Method for producing o-nitroaniline by multiple series-connected kettles

A technology of o-nitroaniline and multiple reactors in series, applied in the field of ammoniation, can solve the problems of short residence time, difficult control, and high energy consumption of pipeline reactors, and achieve the advantages of reducing residence time, increasing overall volume, and prolonging residence time. Effect

Active Publication Date: 2012-01-18
ANHUI BAYI CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide a method for the production of o-nitroaniline in series with multiple reactors, which can overcome the problems of difficult control and low yield caused by unfavorable factors such as the short residence time of the pipeline reactor

Method used

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  • Method for producing o-nitroaniline by multiple series-connected kettles
  • Method for producing o-nitroaniline by multiple series-connected kettles
  • Method for producing o-nitroaniline by multiple series-connected kettles

Examples

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Embodiment 1

[0030] (1) First, add ammonia water with a mass percentage concentration of 37.5% and o-chloronitrobenzene into eight ammoniated autoclaves connected in series at a volume ratio of 1:1, and the materials in each ammoniated autoclave reach the volume of the autoclave When the temperature is 50%, stop feeding, and heat up each hydrogenation autoclave until the temperature rises above 165°C to allow the materials in each ammoniation autoclave to undergo ammoniation reaction.

[0031] (2) Use the discharge valve to control the pressure of the ammoniated autoclave in the system. When the system pressure reaches 4.0-4.5Mpa and 185-195°C, use a pressure pump to add ammonia water and o-chloronitrobenzene at a rate of 2m3 / h. For the first ammoniated autoclave and the second ammoniated autoclave, use the feed regulating valve to control the volume ratio of the feed amount of the first ammoniated autoclave to the second ammoniated autoclave to be 1:3, and use a pressure pump to pump the l...

Embodiment 2

[0039](1) First, add ammonia water with a mass percentage concentration of 38.5% and o-chloronitrobenzene into eight ammoniated autoclaves in series at a volume ratio of 1:1, and the materials in each ammoniated autoclave reach the volume of the autoclave When the temperature is 50%, stop feeding, and heat up each hydrogenation autoclave until the temperature rises above 165°C to allow the materials in each ammoniation autoclave to undergo ammoniation reaction.

[0040] (2) Use the discharge valve to control the pressure of each ammoniated autoclave in the system. When the system pressure reaches 4.0-4.5Mpa and 185-195°C, use a pressure pump to pump ammonia water and o-chloronitrobenzene at a rate of 2.4m3 / h Add to the first ammoniated autoclave and the second ammoniated autoclave, use the feed regulating valve to control the volume ratio of the feed amount of the first ammoniated autoclave and the second ammoniated autoclave to 1:4, and use a pressure pump to Liquid ammonia i...

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Abstract

The invention discloses a method for producing o-nitroaniline by multiple series-connected kettles. The method comprises the following steps of: adding ammonia water and o-chloro nitrobenzene to eight series-connected ammonification autoclaves, and carrying out ammonification reaction on materials when the content of the materials in each autoclave reaches 45-55%; adding ammonia water and o-chloro nitrobenzene to the first and second ammonification autoclaves when the temperature of each ammonification autoclave reaches 185-195 DEG C and the pressure reaches 4.0-4.4Mpa, and adding liquid ammonia to the fourth and sixth ammonification autoclaves at the same time; discharging the materials in the eighth ammonification autoclave to a discharge buffering tank, and then discharging to a flash distillation tank; washing the depressurized materials flash-distilled by the flash distillation tank with water to obtain an ammonified mixture; and pumping the ammonified mixture to a rectifying tower for rectifying, returning o-chloro nitrobenzene to the ammonification process from the tower top for continuing reaction, cooling o-nitroaniline in the tower kettle, and discharging to a finished product tank. In the invention, continuous kettle type ammonification and rectifying separation process are combined, thereby achieving the purposes of improving the productivity, saving the energy and reducing the consumption.

Description

technical field [0001] The invention relates to the ammoniation technology in organic chemical production, in particular to a method for producing o-nitroaniline by ammoniation. Background technique [0002] There are two methods for producing o-nitroaniline through ammoniation of o-chloronitrobenzene: [0003] 1. Use pipeline reactor for continuous ammoniation: [0004] Add o-nitroaniline and ammonia water continuously into the high-pressure pipeline reactor, and o-chloronitrobenzene and ammonia water enter the reactor. Under the conditions of 14.7 MPa pressure and 230 °C temperature, the ammoniation reaction is carried out and stay in the reactor. After 20 minutes, the pressure is lowered to 98kPa once, and then enters the flash tank for evaporation and deamination. The evaporated ammonia is circulated and absorbed by the hydraulic jet pump, absorbs the low-concentration ammonia water produced, and continues to be used for ammonification after adding part of the liquid a...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/10
Inventor 李德昌陈明峰潘颖
Owner ANHUI BAYI CHEM IND
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