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Method for preparing alkyl nitrite

A technology of alkyl nitrite and alkanol, applied in the preparation of nitrite, organic chemistry, etc., can solve the problem of low selectivity of alkyl nitrite, achieve simple structure, improve conversion rate, and ensure residence time Effect

Active Publication Date: 2011-10-19
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 the present invention is the low technical problem of the alkyl nitrite selectivity existing in the previous literature, and a new method for preparing alkyl nitrite is provided

Method used

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Experimental program
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preparation example Construction

[0024] Below in conjunction with accompanying drawing, the equipment of the method for preparing alkyl nitrite of the present invention is described in detail.

[0025] The supergravity reactor in the method for preparing alkyl nitrite of the present invention adopts and comprises reactor housing 1, rotor 5, gas partition 7, liquid inlet 3 and gas outlet 4, wherein the upper gravity reactor is set The packing layer 6 and the lower packing layer 15, the lower side of the lower packing layer 15 is also provided with a first gas inlet 2 and a second gas inlet 16, the two gas inlets respectively enter the nitrogen oxide gas raw material and oxygen, and the liquid inlet 3 tubes A liquid distributor 8 is arranged in the road, and the liquid inlet 3 enters C1-C4 alkyl alcohol. The upper packing layer 6 and the lower packing layer 15 in the high gravity reactor are two layers of coaxial packing layers, and the gas outlet 4 of the high gravity reactor is provided with a foam catcher 9 ...

Embodiment 1

[0030] The gas volume of the first gas containing nitrogen oxide raw material is 100m 3 / h, wherein the concentration of NO is 10% v (the rest is nitrogen), and the gas volume of the second gas oxygen is 2m 3 / h, the two gases enter the supergravity reactor from the first gas inlet 2 and the second gas inlet 16 respectively, and diffuse into the lower packing 15 under the action of the pressure difference, and the rotating packing speed is adjusted to 2000rpm. The methanol solution enters the liquid distributor 8 of the supergravity reactor through the liquid inlet 3 and is sprayed to the inner side of the packing. The molar ratio of nitrogen oxides and methanol liquid in the gas is 1:30, and the gas and liquid are in the upper packing layer 6 of the supergravity reactor. In countercurrent contact, the reaction generates gaseous effluent I and liquid effluent II containing methyl nitrite. The gas effluent I containing methyl nitrite is sent to the follow-up system through the...

Embodiment 2

[0032] The gas volume of the first gas containing nitrogen oxide raw material is 100m 3 / h, wherein, the concentration of NO is 21% v (the rest is nitrogen), the gas volume of the second gas oxygen is 3.8m 3 / h, the two gases enter the supergravity reactor from the first gas inlet 2 and the second gas inlet 16 respectively, and diffuse into the lower packing 15 under the action of the pressure difference, and the rotating packing speed is adjusted to 4000rpm. The methanol solution enters the liquid distributor 8 of the supergravity reactor through the liquid inlet 3 and is sprayed to the inner side of the packing. The molar ratio of nitrogen oxides and methanol liquid in the gas is 1:15, and the gas and liquid are in the upper packing layer 6 of the supergravity reactor. In countercurrent contact, the reaction generates gaseous effluent I and liquid effluent II containing methyl nitrite. The gas effluent I containing methyl nitrite is sent to the follow-up system through the ...

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Abstract

The invention relates to a method for preparing alkyl nitrite, and the method is mainly used for solving the technical problem that the selectivity of target product alkyl nitrite is low in the prior art. The method comprises the following steps: based on nitrogen oxide, oxygen and C1-C4 alkanol serving as raw materials, feeding the raw materials into a super-gravity reactor and then carrying out contact reaction on the rotating packed bed of the super-gravity reactor at the reaction temperature of 0-150 DEG C at the reaction pressure of minus 0.09-1.5MPa based on the conditions that the molar ratio of C1-C4 alkanol to nitrogen oxide is (1-100):1 and the molar ratio of nitrogen oxide to oxygen is (4-50):1, thus generating gaseous effluent containing C1-C4 alkyl nitrite. By utilizing the technical scheme of the invention, the problem in the prior art can be well solved. The method can be used in industrial production for increasing the yield of alkyl nitrite.

Description

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

Claims

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Application Information

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IPC IPC(8): C07C203/00C07C201/04
Inventor 刘俊涛李斯琴刘国强
Owner CHINA PETROLEUM & CHEM CORP
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