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Preparation method of C1-C4 alkyl nitrite and reaction equipment implementing same

A technology of C1-C4 and nitrous acid, applied in the direction of preparation of nitrite ester, chemical method for reacting liquid and gas medium, chemical instrument and method, etc., can solve problems such as inability to effectively control the oxidation composition of nitrogen oxides, and achieve The effect of short reaction time, simple reaction equipment, and few by-products

Active Publication Date: 2010-11-17
PUJING CHEM IND SHA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] About N 2 o 3 The preparation method and reaction equipment have not been mentioned in relevant patents and documents so far. Only the patent CN101096340A mentioned about the oxidation of nitrogen oxides, but the oxidation composition of nitrogen oxides cannot be effectively controlled.

Method used

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  • Preparation method of C1-C4 alkyl nitrite and reaction equipment implementing same
  • Preparation method of C1-C4 alkyl nitrite and reaction equipment implementing same
  • Preparation method of C1-C4 alkyl nitrite and reaction equipment implementing same

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Experimental program
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Effect test

Embodiment 1

[0055] The present invention is carried out in plug-flow isothermal reactors, fully mixed isothermal reactors and packed towers. The plug-flow isothermal reactor is made of quartz glass with an inner diameter of 25mm and a tube length of 250mm; the fully mixed isothermal reaction also uses quartz glass with an inner diameter of 150mm and a height of 250mm, and a stirring paddle is added to accelerate the full mixing (paddle or anchor stirring) device, about 250 to 300 rpm); the esterification packed tower is a stainless steel pipe with an inner diameter of 25mm and a pipe length of 1000mm, filled with different types of fillers. There is a casing outside the three devices, and the constant temperature water of different temperatures provided by the constant temperature water bath is respectively introduced into the casing. Experimental conditions: the pressures of plug flow reactor, fully mixed reactor and esterification packed tower are respectively: 0.2Mpa, 0.1Mpa and 0.1Mpa...

Embodiment 2

[0059] Embodiment 2: other conditions are identical with embodiment 1, be porcelain Raschig ring (Dg25) in the esterification packing tower, and temperature is 100 ℃, changes O 2 The amount of feed, thus changing the NO and O 2 Ratio of feed to prepare methyl nitrite.

[0060] Table 2: NO and O 2 Comparison of the yield of methyl nitrite under the feed ratio

[0061]

[0062] NO and O 2 Feed ratio Methyl nitrite yield (%)

[0063]

[0064] 4:1 99.38

[0065] 4.5:1 99.39

[0066] 5:1 99.39

[0067]

Embodiment 3

[0068] Embodiment 3: Other conditions are the same as in Implementation 1, the esterification packed tower is made of porcelain Raschig rings (Dg25), the temperature is 100° C., and the nitrogen feed flow rate is changed to prepare methyl nitrite.

[0069] Table 3: Comparison of methyl nitrite yields under different nitrogen feed rates

[0070]

[0071] Feed amount of nitrogen (ml / min) Methyl nitrite yield (%)

[0072]

[0073] 20 99.66

[0074] 60 98.65

[0075] 100 97.50

[0076] 120 97.36

[0077]

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Abstract

The invention discloses a preparation method of C1-C4 alkyl nitrite, comprising the following steps: a) oxidizing the gases containing NO to generate a gas mixture basically formed by N2O4, NO2 and NO; b) carrying out chemical balance adjustment on the gas mixture generated in the step a) to obtain a gas mixture basically formed by NO and NO2 with molar ratio of 1:1; and c) reacting the gas mixture generated in the step b) with C1-C4 alkanol to obtain the C1-C4 alkyl nitrite. The invention also provides a reaction device implementing the method, comprising i) a plug flow isothermal reactor, ii) a perfectly mixed isothermal reactor and iii) an esterification packed tower. The invention has the advantages of moderate operation conditions, short reaction time, high product purity, strong suitability to the raw materials, etc.

Description

technical field [0001] The present invention relates to a kind of N 2 o 3 and nitrous C 1 -C 4 Preparation method and reaction equipment of alkyl ester. Background technique [0002] C 1 -C 4 Linear alkyl nitrites have many uses, such as: as motor oil additives, stabilizers for unsaturated organic compounds, antispasmodics, oximation, nitrosation, and diazotization; and as chemical Synthetic intermediates. Currently, C 1 -C 4 The most important application of straight-chain alkyl nitrite is to utilize alkyl nitrite coupling to prepare dialkyl oxalate, and the reaction chemical formula (the alkyl is methyl as an example) is as follows: [0003] 2CO+2CH 3 ONO→2NO+(COOCH 3 ) 2 Coupling reaction(1) [0004] 4NO+4CH 3 OH+O 2 →4CH 3 ONO+2H 2 O regeneration reaction(2) [0005] The reaction system and method for the preparation of alkyl nitrite have been researched by relevant research institutions at home and abroad since the 1980s, such as Bayer's re...

Claims

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Application Information

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IPC IPC(8): C07C203/00C07C201/04B01J10/00
Inventor 柳刚李伟计扬张博毛彦鹏骆念军
Owner PUJING CHEM IND SHA
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