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Method for synthesizing alkyl nitrite

A technology for synthesizing alkyl nitrite and alkyl nitrite, which is applied in the fields of nitrite preparation and organic chemistry, and can solve the problems of low selectivity of alkyl nitrite and high amount of nitric acid produced by reaction

Active Publication Date: 2020-07-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] The technical problem to be solved by the present invention is the low selectivity of alkyl nitrites in the prior art and the high amount of nitric acid produced by the reaction, and a new method for synthesizing alkyl nitrites is provided

Method used

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  • Method for synthesizing alkyl nitrite
  • Method for synthesizing alkyl nitrite
  • Method for synthesizing alkyl nitrite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Such as figure 1 As shown, the reaction raw materials NO and N 2 It enters the tower reactor with packing from 3, methanol enters from 2, oxygen enters from 1, and reacts with NO and methanol through the α-alumina ceramic membrane oxygen distributor with a membrane pore size of 0.48 μm. The height of the ceramic membrane distributor 10% of the reactor height. At a reaction temperature of 50°C, a reaction pressure of 0.1 MPa, a molar ratio of methanol to NO of 10:1, a molar ratio of NO to oxygen of 6:1, and a residence time of reactants of 15 seconds, the reaction produces methyl nitrite. The nitric acid content of the product was determined to be 11 ppm after condensation and gas-liquid separation, and the selectivity of methyl nitrite was 99.6%.

Embodiment 2

[0036] Such as figure 1 As shown, the reaction raw materials NO and N 2It enters the tower reactor with packing from 3, methanol enters from 2, oxygen enters from 1, and reacts with NO and methanol through the α-alumina ceramic membrane oxygen distributor with a membrane pore size of 0.48 μm. The height of the ceramic membrane distributor 10% of the reactor height. At a reaction temperature of 50°C, a reaction pressure of 0.1 MPa, a molar ratio of methanol to NO of 1:1, a molar ratio of NO to oxygen of 6:1, and a residence time of reactants of 15 seconds, methyl nitrite was produced. The nitric acid content of the product was determined to be 46 ppm after condensation and gas-liquid separation, and the selectivity of methyl nitrite was 99.2%.

Embodiment 3

[0038] Such as figure 1 As shown, the reaction raw materials NO and N 2 It enters the tower reactor with packing from 3, methanol enters from 2, oxygen enters from 1, and reacts with NO and methanol through the α-alumina ceramic membrane oxygen distributor with a membrane pore size of 0.48 μm. The height of the ceramic membrane distributor 10% of the reactor height. At a reaction temperature of 50°C, a reaction pressure of 0.1 MPa, a molar ratio of methanol to NO of 1.1:1, a molar ratio of NO to oxygen of 6:1, and a residence time of reactants of 15 seconds, the reaction produces methyl nitrite. The nitric acid content of the product was determined to be 7 ppm after condensation and gas-liquid separation, and the selectivity of methyl nitrite was 99.3%.

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Abstract

The invention relates to a method for synthesizing alkyl nitrite. The invention mainly aims to overcome the problems of low selectivity of alkyl nitrite and high content of produced nitric acid in the prior art. The method comprises a step of allowing nitrogen oxide, oxygen-containing gas and C1-4 alkyl alcohol to contact with each other in a reactor under oxidation and esterification conditions, wherein the oxygen-containing gas enters the reactor via a ceramic-membrane distributor. With such a technical scheme, the above problems are overcome, and the method is applicable to industrial production of C1-4 alkyl nitrite.

Description

technical field [0001] The invention relates to a method for synthesizing alkyl nitrite, in particular to a method for synthesizing C1-C4 alkyl nitrite. Background technique [0002] Oxalate is an important organic chemical raw material, which is widely used in fine chemical industry to prepare various dyes, medicines, solvents, extractants and various intermediates. In addition, hydrogenation of oxalate can produce ethylene glycol, a very important chemical raw material, and this route can replace the current method of producing ethylene glycol by the petroleum route with high cost. [0003] Traditional oxalate production routes include starch nitric acid oxidation method, cellulose alkali fusion method, sodium formate method, ethylene glycol one-step oxidation method, propylene oxidation method and oxalate alcohol esterification reaction method, but the above-mentioned traditional processes have high cost and energy consumption. Large, serious pollution, unreasonable use ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C203/00C07C201/04
CPCC07C201/04C07C203/00
Inventor 龚海燕刘俊涛刘国强
Owner CHINA PETROLEUM & CHEM CORP