Preparation method of paranitroaniline

A technology of p-nitroaniline and p-nitroaniline chloride, which is applied in the field of preparation of p-nitroaniline, can solve the problems of product coking, poor product appearance, hidden safety hazards, etc., and achieve improved purity, large production capacity, and production safe effect

Active Publication Date: 2012-08-01
苏州市罗森助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This new technology allows for better control over how much nitrogen monoxide (NO) gas can be produced while maintaining safety during manufacturing processes. It also improves the efficiency at which NO reacts into amides or imines that make up organic compounds like pesticides.

Problems solved by technology

This patented technical problem addressed in this patents relates to producing p-niitrazoleamines (p-NTA) from nitrobenzenemicarbazides or related compounds such as nicotinonium bromide). These methods require expensive equipment like reactors, solvents, filters, etc., which are dangerous because they can cause fires if overheated during operation. Additionally, these processes have slow times and may result in reduced yields when compared to other chemical synthesis techniques used on industrial scale.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The preparation method of the p-nitroaniline of the present embodiment comprises the steps:

[0015] (1) Use a high-pressure metering pump to pump p-nitrochlorobenzene and concentrated ammonia water with a concentration of 50wt% into the tubular mixer, wherein p-nitrochlorobenzene is discharged from the storage tank at a flow rate of 2000 kg / hour Pumped into the tubular mixer, ammonia water is pumped into the tubular mixer with a flow rate of 7000kg / hour from the concentrated ammonia water storage tank. The two phases are mixed well.

[0016] (2) The materials fully mixed by the tubular mixer continuously enter the pipeline reactor under the delivery pressure of the high pressure pump for high temperature and high pressure reaction. The reaction temperature is 240°C, the pressure is 12MPa, and the residence time of the material in the pipeline reactor is 1 hour. That is, through the pressure relief valve, the material in the pipeline reactor is continuously disc...

Embodiment 2

[0019] The preparation method of the p-nitroaniline of the present embodiment comprises the steps:

[0020] (1) Use a high-pressure metering pump to pump p-nitrochlorobenzene and concentrated ammonia water with a concentration of 55wt% into the tubular mixer, wherein p-nitrochlorobenzene is discharged from the storage tank at a flow rate of 2000 kg / hour Pumped into the tubular mixer, ammonia water is pumped into the tubular mixer with a flow rate of 7000kg / hour from the concentrated ammonia water storage tank. The two phases are mixed well.

[0021] (2) The material fully mixed by the tubular mixer enters the pipeline reactor continuously under the delivery pressure of the high pressure pump for high temperature and high pressure reaction. The reaction temperature is 240°C, the pressure is 14MPa, and the residence time of the material in the pipeline reactor is 1 hour. That is, through the pressure relief valve, the material in the pipeline reactor is continuously disc...

Embodiment 3

[0024] The preparation method of the p-nitroaniline of the present embodiment comprises the steps:

[0025] (1) Use a high-pressure metering pump to pump p-nitrochlorobenzene and concentrated ammonia water with a concentration of 45wt% into the tubular mixer, wherein p-nitrochlorobenzene is discharged from the storage tank at a flow rate of 2000 kg / hour Pumped into the tubular mixer, ammonia water is pumped into the tubular mixer with a flow rate of 7000kg / hour from the concentrated ammonia water storage tank. The two phases are mixed well.

[0026] (2) The material fully mixed by the tubular mixer enters the pipeline reactor continuously under the delivery pressure of the high-pressure pump for high temperature and high pressure reaction. The reaction temperature is 240°C, the pressure is 10MPa, and the residence time of the material in the pipeline reactor is 1 hour. That is, through the pressure relief valve, the material in the pipeline reactor is continuously disc...

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Abstract

The invention relates to a preparation method of paranitroaniline. The preparation method comprises the following steps that: (1) a high-pressure conveying pump is used for respectively pumping p-nitrochlorobenzene and stronger ammonia water with the concentration being 45 to 55 weight percent into a tubular mixer according to a weight ratio of 1:(3.0-4.0), and a mixed material is obtained through sufficient mixing; (2) the mixed material is continuously conveyed into a pipeline reactor for reaction, the reaction temperature is 235 DEG C to 245 DEG C, the pressure is 10.0 to 14.0MPa, the reaction time is 40 to 90 minutes, after the reaction is completed, the materials are discharged into a low-pressure reaction kettle by a pressure relief valve, and ammonia is recovered through ammonia release; and (3) after the ammonia recovery, the separation is carried out, the materials are centrifuged and washed after the separation completion, and the paranitroaniline is obtained after the materials are centrifuged to the dry state. The method provided by the invention belongs to a method for continuously producing the paranitroaniline, the production is safer, the production capability is higher, the appearance and the purity of the obtained products are respectively improved, the product quality is excellent, and in addition, the cost is reduced.

Description

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Claims

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Application Information

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Owner 苏州市罗森助剂有限公司
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