Washing impurity-removing technology of crude nitrochlorobenzene products after chlorobenzene thermal insulation nitration

A technology for crude nitrochlorobenzene and adiabatic nitration, which is applied in the preparation of organic compounds, organic chemistry, chemical instruments and methods, etc., and can solve the problems of wastewater containing organic matter and sulfate, difficult biochemical conversion, and large primary water consumption. , to achieve the effect of facilitating large-scale industrialization, less energy consumption, and reducing the amount of wastewater treatment

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

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Problems solved by technology

[0003] The traditional washing and impurity removal process of crude nitrochlorobenzene uses primary water for mixed washing, which not only consumes a lot of primary water, but also produces a large amount of waste water containing organic matter and sulfate
[0004] The wastewater produced during the adiabatic nitrification of chlorobenzene contains a variety of toxic and harmful organic substances, which are generally difficult to biochemically transform

Method used

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  • Washing impurity-removing technology of crude nitrochlorobenzene products after chlorobenzene thermal insulation nitration

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The main process equipment is: mixing scrubber and liquid-liquid separator, etc.

[0025] like figure 1 Shown, a kind of washing impurity-removing process of nitrochlorobenzene crude product after adiabatic nitration reaction of chlorobenzene, described process step is as follows:

[0026] (1) Mixed washing for the first time: In the static mixing scrubber, the nitrochlorobenzene crude product obtained by decompression flash evaporation and oil-water separation of the material after the adiabatic nitration reaction of chlorobenzene is condensed with the condensate obtained by decompression flash evaporation. The water and the aqueous phase material obtained in the second liquid-liquid separation process are mixed and washed, the volume ratio of the washing water used in the mixed washing to the crude nitrochlorobenzene is 10:1, and the operating temperature of the mixed washing is 80 ° C. Sulfuric acid and a small amount of organic matter entrained in the chlorobenzene...

Embodiment 2

[0033] The main process equipment is: mixing scrubber and liquid-liquid separator, etc.

[0034] like figure 1 Shown, a kind of washing impurity-removing process of nitrochlorobenzene crude product after adiabatic nitration reaction of chlorobenzene, described process step is as follows:

[0035] (1) Mixed washing for the first time: In the tank-type stirring mixed washing equipment, the operating temperature of the mixed washing is 40°C, and the nitrochloride obtained by decompression flash evaporation and oil-water separation of the material after the adiabatic nitration reaction of chlorobenzene The benzene crude product is mixed with the condensed water obtained by decompression flash evaporation and the aqueous phase material obtained in the second liquid-liquid separation process, and the volume ratio of the washing water used for the mixed washing to the nitrochlorobenzene crude product is 1:1. Sulfuric acid and a small amount of organic matter entrained in the crude n...

Embodiment 3

[0042] The main process equipment is: mixing scrubber and liquid-liquid separator, etc.

[0043] like figure 1 Shown, a kind of washing impurity-removing process of nitrochlorobenzene crude product after adiabatic nitration reaction of chlorobenzene, described process step is as follows:

[0044] (1) The first mixed washing: In the tubular mixed washing machine, the operating temperature of the mixed washing is 60 ° C, and the nitrochlorobenzene obtained by decompression flash evaporation and oil-water separation of the material after the adiabatic nitration reaction of chlorobenzene The condensed water obtained by the crude product and decompression flash evaporation and the aqueous phase material obtained in the second liquid-liquid separation process are mixed and washed, and the volume ratio of the washing water used for the mixed washing and the crude product of nitrochlorobenzene is 1: 1. Sulfuric acid and a small amount of organic matter entrained in the nitrochloroben...

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Abstract

The invention discloses a washing impurity-removing technology of crude nitrochlorobenzene products after a chlorobenzene thermal insulation nitration, comprising the following steps: (1) mixed washing of the crude nitrochlorobenzene products with condensation water obtained by vacuum flashing and water-phase materials obtained by secondary liquid-liquid separation is conducted; (2) wastewater in the water-phase materials is removed, and oil-phase materials enter the next step; (3) mixed washing of the oil-phase materials, the water-phase materials obtained by liquid-liquid separation of the third time and a neutralizer is conducted; (4) the water phase materials are used as primary mixed washing water, and the oil-phase materials enter the next step; (5) mixed washing of the oil-phase materials and water is conducted; and (6) the water-phase materials are used as secondary mixed washing water, and the oil-phase materials are separated and refined. The washing impurity-removing technology has the advantages of simpleness, easy operation, less energy consumption, washing water conservation, wastewater reduction, recyclable auxiliary products, saved cost and convenient realization of large-scale industrialization.

Description

technical field [0001] The invention relates to a process for washing and removing impurities of crude nitrochlorobenzene, in particular to a process for washing and removing impurities of crude nitrochlorobenzene after adiabatic nitration reaction of chlorobenzene, and belongs to the technical field of fine chemicals. Background technique [0002] In the process of preparing nitrochlorobenzene by adiabatic nitration of chlorobenzene, sulfuric acid is used as a catalyst, and chlorobenzene and nitric acid undergo a nitration reaction to generate nitrochlorobenzene. The material after the continuous adiabatic nitration reaction adopts the decompression flash technology to cool the reacted material rapidly, distill off the water and the unreacted raw material chlorobenzene; After liquid-liquid separation, the water phase is mainly sulfuric acid aqueous solution, which is recycled for nitration reaction; the oil phase is crude nitrochlorobenzene containing a mixture of p-nitroch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/12C07C201/16
Inventor 许文林王雅琼张小兴张淮浩姚干兵陈小芹
Owner YANGZHOU UNIV
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