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Method for preparing C1-C4 alkyl nitrite ester

A technology of alkyl nitrite and alkanol, which is applied in the preparation of nitrite, organic chemistry, etc., can solve the problem of low selectivity of alkyl nitrite, achieve production efficiency improvement, good technical effect, increase The effect of specific surface area

Active Publication Date: 2014-01-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The technical problem to be solved by this invention is the C 1 ~C 4 The technical problem of low selectivity of alkyl nitrites, providing a new C 1 ~C 4 The preparation method of alkyl nitrite

Method used

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  • Method for preparing C1-C4 alkyl nitrite ester

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Experimental program
Comparison scheme
Effect test

Embodiment 1~11

[0031] Nitrogen oxides are selected from NO, raw materials NO, C 1 ~C 4 The alkanol and the first stream of oxygen enter the first rotating bed supergravity field reactor to react, and the gas phase reaction effluent I containing alkyl nitrite and unreacted nitrogen oxides and the liquid phase reaction containing unreacted alkanol are obtained Effluent I; gas phase reaction effluent I, liquid phase reaction effluent I and the second strand of oxygen enter the second rotating bed supergravity field reactor to react, and obtain reaction effluent II containing alkyl nitrite and liquid phase reaction Effluent III, after separation, gives alkyl nitrite. Wherein, the rotors of the first rotating bed high gravity field reactor and the second rotating bed high gravity field reactor are fixed with porous packing layers, and the first rotating bed high gravity field reactor and the second rotating bed high gravity field reaction The devices are the same as the rotating bed supergravit...

Embodiment 12

[0035] Nitrogen oxides are selected from NO and NO 2 The molar ratio is a mixture of 3:1, the raw material nitrogen oxides, methanol and the first stream of oxygen enter the first rotating bed supergravity field reactor to react, and the gas phase reaction containing alkyl nitrite and unreacted nitrogen oxides is obtained. Effluent I and liquid-phase reaction effluent I containing unreacted methanol; Gas-phase reaction effluent I, liquid-phase reaction effluent I and the second strand of oxygen enter the second rotating bed supergravity field reactor to react to obtain nitrous acid containing The reaction effluent II of the methyl ester and the liquid phase reaction effluent III are separated to obtain methyl nitrite. Wherein, the rotors of the first rotating bed supergravity field reactor and the second rotating bed supergravity field reactor are fixed with porous packing layers, and the raw materials pass through the porous packing layers in the rotating bed supergravity fie...

Embodiment 13

[0037] Nitrogen oxides are selected from NO, and the raw materials NO, methanol and the first stream of oxygen enter the first rotating bed high-gravity field reactor to react, and obtain gas phase reaction effluent I containing methyl nitrite and unreacted nitrogen oxides and containing unreacted nitrogen oxides. The liquid-phase reaction effluent I of methanol reaction; the gas-phase reaction effluent I, the liquid-phase reaction effluent I and the second oxygen enter the second rotating bed supergravity field reactor to react, and obtain the reaction effluent containing methyl nitrite II and the liquid phase reaction effluent III are separated to obtain methyl nitrite. Among them, the rotors of the first rotating bed high-gravity field reactor and the second rotating bed high-gravity field reactor are fixed with porous packing layers, and the raw materials pass through the porous packing layers in a parallel flow in the rotating bed high-gravity field reactors. . The react...

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Abstract

The invention relates to a method for preparing C1-C4 alkyl nitrite ester. The use of the method is aimed to mainly solving the technical problem of low selectivity of the target product alkyl nitrite ester in the prior art. In the method, a technical scheme is adopted as follows: the method comprises the following steps: (a) leading raw materials: nitric oxide, C1-C4 alkanol and first oxygen into a super-gravity field reactor of a first revolving bed for reaction, thus obtaining gas-phase reaction effluent I containing the alkyl nitrite ester, gas-phase reaction effluent I containing unreacted nitric oxide and liquid-phase reaction effluent I containing unreacted C1-C4 alkanol; and (b) leading the gas-phase reaction effluent I, the liquid-phase reaction effluent I and at least second oxygen into at least a super-gravity field reactor of a second revolving bed, so as to obtain the alkyl nitrite ester after the reaction effluent is subjected to separation, thus better solving the problem of the low selectivity of the target product-the alkyl nitrite ester and being used for industrial production of increasing the C1-C4 alkyl nitrite ester.

Description

technical field [0001] The present invention relates to a C 1 ~C 4 The preparation method of alkyl nitrite, especially about the C needed for CO coupling to prepare oxalate 1 ~C 4 Process for the preparation 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 compou...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C203/00C07C201/04
Inventor 刘俊涛李斯琴李蕾
Owner CHINA PETROLEUM & CHEM CORP