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Continuous thermo-insulation method for production of nitro-chlorobenzene

A kind of technology of nitrochlorobenzene and chlorobenzene, applied in the field of producing nitrochlorobenzene, can solve problems such as large expenditure and complexity

Inactive Publication Date: 2005-09-21
LANXESS DEUTDCHLAND GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the disadvantage of this reaction is that relatively large quantities of unwanted m-nitrochlorobenzene are produced, which are complicated and expensive to remove

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 186 kg / h of 81% sulfuric acid, 13.3 kg / h of 70.6% nitric acid and 19.7 kg / h of chlorobenzene containing about 7-8% of nitrochlorobenzene were continuously added to the tubular reactor. The average hybrid density is 6.2 W / L. The temperature during mixing was 40°C. After 180 seconds, the reaction mixture reached the end of the reactor; the temperature at the reactor outlet was 92-94°C. The reaction mixture was heated to 120° C. and the phases were separated in a static separator within 90 seconds. The spent sulfuric acid is reconcentrated to the original sulfuric acid content and recycled to the nitration reaction. Condensers used for condensate are sprayed with chlorobenzene to prevent nitrochlorobenzene dissolved in spent sulfuric acid from forming deposits of nitrochlorobenzene. The nitrochlorobenzene phase is analyzed by gas chromatography, and its composition is as follows:

[0039] Chlorobenzene 8.97%

[0040] o-Nitrochlorobenzene 34.14%

[0041] m-nitrochloro...

Embodiment 2

[0044] Example 2 (do not carry out by the inventive method)

[0045] 186 kg / h of 75% sulfuric acid, 9.6 kg / h of 65% nitric acid and 12.3 kg / h of chlorobenzene containing about 7% of nitrochlorobenzene were continuously added to the tubular reactor. The average hybrid density is 6.2 W / L. The temperature during mixing was 110°C, after 180 seconds the reaction mixture reached the end of the reactor; the temperature at the reactor outlet was 140°C. The phase separation takes place in a static separator. The spent sulfuric acid is reconcentrated to the original sulfuric acid content and recycled to the nitration reaction. Condensers used for condensate are sprayed with chlorobenzene to prevent nitrochlorobenzene dissolved in spent sulfuric acid from forming deposits of nitrochlorobenzene. The nitrochlorobenzene phase is analyzed by gas chromatography, and its composition is as follows:

[0046] Chlorobenzene 2.70%

[0047] o-Nitrochlorobenzene 37.61%

[0048] m-nitrochlorob...

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PUM

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Abstract

The present invention relates to a continuous adiabatic process for preparing nitrochlorobenzene, in which the waste sulfuric acid produced during the practice of the process is reconcentrated and recycled into the nitration reaction.

Description

technical field [0001] The present invention relates to a process for the continuous adiabatic production of nitrochlorobenzene in which the spent sulfuric acid produced during the actual production process is reconcentrated and recycled to the nitration reaction. Background technique [0002] Nitrochlorobenzene is an important intermediate for the preparation of dyes, pharmaceuticals and pesticides. There are special requirements for the ortho-nitrochlorobenzene, which is obtained by nitration of chlorobenzene with a yield of about 35%. p-Nitrochlorobenzene also has some industrial applications. There is basically no need to generate meta-nitrochlorobenzene, and its industrial application is very limited. [0003] In industry, nitrochlorobenzene is produced by nitration of chlorobenzene. For the nitration reaction, a mixture of sulfuric acid, nitric acid and water is usually used. During the reaction, a large amount of spent sulfuric acid is produced, which pollutes the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C201/08C07B61/00C07C205/12
CPCC07C205/12C07C201/08
Inventor R·德穆斯B·-M·科尼T·林H·-J·拉尔茨H·-M·维贝尔E·茨恩吉布尔R·莱贝里希
Owner LANXESS DEUTDCHLAND GMBH
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