Process for the preparation of C1-C4-alkyl nitrites

A technology of alkyl nitrite and esterification, which is applied in the preparation of nitrite, organic chemistry, etc., can solve the problems of loss of economy, removal of reaction heat can not be carried out uniformly and fully, etc., achieve short residence time, increase yield rate, increasing the effect of selectivity

Active Publication Date: 2008-01-02
SHANGHAI HUAYI ENERGY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This invention needs to strictly control the circulation volume of the liquid fraction. If the circulation volume is too small, the reaction heat generated by the gas / liquid contact reaction cannot be removed uniformly and fully. When the circulation volume is large, the economy will be lost.

Method used

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  • Process for the preparation of C1-C4-alkyl nitrites

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Mix gas (N 2 2.43L / min, NO 284mL / min, O 2 70mL / min) enters the oxidation reactor from the position in Figure 1, the reaction temperature of the oxidation reactor is controlled to be 100°C, and the methanol at the top of the esterification reactor enters the reaction system at 4.5mL / min. A certain liquid level is established in the tower kettle in advance, and the temperature is raised for heating. The pressure of the whole reaction system (oxidation reactor and esterification reactor) is 0.1Mpa. The temperature of the tower kettle is about 70°C, the temperature below the reaction section is a temperature distribution between 45-70°C, the temperature of the reaction section is controlled at a temperature distribution between 35-45°C, and the temperature of the refrigerant at the top of the tower is controlled at about -7°C.

[0029] After analysis, the nitric acid and methyl nitrite in the tower bottom material 5 are almost undetectable, and the nitric acid and water...

Embodiment 2-8

[0031] Experiments have been carried out according to the experimental device designed in accompanying drawing (1), wherein the alcohol used is methyl alcohol, and the results are shown in Table 1.

[0032] Table 1

[0033]

Embodiment 9

[0035] Mix gas (N 2 2.43L / min, NO 284mL / min, O 2 70mL / min) enters the oxidation reactor from the position in Figure 1, the reaction temperature of the oxidation reactor is controlled to be 100°C, and the ethanol at the top of the esterification reactor enters the reaction system at 4.5mL / min. A certain liquid level is established in the tower kettle in advance, and the temperature is raised for heating. The pressure of the whole reaction system (oxidation reactor and esterification reactor) is 0.1Mpa. The temperature of the tower kettle is about 100°C, the temperature below the reaction section is a temperature distribution between 50-90°C, the temperature of the reaction section is controlled at a temperature distribution between 35-45°C, and the temperature of the refrigerant at the top of the tower is controlled at about -7°C.

[0036] After analysis, the nitric acid and ethyl nitrite in the tower bottom material 5 are almost undetectable, and the nitric acid and water ...

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Abstract

The invention discloses a making method of C1-C4 alkyl ester of nitrous acid, which comprises the following steps: doing the oxidizing reaction and esterifying reaction in two reactors separately; doing the oxidizing reaction in the oxidizing reactor; doing the esterifying reaction in the esterifying tower reactor; inputting nitrogen oxide, oxygen and one or more of inert gas into oxidizing reactor; selecting the nitrogen oxide from one or more composite gas of NO, N2O3, NO2 and N2O4 with NO constantly; making the mole of NO more than the mole of NO2; using 0.15-0.3 m oxygen for each NO m; making the bulk of inert gas at 0-90% corresponding to total gas; inputting the oxidizing reacting product into the esterifying tower reactor to react with C1-C4 alkanol; using 0.8-3.0 m alkanol for each gram atom nitrogen. The invention can transfer heat effectively to reduce by-product, which is smaller than traditional equipment.

Description

technical field [0001] The present invention relates to a kind of method for preparing alkyl nitrite, more specifically relate to a kind of method through nitrogen oxide, oxygen and C 1 ~C 4 A method for preparing alkyl nitrites from lower alkanols. Background technique [0002] Alkyl nitrite has many uses, such as: as a stabilizer for unsaturated organic compounds; as an additive for motor oil; as a reagent for nitrosation and diazotization. At present, the most important use of alkyl nitrite is to utilize alkyl nitrite to produce alkyl oxalate, and the reaction chemical formula is as follows: [0003] Coupling reaction 2CO+2RONO→2NO+(COOR) 2 (1) [0004] Regeneration reaction 2ROH+0.5O 2 +2NO→2RONO+H 2 O (2) [0005] Due to its use in coupling reactions, people have put forward higher requirements on the method for preparing alkyl nitrites, for example, the gas phase product cannot contain too much water, oxygen, and nitric acid. In addition, for safe and high-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/04C07C203/00
Inventor 单文波黄飚鲁文质吴良泉
Owner SHANGHAI HUAYI ENERGY CHEM
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