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Method for preparing m-nitrobenzaldehyde by using microchannel reactor

A micro-channel reactor, nitrobenzaldehyde technology, applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, preparation of organic compounds, etc. and other problems, to achieve the effect of improving purity and yield, speeding up reaction rate, and continuous reaction process

Pending Publication Date: 2022-05-13
廊坊市北辰创业树脂材料股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this method yield is lower, only has about 60%~80%, and contains a large amount of ortho-position and para-position by-products in the product, because the polarity of ortho-position and para-position by-products is close to m-nitrobenzaldehyde, Difficult to separate and purify, resulting in lower purity of the m-nitrobenzaldehyde product
In addition, when the nitration reaction is carried out in a traditional reactor, not only due to the intense heat release of the reaction, problems such as "flying temperature" or even explosion are prone to occur, but also strong acids (nitric acid and sulfuric acid) will seriously corrode the reaction equipment.

Method used

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  • Method for preparing m-nitrobenzaldehyde by using microchannel reactor

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Experimental program
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Embodiment 1

[0042] The present embodiment provides a kind of method utilizing microchannel reactor to prepare m-nitrobenzaldehyde, and concrete steps are as follows:

[0043] condensation

[0044] Use a metering pump to pump benzaldehyde and isopropylamine into the first microchannel reactor respectively to carry out condensation reaction to generate Schiff base, and control the temperature of the reaction system in the first microchannel reactor to be 10-20°C, wherein benzene The pumping flow rate of formaldehyde is 200mL / min, and the pumping flow rate of isopropylamine is 166mL / min. During the pumping process, a balance is used to check the amount of pumped benzaldehyde and isopropylamine.

[0045] nitrification

[0046] Mixed acid configuration: after mixing nitric acid with a mass fraction of 98% and sulfuric acid with a mass fraction of 98% according to a mass ratio of 1:9, cool to room temperature and set aside;

[0047] The product Schiff base obtained after the condensation reac...

Embodiment 2

[0053] The method that utilizes microchannel reactor to prepare m-nitrobenzaldehyde that this embodiment provides is similar to embodiment 1, and difference only is that the flow rate of each material is different, and the flow rate of benzaldehyde is 300mL / min in the present embodiment, and the flow rate of isopropylamine The flow rate of Schiff base is 273mL / min, the flow rate of Schiff base is 573mL / min, and the flow rate of mixed acid is 1157mL / min.

[0054] The yield of the m-nitrobenzaldehyde product that present embodiment makes is 94.2%, and HPLC purity is 99.6%

Embodiment 3

[0056] The method that utilizes microchannel reactor to prepare m-nitrobenzaldehyde that this embodiment provides is similar to embodiment 1, and difference only is that the flow rate of each material is different, and the flow rate of benzaldehyde is 500mL / min in the present embodiment, and the flow rate of isopropylamine is 435mL / min, the flow rate of Schiff base is 935mL / min, and the flow rate of mixed acid is 1841mL / min.

[0057] The yield of the m-nitrobenzaldehyde product obtained in this embodiment is 92.5%, and the HPLC purity is 99.8%.

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Abstract

The invention discloses a method for preparing m-nitrobenzaldehyde by using a microchannel reactor, which comprises the following steps: carrying out condensation reaction on benzaldehyde and isopropylamine at 10-20 DEG C to generate Schiff base; carrying out nitration reaction on the Schiff base at 5-35 DEG C under the action of mixed acid of concentrated sulfuric acid and concentrated nitric acid; and after the nitration reaction is finished, carrying out hydrolysis and post-treatment to obtain the m-nitrobenzaldehyde. Wherein the condensation reaction and the nitration reaction are respectively carried out in the microchannel reactor. According to the preparation method for preparing m-nitrobenzaldehyde provided by the invention, the yield and purity of the final product m-nitrobenzaldehyde can be remarkably improved by controlling the temperatures of the condensation reaction and the nitration reaction aiming at the specific reaction substrate benzaldehyde. In addition, the preparation method is low in raw material cost, simple to operate and easy to control, convenient in post-treatment, high in safety and suitable for industrial continuous production.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for preparing m-nitrobenzaldehyde using a microchannel reactor. Background technique [0002] m-Nitrobenzaldehyde is an important intermediate in organic synthesis, and can be used in the pharmaceutical industry to prepare calcium iopanoate, iopanoic acid, calcium choline, m-hydroxybitartaric acid, and nifedipine. In addition, m-nitrobenzaldehyde can also be used to make dyes, surfactants, etc. [0003] In the prior art, the production method of m-nitrobenzaldehyde is to use benzaldehyde as a raw material in a traditional stirred tank, and carry out nitration with potassium nitrate, sodium nitrate or nitric acid in the presence of sulfuric acid to generate m-nitrobenzaldehyde. But this method yield is lower, only has about 60%~80%, and contains a large amount of ortho-position and para-position by-products in the product, because the polarity of ortho-position...

Claims

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Application Information

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IPC IPC(8): C07C201/12C07C205/44C07C249/02C07C251/24B01J19/00
CPCC07C201/12C07C249/02B01J19/0093B01J2219/00819B01J2219/00873C07C205/44C07C251/24
Inventor 张子印刘彩霞
Owner 廊坊市北辰创业树脂材料股份有限公司
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