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Method for preparing methyl nitrite through catalyzing dilute nitric acid

A technology for the production of methyl nitrite and nitric acid, which is applied in the field of chemical industry and can solve the problem of large catalyst consumption

Inactive Publication Date: 2018-02-06
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, patent CN201410123581.8 has developed a method for treating wastewater containing dilute nitric acid using a carbon-based catalyst. This method has a better effect in low-concentration nitric acid, but the amount of catalyst is large

Method used

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  • Method for preparing methyl nitrite through catalyzing dilute nitric acid
  • Method for preparing methyl nitrite through catalyzing dilute nitric acid
  • Method for preparing methyl nitrite through catalyzing dilute nitric acid

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Add 1% nitric acid 300g in batch reactor, add 20 purpose catalyst C 3 N 4 0.5g, heated to 70°C, heated and vaporized 15g of methanol, passed it into the nitric acid solution through the bottom tube, stirred vigorously for 4 hours, analyzed the content of nitric acid and nitrous acid in the effluent by ionic liquid chromatography, and calculated the content of nitric acid Conversion and selectivity to nitrous acid. The conversion rate of nitric acid reaches 95%, and the selectivity of methyl nitrite reaches 81%.

Embodiment 2～5

[0019] Embodiment 2~5: repeat the reaction process of embodiment 1, difference is that reaction condition and catalyst are different. The specific reaction conditions and results of each embodiment are listed in Table 1.

[0020] Table 1, embodiment 2~5 specific reaction conditions

[0021]

Embodiment 6

[0023] Such as figure 1 The particle size shown is 15 mesh 5g C 3 N 4 The catalyst is loaded into a glass tube reactor with a diameter of 15mm, and the reaction temperature is 70°C. Add 1wt% dilute nitric acid reaction solution from the top with a metering pump, and methanol gas is introduced from the bottom of the reactor, and the WHSV is 1.0h -1 , Reduction and esterification reactions are carried out under normal pressure. The conversion rate of nitric acid reaches 95%, and the selectivity of methyl nitrite reaches 81%.

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Abstract

The invention discloses a method for preparing methyl nitrite through catalyzing dilute nitric acid. The method comprises the following steps of using dilute nitric acid and methanol as substrates; under the effect of a nitrogen-containing carbon-based catalyst, one-step reaction and high-selectivity conversion are performed to obtain the methyl nitrite. A continuous fixed bed reactor is used; under the effect of the nitrogen-containing carbon-based catalyst, the nitric acid is promoted to be reduced into methyl nitrite for reaction; the nitrogen ingredients in the catalyst are favorable for the proceeding of the esterification process. The catalyst has high dilute nitric acid conversion efficiency.

Description

technical field [0001] The invention relates to the field of chemistry and chemical engineering, in particular to a method for preparing methyl nitrite by catalyzing dilute nitric acid. Background technique [0002] The development and application of coal-to-ethylene glycol technology provides a new technology route for non-petroleum route to produce ethylene glycol. [0003] Methyl nitrite is an important intermediate in the coal-to-ethylene glycol process. Methyl nitrite and CO are oxidized and carbonized to obtain dimethyl oxalate; dimethyl oxalate is further hydrogenated to obtain ethylene glycol. Methyl nitrite is prepared from coal by reacting methanol with nitric acid-sodium nitrite. During this process, a large amount of dilute nitric acid waste liquid will be produced. The current treatment method is to add metered NaOH for neutralization, but the neutralized wastewater still contains a large amount of nitrate and nitrite, which will cause pollution of water reso...

Claims

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Application Information

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IPC IPC(8): C07C201/04C07C203/00
CPCC07C201/04C07C203/00
Inventor 石松徐杰孙颖苗虹高进郑玺
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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