A kind of method for producing ortho/p-chlorobenzaldehyde by low-temperature catalytic oxidation

A technology of p-chlorobenzaldehyde and low-temperature catalysis, which is applied in the field of preparation of o-/p-chlorobenzaldehyde, can solve the problems of high reaction temperature, low product selectivity, unfavorable product separation, etc. The effect of low consumption, short process route and green process

Active Publication Date: 2022-04-15
CHINA SALT CHANGZHOU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The liquid phase oxidation method needs to add a large amount of organic solvent, which is not conducive to product separation, and uses hydrogen peroxide as the oxidant, which is easy to generate a large amount of waste water
Gas-phase catalytic oxidation method has higher reaction temperature, lower product selectivity and poor economy
In addition, using pure o-chlorotoluene or p-chlorotoluene as raw materials, because o-chlorotoluene and p-chlorotoluene have close boiling points, separation is difficult, equipment investment is large, and energy consumption is high

Method used

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  • A kind of method for producing ortho/p-chlorobenzaldehyde by low-temperature catalytic oxidation
  • A kind of method for producing ortho/p-chlorobenzaldehyde by low-temperature catalytic oxidation

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Experimental program
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Effect test

Embodiment 1

[0038] 30.1g Mg 0.1 co 0.5 Ti 0.9 Zr 1.0 o x The composite oxide catalyst is loaded into a quartz reaction tube with a diameter of 20mm, and the reaction tube is installed on the trickle bed reactor, and the space velocity is 500h -1 Nitrogen was introduced, and the temperature was raised to 450°C to activate the catalyst. The activation time was 6 hours. After the catalyst activation was completed, the temperature was lowered to 80.3°C under the protection of nitrogen. Add the mixed solution of pyridine and o- and p-chlorotoluene into the mixing kettle according to the mass ratio of 0.51%, and stir evenly. -1 The mass space velocity is continuously added to the reactor from the upper part of the trickle bed reactor, and at the same time, the nitrogen-oxygen mixed gas oxidant with an oxygen content of 30% is pressed for 710h -1 The volumetric space velocity is continuously fed into the reactor from the bottom of the trickle bed reactor, and the reaction temperature of the...

Embodiment 2

[0041] 30.0g Mg 0.1 co 0.5 Ti 0.9 Zr 1.0 ox The composite oxide catalyst is loaded into a quartz reaction tube with a diameter of 20mm, and the reaction tube is installed on the trickle bed reactor, and the space velocity is 500h -1 Nitrogen was introduced, and the temperature was raised to 450°C to activate the catalyst. The activation time was 6 hours. After the catalyst activation was completed, the temperature was lowered to 119.5°C under the protection of nitrogen. Add the mixed solution of pyridine and o- and p-chlorotoluene into the mixing tank according to the mass ratio of 4.9%, and stir evenly. -1 The mass space velocity is continuously added to the reactor from the upper part of the trickle bed reactor, and the nitrogen-oxygen mixed gas oxidant with an oxygen content of 30% is pressed for 1980h -1 The volumetric space velocity is continuously fed into the reactor from the bottom of the trickle bed reactor, and the reaction temperature of the catalytic oxidation ...

Embodiment 3

[0044] 30.1g Mg 0.1 co 0.5 Ti 0.9 Zr 1.0 o x The composite oxide catalyst is loaded into a quartz reaction tube with a diameter of 20mm, and the reaction tube is installed on the trickle bed reactor, and the space velocity is 500h -1 Nitrogen was introduced, and the temperature was raised to 450°C to activate the catalyst. The activation time was 6 hours. After the catalyst activation was completed, the temperature was lowered to 100.8°C under the protection of nitrogen. Add the mixed solution of pyridine and o- and p-chlorotoluene into the mixing kettle according to the mass ratio of 2.51%, and stir evenly. -1 The mass space velocity is continuously added to the reactor from the upper part of the trickle bed reactor, and at the same time, the nitrogen-oxygen mixed gas oxidant with an oxygen content of 30% is pressed for 1400h -1 The volumetric space velocity is continuously fed into the reactor from the bottom of the trickle bed reactor, and the reaction temperature of t...

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Abstract

The invention discloses a method for producing o- / p-chlorobenzaldehyde by a low-temperature catalytic oxidation method. The method uses mixed o- and p-chlorotoluene as a raw material, multi-metal composite oxide as a catalyst, oxygen as an oxidant, and pyridine as an inhibitor Agent, low-temperature catalytic oxidation of o- and p-chlorotoluene in a trickle bed reactor to obtain a mixture of o- and p-chlorobenzaldehyde, and finally separated and purified by using the principle of different melting points of the products. The method has mild reaction conditions, low energy consumption, short reaction time, high raw material utilization rate, effective control in the reaction process, continuous operation and high production efficiency.

Description

technical field [0001] The invention relates to a preparation method of o / p-chlorobenzaldehyde, in particular to a method for preparing o- and p-chlorobenzaldehyde by low-temperature catalytic oxidation using mixed o- and p-chlorotoluene as raw materials. [0002] technical background [0003] O / p-chlorobenzaldehyde is an important raw material in fine chemical industry and an important intermediate in organic synthesis. It is widely used in pesticides, medicines, dyes and other industries. With the continuous development of downstream products of o-chlorobenzaldehyde, its application fields are also expanding, and the demand for it at home and abroad is also increasing. [0004] The industrial preparation of o / p-chlorobenzaldehyde mostly adopts the chlorination hydrolysis method, but as the chlorination depth deepens, o-, p-chlorobenzylidene dichloride will be chlorinated to generate o-, p-chlorobenzyl trichloride, and there will be A large amount of o- and p-chlorobenzoic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/36C07C47/55B01J23/78
CPCC07C45/36B01J23/78
Inventor 孙运林王顺利张驰马凯刘向超朱成明董亮陶文平姚迪
Owner CHINA SALT CHANGZHOU CHEM
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