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Continuous heat-insulating technology of nitrochlorobenzene

A nitrochlorobenzene and process technology, which is applied in the field of continuous adiabatic process, can solve the problems of complex cost and achieve high yield effect

Inactive Publication Date: 2006-07-26
LANXESS DEUTDCHLAND GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this process has the disadvantage that it yields a relatively high proportion of undesired m-nitrochlorobenzene, whose removal, as already mentioned, is complex and expensive

Method used

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  • Continuous heat-insulating technology of nitrochlorobenzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] At 40°C, 418g H 2 SO 4 (100% concentration), 167g phosphoric acid (85% concentration), 61g water and 53.8g HNO 3 (65% concentration) was first added to an insulated sulfonation cup (diameter 100mm) equipped with flow turbulators and two turbine mixers (diameter 39.9mm) installed on the rotating shaft, after 3 seconds, 68.7g chlorine was added Benzene reacts without cooling. After 120 seconds, the reaction mixture had reached a final temperature of 90°C and stirring was stopped. After phase separation, 85.3 g of an organic phase were obtained.

[0043] Chlorobenzene 5.32% by weight

[0044] o-nitrochlorobenzene 37.19% by weight

[0045] m-nitrochlorobenzene 0.75% by weight

[0046] p-nitrochlorobenzene 56.25% by weight

[0047] Dinitrochlorobenzene 0.25% by weight

[0048] The ratio of para / ortho nitrochlorobenzene is 1.50

[0049] The spent acid was concentrated again to the original water content at 150° C. at 110 mbar and mixed with nitric acid again. After ...

Embodiment 2

[0051] At 40°C, 316.5g H 2 SO 4 (100% concentration), 323.0g phosphoric acid (85% concentration), 6.5g water and 53.8g HNO 3 (65% concentration) was first added to an insulated sulfonation cup (diameter 100mm) equipped with flow turbulators and two turbine mixers (diameter 39.9mm) installed on the rotating shaft, after 3 seconds, 68.7g chlorine was added Benzene reacts without cooling. After 160 seconds, the reaction mixture had reached a final temperature of 90°C and stirring was stopped. After phase separation, 83.9 g of an organic phase were obtained.

[0052] Chlorobenzene 5.59% by weight

[0053] o-Nitrochlorobenzene 38.30% by weight

[0054] m-nitrochlorobenzene 0.70% by weight

[0055] p-Nitrochlorobenzene 54.65% by weight

[0056] Dinitrochlorobenzene 0.23% by weight

[0057] The ratio of para / ortho nitrochlorobenzene is 1.41

[0058] The spent acid was concentrated again to the original water content at 150° C. at 110 mbar and mixed with nitric acid again. A...

Embodiment 3

[0059] Embodiment 3 (not according to the present invention)

[0060] At 40°C, 646.2g H 2 SO 4 (81% concentration) and 53.8g HNO 3 (65% concentration) was first added to an insulated sulfonation cup (diameter 100mm) equipped with flow turbulators and two turbine mixers (diameter 39.9mm) installed on the rotating shaft, after 3 seconds, 68.7g chlorine was added Benzene reacts without cooling. After 135 seconds, the reaction mixture had reached a final temperature of 94°C and stirring was stopped. After phase separation, 87.8 g of organic phase were obtained.

[0061] Chlorobenzene 6.25% by weight

[0062] o-Nitrochlorobenzene 34.43% by weight

[0063] m-nitrochlorobenzene 0.85% by weight

[0064] p-nitrochlorobenzene 57.30% by weight

[0065] Dinitrochlorobenzene 0.14% by weight

[0066] The ratio of para / ortho nitrochlorobenzene is 1.62

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Abstract

A method for the continuous production of nitrochlorobenzene by nitration of chlorobenzene with a mixture of sulfuric, phosphoric and nitric acids and water under adiabatic conditions comprises: (1) mixing the reactants at 10-80 degrees C using a phosphoric acid content of 10-50 wt%; (2) separating the products at the reactor outlet; and (3) concentrating waste acids for recycling. A method for the continuous production of nitrochlorobenzene (I) comprises: (1) feeding chlorobenzene, sulfuric acid, phosphoric acid, nitric acid and water simultaneously or in any sequence into a stirred reactor and mixing at an initial temperature of 10-80 degrees C; (2) using a mixture with a phosphoric acid content (based on all acids and water) of 10-50 wt%; (3) carrying out the reaction under adiabatic conditions; (4) separating crude (I) from the waste acids at the reactor outlet; and (5) concentrating and recycling the acids to the nitration reaction.

Description

technical field [0001] The present invention relates to a continuous adiabatic process for the preparation of nitrochlorobenzene, wherein the spent acid produced during process practice is re-concentrated and recycled for use in the nitration reaction. By adding phosphoric acid it is possible to significantly increase the proportion of valuable o-nitrochlorobenzene product. Suppressing the production of the by-product p-nitrochlorobenzene is beneficial to the valuable product. Background technique [0002] Nitrochlorobenzene is an important intermediate in the preparation of dyes, medicines and pesticides. There is a particularly large demand for o-nitrochlorobenzene, which accounts for about 35% of the usual nitration of chlorobenzenes. p-Nitrochlorobenzene also has many industrial uses. Since m-nitrochlorobenzene has only very limited industrial applications, its products are generally undesirable. [0003] Industrially, nitrochlorobenzene is prepared by the nitration ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C205/11C07C201/08C07B61/00C07C205/12
CPCC07C205/12C07C201/08
Inventor R·德马思M·戈特塔T·林恩H·-M·韦伯E·泽恩吉贝尔
Owner LANXESS DEUTDCHLAND GMBH