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Method and equipment for continuously producing methyl nitrite

A technology of methyl nitrite and methanol, applied in the preparation of nitrite, organic chemistry, etc., can solve the problems of increasing the amount of wastewater generated, and achieve the effects of minimizing factory investment, minimizing wastewater discharge, and reducing the amount of wastewater generated

Inactive Publication Date: 2013-01-30
SHANGHAI HUAYI ENERGY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this production process uses water as a purifying agent, which increases the amount of wastewater generated during the production process.

Method used

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  • Method and equipment for continuously producing methyl nitrite
  • Method and equipment for continuously producing methyl nitrite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Methyl nitrite is produced by the above-mentioned process.

[0067] (1) The raw material liquid methanol 2000kg / h is pressurized to 0.7MPa (G) by the pump and sent to the top distributor of esterification reaction tower 1, 200Nm 3 / h0.5~1MPa(G) Oxygen is sent to the top distributor of esterification reaction tower 1 through the pipeline, and the amount of NO input is 78kg / h, which can be mixed with the circulating gas returned from the carbonylation system, and flows into the packing reaction zone for reaction. Both the oxidation and esterification of NO take place in the entire reactor space. By turning on the methanol circulation pump at the bottom of the esterification reaction tower 1, the 20t / h methanol solution was transported to the methanol external heat exchanger 3 for cooling, and then returned to the top of the esterification reaction tower for redistribution. The esterification reaction temperature was controlled at 85 °C and the reaction pressure was 0.65 ...

Embodiment 2

[0075] Repeat the process described in Example 1 to produce methyl nitrite. But purifying tower 4 selects toluene as purifying agent, recovery tower 6 is extraction tower, top operating pressure is 0.1MPa (G), operating temperature is 25 ℃. The bottom line 13 of the recovery tower 6 obtains 893 kg / h of esterification by-product materials such as water and nitric acid.

Embodiment 3

[0077] Repeat the process described in Example 1 to produce methyl nitrite. But the purifying agent of purification tower 4 is ethanol, the flow rate of the purifying agent is 5500kg / h (equivalent to the purifying agent per unit time: the molar ratio of the outlet reaction gas is 30:1), the operating pressure at the top of the recovery tower 6 is 0.35MPa (G), and the operating temperature is 35 °C. The bottom line 13 of the recovery tower 6 obtains 1250kg / h of by-product materials of the esterification reaction such as water and nitric acid.

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Abstract

The invention relates to a method and equipment for continuously producing methyl nitrite in large scale. The method for producing methyl nitrite comprises the following steps of: carrying out the esterification of methanol, oxygen and a nitrogen oxide in an esterification reaction tower to obtain methyl nitrite; circulating and returning the liquid flow from the outlet at the bottom of the esterification reaction tower to the top of the tower, leading the gas flow from the outlet at the bottom of the esterification reaction tower to a purification tower and washing the gas from the bottom of the esterification tower by countercurrent contact with an organic purifier; drying the gas from the top of the purification tower in a dryer to obtain methyl-nitrite-containing dry gas; and leading liquid at the bottom of the purification tower to a recovery tower, and separating a recovery purifier. The methyl nitrite produced by the method can be directly used to prepare dimethyl oxalate through oxidization, carbonylation and coupling reaction with CO. Compared with the conventional production process, the method for producing methyl nitrite has the characteristics of economy, environment friendliness, less waste water and the like.

Description

technical field [0001] The invention relates to a method for industrialized continuous production of methyl nitrite and a matching device thereof. Background technique [0002] The oxidative carbonylation of CO coupled to form dimethyl oxalate is a well-known chemical reaction. By introducing methyl nitrite as a strong oxidant, in Pd / Al 2 O 3 Under the action of the catalyst, under suitable temperature and reaction pressure process conditions, CO and methyl nitrite undergo carbonylation coupling reaction to generate dimethyl oxalate and NO. The generated NO is esterified with methanol and oxygen to regenerate new methyl nitrite, thereby realizing the methyl nitrite cycle. [0003] The methyl nitrite regeneration reaction is easy to carry out, no catalyst is required, and the reaction conditions are mild. The regeneration of methyl nitrite (MN, Methyl Nitrite), the main reaction is: [0004] [0005] Side reaction: CH 3 OH+N 2 O4→CH 3 ONO+HNO 3 [0006] 3N 2 O ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/04C07C203/00
Inventor 吴良泉李俊岭应于舟何明康蒋文
Owner SHANGHAI HUAYI ENERGY CHEM
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