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Preparation methods of p-chlorobenzonitrile and p-chlorobenzamide

A technology of chlorobenzamide and p-chlorobenzonitrile, applied in the preparation of p-chlorobenzamide and p-chlorobenzonitrile, can solve the problems of high catalyst and equipment requirements, high operation requirements and high reaction temperature, and achieves the preparation route The effect of short time, less environmental pollution and low production cost

Inactive Publication Date: 2019-11-12
三门峡环宇生化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When p-chlorobenzonitrile is prepared by ammoxidation of p-chlorotoluene, side reactions such as deep oxidation may occur, and the requirements for catalysts and equipment are high, the investment is large, the reaction temperature is high (300-500 ° C), and the operation requirements are high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] In this example, p-chlorobenzoic acid and ammonia are used as raw materials, and p-chlorobenzonitrile is generated by the reaction of p-chlorobenzoic acid and ammonia. The entire reaction process is carried out in stages, and the specific preparation process is as follows.

[0018] First, add 200 g of p-chlorobenzoic acid with a content of 98.0% to a 500ml four-necked flask equipped with a thermometer, an ammonia pipe and a distillation column, turn on the heating mantle power supply to heat up, and when the temperature rises to 245 °C, it is basically melted, and then turn on The ammonia gas valve and the pressure reducing valve of the liquid ammonia steel cylinder pass ammonia into the four-necked flask, turn on stirring, control the reaction temperature in the early stage at 240~250 ℃, react for 2h, generate the first intermediate reaction mixture containing ammonium p-chlorobenzoate, stop Through ammonia. The molar ratio of p-chlorobenzoic acid to ammonia was 1:1.5....

Embodiment 2

[0023] In this example, p-chlorobenzoic acid and ammonia are used as raw materials, and p-chlorobenzonitrile is generated by the reaction of p-chlorobenzoic acid and ammonia. The entire reaction process is carried out in stages, and the specific preparation process is as follows.

[0024] First, add 200 g of p-chlorobenzoic acid with a content of 98.0% to a 500ml four-necked flask equipped with a thermometer, an ammonia pipe and a distillation column, turn on the heating mantle power supply to heat up, and when the temperature rises to 245 °C, it is basically melted, and then turn on The ammonia gas valve and the pressure reducing valve of the liquid ammonia steel cylinder pass ammonia into the four-necked flask, turn on stirring, and control the early stage reaction at 240~250 ° C, and react for 2h to generate the first intermediate reaction mixture containing ammonium p-chlorobenzoate, and stop the pass through. ammonia. The molar ratio of p-chlorobenzoic acid to ammonia was...

Embodiment 3

[0028] In this embodiment, p-chlorobenzoic acid and ammonia are used as raw materials, and p-chlorobenzonitrile is generated by the reaction of p-chlorobenzoic acid and ammonia. The entire reaction process is carried out in stages, and the specific preparation process is as follows.

[0029] First, add 3000g of p-chlorobenzoic acid with a content of 98.0% to the 10L ultrasonic constant temperature kettle equipped with a thermometer probe, an ultrasonic generator probe, an ammonia-passing tube and a distillation column, turn on the heating power supply and heat up, and basically melt when the temperature rises to 245°C. After completion, start stirring, then open the ammonia gas valve and pressure reducing valve of the liquid ammonia cylinder to pass ammonia into the ultrasonic thermostatic kettle. In the middle of the reaction mixture, the ammonia flow was stopped. The molar ratio of p-chlorobenzoic acid to ammonia was 1:1.2. The content of ammonium p-chlorobenzoate in the fi...

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PUM

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Abstract

The invention provides preparation methods of p-chlorobenzonitrile and p-chlorobenzamide, and belongs to the technical field of organic chemistry, further to the technical field of organic fine chemicals. The p-chlorobenzonitrile preparation method comprises: generating a p-chlorobenzonitrile-containing mixture by using a p-chlorobenzamide dewatering reaction, carrying out pressure reducing distillation on the p-chlorobenzonitrile-containing mixture to obtain crude nitrile, carrying out water washing on the crude nitrile, filtering, drying, and carrying out pressure reducing distillation to obtain a finished product p-chlorobenzonitrile. According to the present invention, p-chlorobenzamide is generated by carrying out a reaction on p-chlorobenzoic acid and ammonia, wherein p-chlorobenzoicacid and ammonia are used as raw materials, and are subjected to a series of reactions to generate p-chlorobenzonitrile, such that the whole reaction process is continuous and controllable, and the route is short; and the whole reaction process recovers and utilizes the unreacted raw material and the intermediate product so as to reduce the emission of three-waste, achieve the safe, clean and environmentally friendly production and significantly reduce the production cost.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry and the technical field of organic fine chemicals, in particular to a preparation method of p-chlorobenzonitrile and p-chlorobenzamide. Background technique [0002] p-Chlorobenzonitrile, also known as p-chlorobenzonitrile, 4-chlorobenzonitrile, is an important fine chemical and organic preparation intermediate. Due to the chemical activity of the aromatic nitrile cyano group of p-chlorobenzonitrile, a series of fine chemical products can be synthesized through reactions such as hydrolysis, hydrogenation, addition or polycondensation. raw material. It can be used to synthesize pigment diketopyrrolopyrrole (DPP). [0003] At present, there are mainly two preparation methods for p-chlorobenzonitrile. One method is to use p-chlorobenzaldehyde and hydroxylamine hydrochloride to synthesize p-chlorobenzaldehyde oxime, and to dehydrate p-chlorobenzaldehyde oxime to prepare p-chlorobenzonitril...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/20C07C253/34C07C255/50C07C231/02C07C233/65
CPCC07C253/20C07C253/34C07C231/02C07C233/65C07C255/50
Inventor 张卫民梁振贤魏战勇谭静段敬杰张坤王馨悦王艳王志全
Owner 三门峡环宇生化科技有限公司
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