Method for preparing 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 catalyst, etc., can solve the problems of high content of nitric acid by side reaction product and low selectivity of alkyl nitrite.

Inactive Publication Date: 2011-03-30
SHANGHAI RES INST OF PETROCHEMICAL TECH SINOPEC
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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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Nitrogen oxides and oxygen first enter the reactor I, contact with the ZSM-5 molecular sieve catalyst with a Si / Al molar ratio of 400:1, and react to generate NO containing 2 and effluent I of unreacted NO; effluent I and methanol enter reactor II, and the reaction generates effluent II containing methyl nitrite; the effluent II containing methyl nitrite is separated to obtain methyl nitrite, and then After drying, it is used in the subsequent reaction unit; wherein, the nitrogen oxide is selected from NO, the ratio of the mole number of NO to oxygen is 6:1, the reaction temperature of the reactor I is 80 ° C, the reaction pressure is 0.01 MPa, and the reaction contacts The time is 2 seconds, the reaction temperature of the reactor II is 30 ° C, the reaction pressure is 0.01 MPa, the reaction contact time is 10 seconds, the ratio of the mole number of methanol to the NO in the effluent I is 3:1, and the reactor II is filled with Under the condition of inert alumina, the...

Embodiment 2

[0028] Nitrogen oxides and oxygen first enter the reactor I, contact with the ZSM-5 molecular sieve catalyst with a Si / Al molar ratio of 200:1, and react to generate NO containing 2 and effluent I of unreacted NO; effluent I and methanol enter reactor II, and the reaction generates effluent II containing methyl nitrite; the effluent II containing methyl nitrite is separated to obtain methyl nitrite, and then After drying, it enters the subsequent reaction unit for use; wherein, nitrogen oxides are selected from NO, the ratio of the mole number of NO to oxygen is 4:1, the reaction temperature of the reactor I is 121 ° C, the reaction pressure is -0.05MPa, the reaction The contact time is 60 seconds, the reaction temperature of the reactor II is 80 ° C, the reaction pressure is -0.05MPa, the reaction contact time is 80 seconds, the ratio of the mole number of methanol to the NO in the effluent I is 9:1, the reactor II Under the condition of filling inert silica, the result is th...

Embodiment 3

[0030] Nitrogen oxides and oxygen first enter the reactor I, and contact with the ZSM-5 molecular sieve catalyst with a Si / Al molar ratio of 50:1, and the reaction generates NO containing 2 and effluent I of unreacted NO; effluent I and methanol enter reactor II, and the reaction generates effluent II containing methyl nitrite; the effluent II containing methyl nitrite is separated to obtain methyl nitrite, and then The nitrogen oxide is selected from NO, the ratio of the mole number of NO and oxygen is 5:1, the reaction temperature of the reactor I is 160 ° C, the reaction pressure is 0.5 MPa, and the reaction contacts The time is 10 seconds, the reaction temperature of the reactor II is 40 ° C, the reaction pressure is 0.5 MPa, the reaction contact time is 20 seconds, the ratio of the mole number of methanol to the NO in the effluent I is 3.5:1, and the reactor II is filled with Under the condition of 5A molecular sieve, the result is: the selectivity of methyl nitrite is 98...

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Abstract

The invention relates to a method for preparing C1-C4 alkyl nitrites, which mainly solves the technical problems of low target product selectivity and high content of nitric acid as side products in the prior art. The method comprises the following steps of: a, enabling nitric oxide and oxygen to firstly enter a reactor I, reacting to generate an effluent I containing NO2 and unreacted NO; b, enabling the effluent I and C1-C4 alkanols to enter a reactor II, reacting to generate an effluent II containing the nitrites; and c, obtaining the nitrites after separating the effluent II containing the nitrites, enabling the nitrites subjected to the dryness to enter a subsequent reaction unit for use, wherein the nitric oxide contains the NO, and the mol number of the NO is more than that of the NO2, the mol ratio of the NO to the oxygen in the nitric oxide is 4-25:1. The invention better solves the problems, and can be used in the industrialized production for increasing the yield of C1-C4 alkyl nitrites.

Description

technical field [0001] The present invention relates to a kind of preparation C 1 ~C 4 Process for alkyl nitrites, especially with respect to the C required for CO coupling to produce oxalates 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 fine chemicals to produce various dyes, medicines, important solvents, extractants and various intermediates. Entering the 21st century, oxalate has attracted international attention as a biodegradable and environmentally friendly engineering plastic monomer. In addition, oxalic acid can be obtained by normal pressure hydrolysis of oxalate, and high-quality slow-acting chemical fertilizer oxalamide can be obtained by normal pressure ammonolysis. Oxalate esters can also be used as solvents to produce pharmaceutical and dye intermediates, etc., such as various condensation reactions with fatty acid esters, cyclohexyl acetop...

Claims

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Application Information

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IPC IPC(8): C07C201/04C07C203/00B01J29/06B01J29/40B01J29/70B01J29/08
Inventor 刘俊涛宗弘元孙凤侠蒯骏
Owner SHANGHAI RES INST OF PETROCHEMICAL TECH SINOPEC
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