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Method for preparing C1-C4 alkyl nitrous acid ester by catalytic reaction

A technology of alkyl nitrite and catalytic reaction, applied in the preparation of nitrite, organic chemistry, etc., can solve the problem of low selectivity of alkyl nitrite, improve production efficiency, increase specific surface area, micro-mixing and the effect of mass transfer process enhancement

Active Publication Date: 2012-08-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The technical problem to be solved by this invention is the C 1 ~C 4 The technical problem of low selectivity of alkyl nitrites provides a new way to produce C by catalytic reaction 1 ~C 4 Alkyl Nitrite Method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Nitrogen oxides and oxygen first enter the reactor I, contact with the ZSM-5 molecular sieve catalyst I with a Si / Al molar ratio of 280:1, and react to form NO 2 And the effluent I of unreacted NO; The effluent I and methanol enter the reactor II, and the ZSM-5 molecular sieve catalyst II with a Si / Al molar ratio of 50:1 contacts and reacts to generate the effluent II containing methyl nitrite; The effluent II of methyl nitrite is separated to obtain methyl nitrite; wherein, reactor II is a rotating bed supergravity field reactor, which is the same as the rotating bed supergravity field reactor in Example 1 of the patent CN1895766A (Below the same), only resin catalyst is loaded on the rotor; Nitrogen oxide is selected from NO, and the ratio of the molar number of NO and oxygen is 6: 1, and the reaction temperature of reactor 1 is 80 ℃, and reaction pressure is 0.01MPa, reaction The contact time is 3 seconds, the reaction temperature of the reactor II is 30°C, the react...

Embodiment 2

[0032] Nitrogen oxides and oxygen first enter the reactor I, contact with the ZSM-5 molecular sieve catalyst I with a Si / Al molar ratio of 200:1, and react to form NO 2 And the effluent I of unreacted NO; The effluent I and methanol enter the reactor II, and the ZSM-5 molecular sieve catalyst II with a Si / Al molar ratio of 100:1 contacts and reacts to generate the effluent II containing methyl nitrite; The effluent II of methyl nitrite is separated to obtain methyl nitrite; wherein, reactor II is a rotating bed supergravity field reactor, nitrogen oxides are selected from NO, and the molar ratio of NO to oxygen is 4:1 , the reaction temperature of reactor I is 121°C, the reaction pressure is -0.05MPa, the reaction contact time is 60 seconds, the reaction temperature of reactor II is 80°C, the reaction pressure is -0.05MPa, the methanol and NO in effluent I The ratio of the number of moles is 9:1, and under the condition that the rotating speed of the rotor of the rotating bed ...

Embodiment 3

[0034] Nitrogen oxides and oxygen first enter the reactor I, contact with the ZSM-5 molecular sieve catalyst I with a Si / Al molar ratio of 50:1, and react to form NO 2 And the effluent I of unreacted NO; The effluent I and methanol enter the reactor II, and the ZSM-5 molecular sieve catalyst II with a Si / Al molar ratio of 300: 1 contacts and reacts to generate the effluent II containing methyl nitrite; The effluent II of methyl nitrite is separated to obtain methyl nitrite; wherein, reactor II is a rotating bed supergravity field reactor, nitrogen oxides are selected from NO, and the molar ratio of NO to oxygen is 5:1 , the reaction temperature of reactor I is 160°C, the reaction pressure is 0.5MPa, the reaction contact time is 10 seconds, the reaction temperature of reactor II is 40°C, the reaction pressure is 0.5MPa, the moles of methanol and NO in effluent I The ratio is 3.5: 1, under the condition that the rotating speed of the rotor of the rotary bed high gravity reactor ...

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PUM

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Abstract

The invention relates to a method for preparing C1-C4 alkyl nitrous acid ester by a catalytic reaction, which mainly solves the problem in the prior art that a product, namely nitrous acid ester is low in selectivity. The method comprises the following steps: (a), a nitrogen oxide and oxygen enter a reactor I at first and are in contact reaction with a catalyst I, so as to generate an effluence I containing NO2 and unreacted NO; (b), the effluence I and the C1-C4 alkanol enter a reactor II and are in contact reaction with a ZSM-5 molecular sieve catalyst so as to generate an effluence II containing nitrous acid ester; and (c), the nitrous acid ester is obtained through separating the effluence II containing the nitrous acid ester, wherein the reactor I is a fixed bed reactor, the reactor II is a revolving bed high-gravity field reactor, and a ZSM-5 molecular sieve catalyst layer is fixed on the rotor of the revolving bed high-gravity field reactor. According to the invention, the problem is better solved, and the method is suitable for the industrial production of C1-C4 alkyl nitrous acid ester.

Description

technical field [0001] The present invention relates to a kind of production C by catalytic reaction 1 ~C 4 Alkyl nitrite methods, especially with regard to the C 1 ~C 4 The production method of alkyl nitrite by step-by-step combination reaction. 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C203/00C07C201/04
Inventor 刘俊涛孙凤侠
Owner CHINA PETROLEUM & CHEM CORP
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