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Method for preparing C1-C4 alkyl nitrous acid ester

A technology of methyl nitrite and supergravity field, which is applied in the preparation of nitrite and organic chemistry, etc., can solve the problem of low selectivity of alkyl nitrite, achieve production efficiency improvement, good technical effect, microscopic mixing and The effect of mass transfer process enhancement

Active Publication Date: 2014-03-26
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 Alkyl nitrite selectivity is low technical problem, provides a kind of new preparation C 1 ~C 4 Alkyl Nitrite Method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Nitrogen oxides, oxygen and methanol enter the rotating bed supergravity field reactor in countercurrent, which is the same as the rotating bed supergravity field device reactor in Example 1 of patent CN1895766A (the same below), except that the packing layer is filled with Suqing brand 002CR resin catalyst, nitrogen oxide is selected from NO, the ratio of moles of NO to oxygen is 6:1, the reaction temperature is 10°C, the reaction pressure is -0.08MPa, and the ratio of moles of methanol to NO is 2: 1. Under the condition that the rotation speed of the rotor of the rotating bed high gravity field device is 500 rpm, the raw materials are contacted and reacted in the rotating bed high gravity field device. The result is: the conversion rate of oxygen is 100%, and the selectivity of methyl nitrite is 99.75% .

Embodiment 2

[0030] The reactor of the high gravity field device is filled with Suqing brand 002CR resin catalyst. The nitrogen oxide, oxygen and methanol enter the reactor of the rotating bed high gravity field device in countercurrent. The nitrogen oxide is selected from NO. The ratio of the number of moles of NO to oxygen is 5:1, when the reaction temperature is 30℃, the reaction pressure is -0.05MPa, the mole ratio of methanol to NO is 1.5:1, and the rotation speed of the rotor of the rotating bed supergravity field device is 1000rpm, the raw materials are in the rotating bed The result of the contact reaction in the high gravity field device is that the selectivity of methyl nitrite is 99.81%.

Embodiment 3

[0032] The reactor of the high gravity field device is filled with Suqing brand 002CR resin catalyst. The nitrogen oxide, oxygen and methanol enter the reactor of the rotating bed high gravity field device in countercurrent. The nitrogen oxide is selected from NO. The ratio of the number of moles of NO to oxygen is 8:1, the reaction temperature is 50℃, the reaction pressure is -0.02MPa, the mole ratio of methanol to NO is 20:1, and the rotation speed of the rotor of the rotating bed supergravity field device is 3000rpm, the raw materials are in the rotating bed The result of the contact reaction in the high gravity field device is that the selectivity of methyl nitrite is 99.93%.

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Abstract

The invention relates to a method for preparing C1-C4 alkyl nitrous acid ester, which mainly solves the problem in the prior art that a product is low in selectivity. According to the invention, raw materials are nitrogen oxides, oxygen and C1-C4 alkanol, and a revolving bed high gravity field device filled with resin catalysts is adopted as a reactor, under conditions that the reaction temperature is 0-150 DEG C, the reaction pressure is negative 0.09-1.5 MPa, the molar ratio of the C1-C4 alkanol to nitrogen oxide is (1-100):1, and the molar ratio of the nitrogen oxides to the oxygen is (4-50):1, the raw materials is in contact with the catalyst in the revolving bed high gravity field device, so as to generate an effluence with the C1-C4 alkyl nitrous acid ester through reaction. According to the invention, the problem is better solved, and the method is suitable for the industrial production of increasing yield of the C1-C4 alkyl nitrous acid ester.

Description

Technical field [0001] The present invention relates to a preparation C 1 ~C 4 The method of alkyl nitrite, especially the C required for CO coupling to produce oxalate 1 ~C 4 Production method of alkyl nitrite. Background technique [0002] Oxalate is an important organic chemical raw material, which is widely used in fine chemical production of various dyes, medicines, important solvents, extractants and various intermediates. In the 21st century, oxalate has received extensive international attention as a degradable and environmentally friendly engineering plastic monomer. In addition, oxalate can be hydrolyzed at atmospheric pressure to obtain oxalic acid, and ammonia hydrolysis at atmospheric pressure can be used to obtain high-quality slow-acting fertilizer oxalamide. Oxalate esters can also be used as solvents to produce pharmaceutical and dye intermediates, such as various condensation reactions with fatty acid esters, cyclohexylacetophenone, amino alcohols and many hete...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C203/00C07C201/04
Inventor 刘俊涛张琳娜李蕾
Owner CHINA PETROLEUM & CHEM CORP