermal reactor A2 has an inner diameter of 50 cm and a tube length of 0.85 m; plug-flow isothermal reactor A3 has an inner diameter of 50 cm and a tube length of 1.7 m. The reaction temperature of catalytic esterification was maintained at 50°C, and the content of nitric acid in the catalytic esterification tower was changed to investigate its influence on NO conversion rate and MN molar content. The experimental data are shown in Table 3:

[0077] table 3

[0078]

[0079] Compared with Table 2, after connecting three plug-flow isothermal reactors in series, a higher NO conversion rate can still be maintained at a lower nitric acid content range, so this method is also suitable for processing reactions w...

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Abstract

The present invention involves a method and device for nitride nitride. This method includes the following steps: (1) mixing the iliac tail gas and oxygen that combines the CO 羰 本 本 to the dihydrin reaction.NO, NO 2 Gas mixture composed of nitrodine; (2) Under the presence of solid -phase catalysts, the NO in the gas mixture reacts with the water solution containing methanol and nitric acid.To reduce the content of nitric acid, the water solution containing methanol and nitric acid comes from the ester section of the nitrite synthesis process;Compared with the existing technology, the present invention has the characteristics of simple equipment, short response time, low energy consumption, high safety and easy control, and realizes the continuous, stable and efficient recycling of nitrogen elements in the tail gas, which can be widely recovered, which can be widespread.Apply to the production device of industrial ethylene glycol.

Description

technical field [0001] The invention relates to the technical field of organic compound synthesis, and relates to a method and equipment for preparing methyl nitrite, in particular to a method for preparing methyl nitrite by using the carbonylation tail gas of CO carbonylation coupling synthesis of dimethyl oxalate as a raw material and equipment. Background technique [0002] Methyl nitrite (MN) is an important reactant and intermediate in the esterification and carbonylation sections of the coal-based synthesis gas to ethylene glycol process, and its preparation process and reaction equipment have received extensive attention and research. [0003] At present, the synthesis process of methyl nitrite in a typical industrial device for producing ethylene glycol from syngas is divided into two steps, see Chinese patent CN103373925A, firstly, the gas phase oxidation reaction of NO and oxygen to generate NO, NO 2 with N 2 o 4 The mixture, the main reaction formula is as foll...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C201/04C07C203/00
CPCC07C201/04C07C203/00
Inventor 毛彦鹏张博骆念军计扬
Owner PUJING CHEM IND SHA