Process for workup of NOx-containing offgases from wastewater streams of nitration plants

Patent metadata

Field	Value
Publication number	US-9630866-B2
Application number	US-201013511256-A
Country	US
Kind code	B2
Filing date	Dec 13, 2010
Priority date	Dec 16, 2009
Publication date	Apr 25, 2017
Grant date	Apr 25, 2017

Abstract

The present invention relates to a process for workup of nitrite-comprising alkaline process wastewaters from the nitration of aromatic compounds, wherein the alkaline process wastewater is acidified by addition of acids and the offgas which comprises nitrogen oxides and escapes from the acidified process wastewater is worked up, comprising the steps of
a) acidifying the process wastewater by adding acid to a pH below 5, which forms an organic phase which separates out, an acidic aqueous phase and a gaseous NO x -containing phase, and b) removing the gaseous NO x -containing phase.

First claim

The invention claimed is:

1. A process for workup of an alkaline process wastewater obtained from a nitration of an aromatic compound to produce mono-, di- and tri-nitroaromatics, comprising:
(a) acidifying the alkaline process wastewater by adding acid to obtain a mixture with a pH below 5, which forms an organic phase which separates out, an acidic aqueous phase, and a gaseous NO x -containing phase, and
(b) removing the gaseous NO x -containing phase,
wherein the acid in (a) is a concentrated sulfuric acid obtained from the workup of an aqueous sulfuric acid-containing phase obtained in the nitration, wherein the concentrated sulfuric acid has a sulfuric acid concentration of 85% to 95% by weight.

2. The process of claim 1 , wherein the NO x formed in the course of acidification in step (a) are stripped out of the organic and acidic aqueous phases by an inert gas and converted to the gaseous phase.

3. The process of claim 1 , wherein the NO x formed in the course of acidification in (a) are stripped out of the organic and acidic aqueous phases by nitrogen, mixtures of nitrogen and oxygen, air or carbon dioxide and converted to the gaseous NO x -containing phase.

4. The process of claim 1 , wherein the alkaline process wastewater originates from the scrubbing of a crude product from the nitration with aqueous alkali metal carbonate or alkali metal hydrogencarhonate solution, and nitrogen oxides are stripped out of the organic and acidic aqueous phases by the carbon dioxide formed in the course of acidification of the alkaline process wastewater and converted to the gaseous NO x -containing phase.

5. The process of claim 1 , wherein the aromatic compound to be nitrated is benzene, toluene, xylene, chlorobenzene or dichlorobenzene.

6. The process of claim 1 , wherein the alkaline process wastewater is acidified at a temperature of 20 to 90° C.

7. The process of claim 6 , wherein the temperature is from 55 to 70° C.

8. The process of claim 1 , wherein (b) is performed before further treatment of the organic and aqueous phases.

9. The process of claim 1 , wherein the acidic aqueous phase is extracted with a solvent after removal of the organic phase.

10. The process of claim 1 , wherein the acidic aqueous phase, after removal of the organic phase, is sent to an ozonolysis, a thermolysis or a biological wastewater treatment.

11. The process of claim 1 , further comprising, after (b):
(c) further processing of the NO x present in the gaseous NO x -containing phase removed to produce nitric acid.

12. The process of claim 11 , wherein the gaseous NO x -containing phase removed is supplied in (c), without prior purification and removal of other gas constituents, directly to an absorption column for nitric acid production.

13. The process of claim 11 , wherein the nitric acid obtained in (c) is recycled into the nitration of the aromatic compounds.

14. The process of claim 1 , wherein the NO x -containing phase removed after (b) is sent to an incineration.

15. The process of claim 1 , wherein the alkaline process wastewater contains nitrites and the amount of nitrites is lowered by 90% to 99% after (a) and (b).

16. The process of claim 1 , wherein the concentrated sulfuric acid has a sulfuric acid concentration of 90% to 93% by weight.

17. In a process of nitrating an aromatic compound, wherein an alkaline process wastewater is obtained from the nitration and a concentrated sulfuric acid phase is obtained from a distillation of an aqueous phase produced in the nitration, the improvement comprising (a) acidifying the alkaline process wastewater with the concentrated sulfuric acid phase to produce an aqueous phase, an organic phase and a gaseous NO x -containing phase and (b) removing the gaseous NO x -containing phase.

Assignees

• Fritz Ruediger
• Hempel Renate
• Zoellinger Michael
• Allardt Holger
• Reetz Reiner
• Basf Se

Inventors

• Fritz Ruediger
• Hempel Renate
• Zoellinger Michael
• Allardt Holger
• Reetz Reiner

Classifications

• C02F9/00 Primary

  Multistage treatment of water, waste water or sewage · CPC title

• C01B21/40

  Preparation by absorption of oxides of nitrogen {(C01B21/26 takes precedence)} · CPC title

• C02F1/20

  by degassing, i.e. liberation of dissolved gases (degasification of liquids in general B01D19/00; arrangement of degassing apparatus in boiler feed supply F22D) · CPC title

• C02F2209/06

  pH · CPC title

• C07C201/08

  by substitution of hydrogen atoms by nitro groups · CPC title