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Method for producing C1-C4 alkyl nitrites

A technology of alkyl nitrite and alkanol, which is applied in the preparation of nitrite, chemical instruments and methods, molecular sieve catalysts, etc., and can solve the problems of high content of nitric acid in side reaction products and low selectivity of alkyl nitrite

Active Publication Date: 2011-03-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The technical problem to be solved by this invention is the C 1 ~C 4 Alkyl nitrite selectivity is low, the technical problem of side reaction product nitric acid content is high, provide a kind of new production C 1 ~C 4 Alkyl Nitrite Method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The nitrogen oxide raw material and the first methanol produced by the oxidation of ammonia and air first enter the reactor I, and react to form an effluent I containing methyl nitrite; the effluent is separated to obtain a gas phase effluent II containing NO and containing The liquid phase effluent III of methyl nitrite; the gas phase effluent II containing NO enters the reactor II with the first stream of oxygen, contacts with the aluminosilicate catalyst, and reacts to generate NO 2 and the effluent IV of unreacted NO; the second stream of methanol and effluent IV enters the reactor III, and the reaction generates effluent V containing methyl nitrite; the effluent is separated to obtain non-condensable gas effluent VI and Methyl nitrate effluent VII; non-condensable gas effluent VI is emptied, and the effluent VII containing methyl nitrite enters the subsequent reaction unit after drying treatment; the aluminosilicate catalyst is selected from ZSM-5, and its Si / Al mol...

Embodiment 2

[0030] According to the flow process of Example 1, except that the aluminosilicate catalyst is selected from ZSM-5, and its Si / Al molar ratio is 200:1, silicon oxide is filled in reactor I, and ZSM-5 molecular sieve is packed in reactor III. In reactor I, the reaction temperature is 70°C, the reaction pressure is 1.8 MPa, and the reaction contact time is 150 seconds. 2 The molar ratio is 70:1. The reaction temperature of reactor II is 175° C., the reaction pressure is 1.5 MPa, the reaction contact time is 60 seconds, and the molar ratio of NO in the NO-containing gas phase effluent II to the first stream of oxygen is 18:1. The reaction temperature of Reactor III is 70°C, the reaction pressure is 1.8MPa, and the reaction contact time is 150 seconds. The NO in the second stream of methanol and effluent IV 2 The molar ratio is under the condition of 70:1, and its result is: the selectivity of methyl nitrite is 98.0%, and the content of nitric acid is 3ppm.

Embodiment 3

[0032] According to the flow process of Example 1, except that the aluminosilicate catalyst is selected from ZSM-5, and its Si / Al molar ratio is 50:1, the reactor I is filled with alumina, and the reactor III is filled with ZSM-5 molecular sieves. In reactor I, the reaction temperature is 40°C, the reaction pressure is 0.8 MPa, and the reaction contact time is 50 seconds. 2 The molar ratio is 40:1. The reaction temperature of reactor II is 150° C., the reaction pressure is 0.8 MPa, the reaction contact time is 3 seconds, and the molar ratio of NO in the NO-containing gas phase effluent II to the first stream of oxygen is 8:1. The reaction temperature of reactor III is 45°C, the reaction pressure is 0.8MPa, the reaction contact time is 60 seconds, the second stream of methanol and the NO in effluent IV 2 Under the condition of 10:1 in molar ratio, the result is: the selectivity of methyl nitrite is 98.5%, and the content of nitric acid is 2ppm.

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Abstract

The invention relates to a method for producing C1-C4 alkyl nitrites, which mainly solves the technical problems of low objective product selectivity and high side reaction product nitric acid content in the prior art. The method comprises the following steps of: a) delivering a nitrogen oxide raw material generated by oxidation of ammonia and air and a first stream of C1-C4 alkanol into a reactor I to generate an effluent I containing C1-C4 alkyl nitrites, and separating the effluent to obtain a gas effluent II and a liquid effluent III; b) delivering the gas effluent II and a first stream of oxygen into a reactor II to contact with an aluminosilicate catalyst to generate an effluent IV; c) delivering a second stream of C1-C4 alkanol and the effluent IV into a reactor III to generate an effluent V by reaction, and separating the effluent to obtain a non-condensed gas effluent VI and an effluent VII containing C1-C4 alkyl nitrites; and d) drying the effluent VII, and then delivering the dried effluent VII to a subsequent reaction unit for use. According to the technical scheme, the method well solves the problems, and can be used for industrial production of the increased C1-C4 alkyl nitrites.

Description

technical field [0001] The present invention relates to a kind of production C 1 ~C 4 Alkyl nitrite methods, especially with regard to the C 1 ~C 4 Process for the production of alkyl nitrites. Background technique [0002] Oxalate is an important organic chemical raw material, which is widely used in the fine chemical industry to produce various dyes, medicines, important solvents, extractants and various intermediates. In the 21st century, oxalate, as a degradable and environmentally friendly engineering plastic monomer, has received extensive international attention. In addition, oxalic acid can be obtained by normal pressure hydrolysis of oxalate, and oxalamide can be obtained by normal pressure ammonia solution. Oxalate can also be used as a solvent to produce pharmaceutical and dye intermediates, etc., such as various condensation reactions with fatty acid esters, cyclohexylacetophenone, amino alcohols, and many heterocyclic compounds. It can also synthesize thym...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/04C07C203/00B01J29/06B01J29/40B01J29/70B01J29/08
Inventor 李斯琴刘俊涛蒯骏张惠明
Owner CHINA PETROLEUM & CHEM CORP
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