Method for preparing p-chlorobenzaldehyde through continuous oxidization of p-chlorotoluene

A technology of p-chlorobenzaldehyde and p-chlorotoluene, which is applied in the field of organic synthesis process technology, can solve the problems of low selectivity of p-chlorobenzaldehyde, target product selectivity, low yield, low conversion rate, etc., and achieve improved reaction Rate and utilization of raw materials, avoiding the use of co-catalysts, and the effect of saving production costs

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

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Problems solved by technology

The advantage of this method is low cost and simple process; the disadvantage is that the reaction time is long, the catalyst cannot be reused, and the conversion rate is low.
In summary, existing technologies have many shortcomings such as high cost, high energy consumption, complicated process, and low selectivity to p-chlorobenzaldehyde.
[0007] The above method optimizes and improves the preparation of p-chlorobenzaldehyde from different angles by the oxidation of p-chlorotoluene, but there are still some problems to be solved: firstly still mainly adopt the batch production of batch still in the large-scale

Method used

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  • Method for preparing p-chlorobenzaldehyde through continuous oxidization of p-chlorotoluene
  • Method for preparing p-chlorobenzaldehyde through continuous oxidization of p-chlorotoluene
  • Method for preparing p-chlorobenzaldehyde through continuous oxidization of p-chlorotoluene

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Experimental program
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Effect test

Embodiment 1

[0032] (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. The heat exchange medium is heat conduction Oil.

[0033] (2) Dissolve 3.03g of cobalt acetate and 3.03g of sodium molybdate in 200ml of p-chlorotoluene and 200ml of acetic acid to form a mixed solution. At this time, n (cobalt acetate): n (p-chlorotoluene) = 0.0075:1, and 3.03g Sodium bromide dissolved in 15% H 2 o 2 form H 2 o 2 -Acetic acid solution, at this time n (sodium bromide):n (p-chlorotoluene)=0.0075:1, p-chlorotoluene-acetic acid solution and H 2 o 2 -Acetic acid solution is injected in the tubular reactor of continuous heat exchange by constant flow pump respectively with the flow velocity of 8.33ml / min and 16.67ml / min, at this moment n (H ...

Embodiment 2

[0035] (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.

[0036] (2) Dissolve 6.06g of cobalt acetate and 6.06g of sodium molybdate in 200ml of p-chlorotoluene and 200ml of acetic acid to form a mixed solution. At this time, n (cobalt acetate): n (p-chlorotoluene) = 0.015:1, and 6.06g Sodium bromide dissolved in 15% H 2 o 2 form H 2 o 2 -Acetic acid solution, at this time n(sodium bromide):n(p-chlorotoluene)=0.015:1, p-chlorotoluene-acetic acid solution and H 2 o 2 -Acetic acid solution is injected in the tubular reactor of continuous heat exchange by constant flow pump respectively with the flow velocity of 8.33ml / min and 16.67ml / min, at this moment n (...

Embodiment 3

[0038] (1) Device: refer to figure 2 Determine the connection mode of the tubular reactor. The pipeline type is: (3a+3d) straight-through channel + enhanced mixing circular 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. .

[0039] (2) Dissolve 6.06g of cobalt acetate and 6.06g of sodium molybdate in 200ml of p-chlorotoluene and 200ml of acetic acid to form a mixed solution. At this time, n (cobalt acetate): n (p-chlorotoluene) = 0.015:1, and 6.06g Sodium bromide dissolved in 15% H 2 o 2 form H 2 o 2 -Acetic acid solution, at this time n(sodium bromide):n(p-chlorotoluene)=0.015:1, p-chlorotoluene-acetic acid solution and H 2 o 2 -Acetic acid solution is injected in the tubular reactor of continuous heat exchange by constant flow pump respectively with the flow velocity of 8.33ml / min and 16.67ml / min, at this moment n...

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Abstract

The invention relates to a method for preparing p-chlorobenzaldehyde through continuous oxidization of p-chlorotoluene and belongs to the technical field of organic synthesis processes. The method is a process technology for preparing p-chlorobenzaldehyde by continuously oxidizing p-chlorotoluene in a tubular reactor with a p-chlorotoluene compound as a raw material, one or more metal ion complexes of cobalt, molybdenum and bromine as a catalyst, hydrogen peroxide as an oxidizing agent 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 p-chlorobenzaldehyde by continuous oxidation of p-chlorotoluene under liquid phase reaction conditions, more specifically using p-chlorotoluene as a substrate, hydrogen peroxide as an oxidant, cobalt, One or several metal ion complexes of molybdenum and bromine are used as catalysts, monocarboxylic acid is used as solvent, and p-chlorobenzaldehyde products are continuously prepared in tubular reactors with different microstructures. Background technique [0002] 4-Chlorobenzaldehyde is an important chemical intermediate, which has very important application value in medicine, pesticides, dyes, etc. Amino acid and other drugs. In addition, p-chlorobenzaldehyde is also used in the synthesis of acid blue 7BF, acid brilliant blue 6B and other fuels and intermediates in the synthesis of photosensitive materials. [0003] The industrial produ...

Claims

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Application Information

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IPC IPC(8): C07C45/28C07C47/55B01J19/00B01J19/24
CPCC07C45/28B01J19/0053B01J19/2415B01J2219/2403C07C47/55
Inventor 严生虎蒋鑫张跃刘建武沈介发马晓明陈代祥辜顺林倪风超李彦飞王秋红陈明珠魏进吴飞张勇超
Owner CHANGZHOU UNIV
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