Method of preparing 2,4-dichlorobenzaldehyde through continuous oxidation of 2,4-dichlorotoluene

A technology of dichlorobenzaldehyde and dichlorotoluene, applied in the fields of oxidative preparation of carbonyl compounds, chemical instruments and methods, organic chemistry, etc., can solve problems such as harsh reaction conditions, achieve short reaction time, high production efficiency, and save production costs Effect

Inactive Publication Date: 2017-05-24
CHANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] In the production process of the above method, it is necessary to strictly control the depth of chlorination to prevent side reactions; on, actually implement
[0012] The method described above optimizes and improves the preparation of 2,4-dichlorobenzaldehyde by oxidation of 2,4-dichlorotoluene from different angles, but there are still some problems to be solved: firstly, batch stills are still mainly used in large-scale production. Batch production; Secondly, in the production process, the extensive use of catalysts, the control of the degree of chlorination and the monitoring of subsequent reactions all put forward strict requirements for industrial production

Method used

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  • Method of preparing 2,4-dichlorobenzaldehyde through continuous oxidation of 2,4-dichlorotoluene
  • Method of preparing 2,4-dichlorobenzaldehyde through continuous oxidation of 2,4-dichlorotoluene
  • Method of preparing 2,4-dichlorobenzaldehyde through continuous oxidation of 2,4-dichlorotoluene

Examples

Experimental program
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Effect test

Embodiment 1

[0037] (1) Device: refer to figure 2 Determine the connection mode of the tubular reactor, the pipeline type is: (3a+3b) direct flow channel + round cake pulse variable diameter rectangular flat pipeline, the inner diameter and volume of the pipeline are determined according to the flow rate and reaction residence time, and the heat exchange medium is heat conduction Oil.

[0038](2) Dissolve 1.01g of cobalt acetate and 1.01g of sodium molybdate in 200ml of 2,4-dichlorotoluene and 200ml of acetic acid respectively to form a mixed solution. At this time, n(cobalt acetate):n(2,4-dichlorotoluene)= 0.0025:1, dissolve 1.01g NaBr in 15% H 2 o 2 form H 2 o 2 -Acetic acid solution, at this time n (sodium bromide):n (2,4-dichlorotoluene)=0.0025:1,2,4-dichlorotoluene-acetic acid solution and H 2 o 2 -Acetic acid solution is injected in the tubular reactor of continuous heat exchange by the flow rate of 5.33ml / min and 10.67ml / min respectively, at this moment n(H 2 o 2 ): n(2,4-d...

Embodiment 2

[0040] (1) Device: refer to figure 2 Determine the connection mode of the tubular reactor. The pipeline type is: (3a+3c) direct flow channel + oblique square cake pulse variable diameter rectangular flat pipeline. The inner diameter and volume of the pipeline are determined according to the flow rate and reaction residence time. The heat exchange medium is heat transfer oil.

[0041] (2) Dissolve 6.06g of cobalt acetate and 6.06g of sodium molybdate in 200ml of 2,4-dichlorotoluene and 200ml of acetic acid respectively to form a mixed solution. At this time, n (cobalt acetate): n(2,4-dichlorotoluene)= 0.015:1, 6.06g NaBr dissolved in 15% H 2 o 2 form H 2 o 2 - acetic acid solution, at this time n (sodium bromide): n (2,4-dichlorotoluene)=0.015:1,2,4-dichlorotoluene-acetic acid solution and H 2 o 2 -Acetic acid solution is injected in the tubular reactor of continuous heat exchange by the flow velocity of 8.33ml / min and 16.67ml / min respectively, at this moment n(H 2 o 2...

Embodiment 3

[0043] (1) Device: refer to figure 2 Determine the connection mode of the tubular reactor. The pipeline type is: (3a+3d) direct flow channel + enhanced mixed round cake type rectangular flat pipeline. The inner diameter and volume of the pipeline are determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil. .

[0044] (2) Dissolve 6.06g of cobalt acetate and 6.06g of sodium molybdate in 200ml of 2,4-dichlorotoluene and 200ml of acetic acid respectively to form a mixed solution. At this time, n (cobalt acetate): n(2,4-dichlorotoluene)= 0.015:1, 6.06g NaBr dissolved in 15% H 2 o 2 form H 2 o 2 - acetic acid solution, at this time n (sodium bromide): n (2,4-dichlorotoluene)=0.015:1,2,4-dichlorotoluene-acetic acid solution and H 2 o 2 -Acetic acid solution is injected in the tubular reactor of continuous heat exchange by the flow velocity of 8.33ml / min and 16.67ml / min respectively, at this moment n(H 2 o 2 ): n(2...

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Abstract

The invention relates to a method of preparing 2,4-dichlorobenzaldehyde through continuous oxidation of 2,4-dichlorotoluene, and belongs to the technical field of organic synthetic process. The method includes the steps that a 2,4-dichlorotoluene compound is used as a raw material, one or more metal ion complexes of cobalt, molybdenum and bromine are used as catalysts, hydrogen peroxide is used as an oxidizing agent, acetic acid is used as solvent, and 2,4-dichlorotoluene is continuously oxidized in a tubular reactor to prepare 2,4-dichlorobenzaldehyde. The method is mild in condition, short in reaction time, high in raw material use ratio, safe, stable and high in production efficiency and can achieve effect control in the reaction process and continuous operation.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and relates to a method for preparing 2,4-dichlorobenzaldehyde by continuous oxidation of 2,4-dichlorotoluene under liquid-phase reaction conditions, more specifically, using 2,4-dichlorobenzaldehyde Chlorotoluene is used as a substrate, hydrogen peroxide is used as an oxidant, one or several metal ion complexes of cobalt, molybdenum, and bromine are used as catalysts, and monocarboxylic acids are used as solvents. Continuously prepare 2 in tubular reactors with different microstructures, 4-Dichlorobenzaldehyde product. Background technique [0002] 2,4-Dichlorobenzaldehyde is a very important fine chemical, it is an intermediate in the synthesis of many important chemicals, 2,4-Dichlorobenzaldehyde is used to produce dye intermediates benzaldehyde-2,4-di Sulfonic acid, while benzaldehyde-2,4-disulfonic acid is used to synthesize active blue K-FGR, acid lake blue A, acid lak...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/28C07C47/55B01J19/24
CPCC07C45/28B01J19/242C07C47/55
Inventor 刘建武蒋鑫张跃严生虎沈介发马晓明陈代祥辜顺林倪风超李彦飞王秋红陈明珠
Owner CHANGZHOU UNIV
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