Exhaust gas cleaning in a method for continuously producing dinitrotoluene

Patent metadata

Field	Value
Publication number	US-9896407-B2
Application number	US-201515514107-A
Country	US
Kind code	B2
Filing date	Sep 29, 2015
Priority date	Oct 2, 2014
Publication date	Feb 20, 2018
Grant date	Feb 20, 2018

Abstract

The invention relates to a method for producing dinitrotoluene, comprising the following steps: a) nitrating toluene with a mixture of nitric acid and sulfuric acid and subsequently separating a sulfuric-acid-containing aqueous phase that arises in the nitration, wherein a raw dinitrotoluene is obtained, b) washing the raw dinitrotoluene in a water wash with neutral and/or alkaline washing water, wherein a pre-cleaned dinitrotoluene, which contains at least water in addition to dinitrotoluene, is obtained after the washing water used in the last wash has been separated, and c) separating the water from the pre-cleaned dinitrotoluene, d) collecting the waste water from steps a), b), and/or c), e) optionally extracting the collected waste water from step d) with toluene and returning the thus obtained organic phase to step a), f) freeing the collected waste water from step d), or, if the optional step e) is performed, the extracted waste water from step e), of toluene in a toluene stripper, wherein a toluene-containing exhaust gas flow is obtained, g) feeding at least one exhaust gas flow from steps a), b), c), d), e), or f) into an exhaust gas condenser and removing the toluene contained in the at least one exhaust gas flow in said exhaust gas condenser, wherein the method comprises the following further step: h) feeding the exhaust gas flow arising in step g) after the condensing out of the toluene to a thermal exhaust air cleaning, wherein nitrogen is added to the exhaust gas flow to be fed to the exhaust gas condenser or to the exhaust gas flow leaving the exhaust gas condenser, wherein preferably a nitrogen concentration in the exhaust gas flow of at least 0.1 vol % is set, especially preferably of at least 0.5 vol %.

First claim

The invention claimed is:

1. A process for producing dinitrotoluene, comprising:
a) nitrating toluene with a mixture of nitric acid and sulfuric acid with subsequent separation of a sulfuric-acid-containing aqueous phase formed during the nitration to obtain a crude dinitrotoluene,
b) washing the crude dinitrotoluene in a water wash with neutral and/or alkaline washing water, wherein after separation of the washing water employed in the last wash a prepurified dinitrotoluene is obtained which comprises not only dinitrotoluene but also at least water,
c) separating the water from the prepurified dinitrotoluene,
d) collecting the wastewaters from steps a), b) and/or c),
e) optional extraction of the collected wastewaters from step d) with toluene and recycling of the thus obtained organic phase into step a),
f) freeing the collected wastewaters from step d) or, if optional step e) is performed, the extracted wastewater from step e) of toluene in a toluene stripper to obtain a toluene-containing offgas stream,
g) supplying at least one offgas stream from steps a), b), c), d), a) or f) into an offgas condenser and removing the toluene present in the at least one offgas stream in this offgas condenser, and
h) supplying the offgas stream generated in step g) after the condensing-out of the toluene to a thermal exhaust air purification, wherein nitrogen is added to the offgas stream to be supplied to the offgas condenser or to the offgas stream leaving the offgas condenser.

2. The process as claimed in claim 1 , wherein in step g) the offgas stream from step f) is supplied to the offgas condenser and all offgas streams from steps a), b) and C) and also optionally d) and optionally e) are combined and fed either into the offgas stream from step g) that is to be supplied to the offgas condenser or into the offgas stream leaving the offgas condenser.

3. The process of claim 1 , wherein the nitration of toluene in step a) is performed in a continuous, two-stage process, wherein in the first stage a crude mononitrotoluene is obtained which in the second stage is converted into the crude dinitrotoluene.

4. The process of claim 1 , wherein the washing of the crude dinitrotoluene in step b) is effected such that initially neutral, then alkaline and finally neutral washing water is employed.

5. The process of claim 1 , wherein the separation in step c) is accomplished in a storage tank comprising a separator.

6. The process of claim 1 , wherein an absolute pressure in the range from 10 mbar to 1200 mbar, is established in the offgas condenser in step g).

7. The process of claim 1 , wherein a temperature of 20° C. to 75° C. is established in the offgas condenser in step g).

8. The process of claim 1 , wherein the toluene condensed out in step g) is supplied to the nitration in step a).

9. The process of claim 1 , wherein the offgas stream to be supplied to the offgas condenser or the offgas stream leaving the offgas condenser is freed of nitrogen oxides.

10. The process of claim 1 , wherein after the separation in step a) the sulfuric-acid-containing aqueous phase is purified and optionally concentrated and/or recycled.

11. The process of claim 1 , wherein a nitrogen concentration in the offgas stream of at least 0.1 vol % is established.

12. The process of claim 11 , wherein the nitrogen concentration in the offgas stream is at least 0.5 vol %.

13. The process of claim 6 , wherein the absolute pressure is in the range of 100 mbar to 1150 mbar.

14. The process of claim 7 , wherein the temperature is 25° C to 60° C.

15. The process of claim 14 , wherein the temperature is 30° C. to 45° C.

Assignees

• Covestro Deutschland Ag

Inventors

• Knauf Thomas
• Muennig Juergen
• Lorenz Wolfgang
• Pennemann Bernd

Classifications

• C07C205/06

  having nitro groups bound to carbon atoms of six-membered aromatic rings · CPC title

• C07C201/16

  Separation; Purification; Stabilisation; Use of additives · CPC title

• C07C201/08 Primary

  by substitution of hydrogen atoms by nitro groups · CPC title

• B01D2257/7027

  Aromatic hydrocarbons · CPC title

• B01D53/002 Primary

  by condensation · CPC title