Rapid material cooling and waste acid recycling process after chlorobenzene thermal insulation nitration

An adiabatic nitration and rapid cooling technology, applied in the preparation of nitro compounds, the preparation of organic compounds, organic chemistry, etc., can solve problems such as short process flow, avoid side reactions and save energy consumption.

Inactive Publication Date: 2009-12-23
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a process technology with short process flow, high resource utilization rate, simple separation process, low energy consumption, safe a

Method used

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  • Rapid material cooling and waste acid recycling process after chlorobenzene thermal insulation nitration

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Experimental program
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Effect test

Embodiment 1

[0026] The main process equipment is: adiabatic nitrification reactor, reduced pressure flash evaporation equipment, cooling and condensation equipment, gas-liquid separation equipment and liquid-liquid separation equipment, etc.

[0027] Such as figure 1 As shown, a process for rapid cooling of materials after adiabatic nitration of chlorobenzene and recycling of waste acid, the process steps are as follows:

[0028] (1) Adiabatic nitrification: In the adiabatic nitrification static mixing reactor, the mixed acid of the nitration reaction is made by mixing industrial grade mass fraction of 98% sulfuric acid, 65% nitric acid and water in a certain proportion, and the dehydration value of the mixed acid is 4.0, chlorine The molar ratio of benzene to nitric acid is 1.05:1.0. Mix chlorobenzene and mixed acid to cause nitration reaction. The temperature of the materials after the nitration reaction is about 120°C, and the reacted materials enter the next step;

[0029] (2) Reduced pre...

Embodiment 2

[0038] The main process equipment is: adiabatic nitrification reactor, reduced pressure flash evaporation equipment, cooling and condensation equipment, gas-liquid separation equipment and liquid-liquid separation equipment, etc.

[0039] Such as figure 1 As shown, a process for rapid cooling of materials after adiabatic nitration of chlorobenzene and recycling of waste acid, the process steps are as follows:

[0040] (1) Adiabatic nitrification: In the SV type adiabatic nitrification static mixing reactor, the mixed acid of the nitration reaction is mixed with industrial grade mass fraction of 98% sulfuric acid, 65% nitric acid and waste acid in a certain proportion. The dehydration value of the mixed acid is 3.0, the molar ratio of chlorobenzene to nitric acid is 1.1:1.0, mixing chlorobenzene and mixed acid to cause a nitration reaction, the temperature of the material after the nitration reaction is about 140°C, and the reacted material enters the next step;

[0041] (2) Flash ...

Embodiment 3

[0050] The main process equipment is: adiabatic nitrification static mixing reactor, reduced pressure flash evaporation equipment, cooling and condensation equipment, gas-liquid separation equipment and liquid-liquid separation equipment, etc.

[0051] Such as figure 1 As shown, a process for rapid cooling of materials after adiabatic nitration of chlorobenzene and recycling of waste acid, the process steps are as follows:

[0052] (1) Adiabatic nitrification: In the SV type adiabatic nitrification static mixing reactor, the mixed acid of the nitration reaction is mixed with industrial grade mass fraction of 98% sulfuric acid, 65% nitric acid and waste acid in a certain proportion. The dehydration value of the mixed acid is 2.0, the molar ratio of chlorobenzene to nitric acid is 1.1:1.0, mixing chlorobenzene and mixed acid to produce a nitration reaction, the temperature of the material after the nitration reaction is about 160°C, and the reacted material enters the next step;

[...

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Abstract

The invention discloses a rapid material cooling and waste acid recycling process after chlorobenzene thermal insulation nitration, comprising the following steps of: (1) chlorobenzene nitration; (2) vacuum flashing of material after the reaction; (3) gas-liquid separation; (4) gas-phase material cooling and condensation; (5) gas-liquid separation and gas-phase material treatment; (6) liquid-liquid separation of gas-phase materials from the previous step and treatment of oil-phase materials, and the use of water-phase materials as washing water of nitrochlorobenzene crude products in the eighth step; (7) liquid-liquid separation to the liquid-phase materials obtained from gas-liquid separation in the third step, utilization of water phase for mixed acid ingredients and treatment of the oil-phase materials in a next step; (8) mixed washing of the nitrochlorobenzene crude products and the water-phase materials obtained from the liquid-liquid separation in the sixth step; and (9) further treatment of the water-phase materials obtained from the liquid-liquid separation, and further separation and refining of the oil-phase nitrochlorobenzene for obtaining the products. The rapid material cooling and waste acid recycling process after chlorobenzene thermal insulation nitration has the advantages of less three wastes, cost conservation and convenient industrial implementation.

Description

Technical field [0001] The invention relates to a process for rapid cooling of materials after chlorobenzene nitration reaction and waste acid recycling process, in particular to a process for rapid cooling of materials after chlorobenzene adiabatic nitration reaction and waste acid recycling process, belonging to the technical field of fine chemicals . Background technique [0002] Nitrochlorobenzene is mainly o-nitrochlorobenzene, m-nitrochlorobenzene and p-nitrochlorobenzene. Nitrochlorobenzene is an important intermediate in dye, medicine, perfume and other industries. [0003] The method for preparing nitrochlorobenzene by the adiabatic nitration reaction of chlorobenzene is to preheat the raw material chlorobenzene and the mixed acid to undergo a nitration reaction in an adiabatic reactor. The mixed acid used in the nitration reaction is mixed with nitric acid, sulfuric acid and water in a certain proportion. In the process of adiabatic nitration of chlorobenzene, the outle...

Claims

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Application Information

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IPC IPC(8): C07C205/12C07C201/08C07C201/16
Inventor 许文林王雅琼姚干兵张淮浩张小兴陈小芹
Owner YANGZHOU UNIV
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