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Method for preparing 3,4-difluorobenzaldehyde through continuous oxidation of 3,4-difluorotoluene

A technology of difluorobenzaldehyde and difluorotoluene, which is applied in the direction of oxidative preparation of carbonyl compounds, separation/purification of carbonyl compounds, organic chemistry, etc., can solve the problems of shortening reaction time, increasing production cost, and producing a large amount of waste acid wastewater. Achieve the effect of wide application range, saving production cost and avoiding the use of co-catalyst

Inactive Publication Date: 2017-05-31
CHANGZHOU UNIV
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  • Description
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  • Application Information

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Problems solved by technology

The defect that this method exists: at first, need to control the depth and condition of chlorination while chlorination; Secondly, also need to add a large amount of catalysts to shorten reaction time in hydrolysis reaction; Finally, will produce a large amount of unavoidable in the reaction Waste acid wastewater, increased production costs

Method used

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  • Method for preparing 3,4-difluorobenzaldehyde through continuous oxidation of 3,4-difluorotoluene
  • Method for preparing 3,4-difluorobenzaldehyde through continuous oxidation of 3,4-difluorotoluene
  • Method for preparing 3,4-difluorobenzaldehyde through continuous oxidation of 3,4-difluorotoluene

Examples

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Effect test

Embodiment 1

[0030] (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.

[0031] (2) Dissolve 2.02g cobalt acetate and 2.02g sodium molybdate in 200ml3,4-difluorotoluene and 200ml acetic acid respectively to form a mixed solution. At this time, n(cobalt acetate):n(3,4-difluorotoluene)= 0.005:1, 2.02g NaBr dissolved in 15% H 2 o 2 form H 2 o 2 -Acetic acid solution, at this time n(sodium bromide):n(3,4-difluorotoluene)=0.005:1,3,4-difluorotoluene-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(3,4-difluorotoluene)...

Embodiment 2

[0033](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.

[0034] (2) Dissolve 6.06g cobalt acetate and 6.06g sodium molybdate in 200ml3,4-difluorotoluene and 200ml acetic acid respectively to form a mixed solution. At this time, n(cobalt acetate):n(3,4-difluorotoluene)= 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(3,4-difluorotoluene)=0.015:1,3,4-difluorotoluene-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(3,4-difluoroto...

Embodiment 3

[0036] (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. .

[0037] (2) Dissolve 6.06g cobalt acetate and 6.06g sodium molybdate in 200ml3,4-difluorotoluene and 200ml acetic acid respectively to form a mixed solution. At this time, n(cobalt acetate):n(3,4-difluorotoluene)= 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(3,4-difluorotoluene)=0.015:1,3,4-difluorotoluene-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(3,4-difluorotoluene)...

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Abstract

The invention provides a method for preparing 3,4-difluorobenzaldehyde through continuous oxidation of 3,4-difluorotoluene and belongs to the technical field of organic synthesis processes. The method is a process technology for preparing 3,4-difluorobenzaldehyde by continuously oxidizing 3,4-difluorotoluene in a tubular reactor with a 3,4-difluorotoluene compound as a raw material, one or more of metal ion complexes of cobalt, molybdenum and bromine as a catalyst, hydrogen peroxide as an oxidant and acetic acid as a solvent. The method has mild conditions and takes short time, the utilization rate of the raw material is high, effective control in the reaction process can be realized, safe, stable and continuous operation is realized, and the production efficiency is high.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and relates to a method for preparing 3,4-difluorobenzaldehyde by continuous oxidation of 3,4-difluorotoluene under liquid-phase reaction conditions, more specifically, using 3,4-difluorotoluene Fluorotoluene is used as substrate, hydrogen peroxide is used as oxidant, one or more metal ion complexes of cobalt, molybdenum, and bromine are used as catalyst, and monocarboxylic acid is used as solvent. Continuous preparation in tubular reactors with different microstructures 3, 4-Difluorobenzaldehyde product. Background technique [0002] 3,4-Difluorobenzaldehyde, molecular formula: C 7 h 4 f 2 O, molecular weight 142.1, finished product is colorless transparent liquid, boiling point 53-55 ℃, density 1.288g / ml, slightly soluble in hot alcohol and ether, insoluble in water, can volatilize with water vapor. 3,4-Difluorobenzaldehyde is one of the important raw materials for the ...

Claims

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Application Information

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IPC IPC(8): C07C45/28C07C45/82C07C47/55
CPCC07C45/28C07C45/82C07C47/55
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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