PROCESS FOR CONCENTRATING DILUTED SULFURIC ACID

Abstract

The invention relates to a process for concentrating diluted sulfuric acid (10) which may comprise at least one nitroaromatic compound and/or nitric acid as impurities, comprising: (a) feeding the diluted sulfuric acid (10) into a first stage (1) in which low boilers are removed by evaporation and/or stripping to obtain a first concentrated sulfuric acid (12); (b) optionally feeding the first concentrated sulfuric acid (12) into a second evaporation stage (2) to obtain a second concentrated sulfuric acid (14); (c) feeding the second concentrated sulfuric (14) acid into a third evaporation stage (3) if step (b) is carried out, or feeding the first concentrated sulfuric acid (12) into the third evaporation stage (3) if step (b) is not carried out, to obtain concentrated sulfuric acid (16) as product, wherein an oxidizing agent (17) and/or a precursor of an oxidizing agent is fed into the third evaporation stage (3).

Claims

1.-15. (canceled)

16. A process for concentrating diluted sulfuric acid which may comprise at least one nitroaromatic compound and/or nitric acid as impurities, comprising: (a) feeding the diluted sulfuric acid into a first stage in which low boilers are removed by evaporation and/or stripping to obtain a first concentrated sulfuric acid; (b) optionally feeding the first concentrated sulfuric acid into a second evaporation stage to obtain a second concentrated sulfuric acid; (c) feeding the second concentrated sulfuric acid into a third evaporation stage if step (b) is carried out, or feeding the first concentrated sulfuric acid into the third evaporation stage if step (b) is not carried out, to obtain concentrated sulfuric acid as product, wherein an oxidizing agent and/or a precursor of an oxidizing agent is fed into the third evaporation stage.

17. The process according to claim 16, wherein at least one of the at least one nitroaromatic compound is mononitrotoluene and/or dinitrotoluene.

18. The process according to claim 16, wherein the oxidizing agent is selected from the group consisting of nitric acid, nitrous acid, nitrosylsulfonic acid and combinations thereof, and/or the precursor of the oxidizing agent is sodium nitrite.

19. The process according to claim 16, wherein the amount of oxidizing agent is in the range from 0.01 to 100 g per kg concentrated sulfuric acid.

20. The process according to claim 16, wherein the first stage comprises an evaporation which is operated at a temperature in the range from 130 to 200 C. and a pressure in the range from 800 to 1200 mbar(abs).

21. The process according to claim 16, wherein the second evaporation stage is operated at a pressure in the range from 10 to 800 mbar (abs) and a temperature in the range from 120 to 200 C.

22. The process according to claim 16, wherein the second evaporation stage, if carried out, comprises 1 to 5 evaporation units.

23. The process according to claim 16, wherein the third evaporation stage is operated at a pressure in the range from 10 to 800 mbar (abs) and a temperature in the range from 180 to 300 C.

24. The process according to claim 16, wherein the third evaporation stage comprises 1 to 5 evaporation units.

25. The process according to claim 16, wherein the evaporation units used in the third evaporation stage are circulation evaporators, horizontal evaporators or falling film evaporators.

26. The process according to claim 16, wherein the oxidizing agent and/or the precursor of the oxidizing agent is fed into an evaporation loop.

27. The process according to claim 16, wherein the oxidizing agent and/or the precursor of the oxidizing agent is mixed with the second concentrated sulfuric acid if step (b) is carried out, or with the first concentrated sulfuric acid if step (b) is not carried out before feeding into the third evaporation stage.

28. The process according to claim 16, wherein the diluted sulfuric acid has a concentration in the range from 60 to 85 wt %.

29. The process according to claim 16, wherein the concentrated sulfuric acid has a concentration in the range from 80 to 99 wt %.

30. The process according to claim 16, wherein the diluted sulfuric acid is obtained in a process for producing nitrotoluene and wherein the concentrated sulfuric acid is recycled into the process for producing nitrotoluene.

Description

EXAMPLE 1

[0071] Diluted sulfuric acid comprising 71 wt % sulfuric acid, 1 wt % nitric acid, 0.5 wt % dinitrotoluene and the remainder being water was fed into a first evaporation stage having a feed temperature of 135 C. The first evaporation stage was operated at a pressure of 1 bar and a bottom temperature of 180 C.

[0072] The thus obtained first concentrated sulfuric acid was withdrawn at the bottom of the first evaporation stage and fed into a second evaporation stage having a feed temperature of 180 C. The second evaporation stage was operated at a pressure of 0.09 bar and a bottom temperature of 160 C. At the bottom of the second evaporation stage a second concentrated sulfuric acid was obtained which then was fed into the third evaporation stage with a feed temperature of 160 C. The third evaporation stage was operated at a pressure of 0.09 bar and a bottom temperature of 210 C. and the concentrated sulfuric acid obtained in the bottom of the third evaporation stage was withdrawn as product.

[0073] 5 g of 99.8% nitric acid per kg feed stream were added into the third stage as oxidizing agent.

[0074] The TOC of the product was 0.015, the density of the product 1.837 g/ml and the concentration of the sulfuric acid 96 wt %. No solids were observed in the product and the product was colorless.

Example 2

[0075] Diluted sulfuric acid comprising 71 wt % sulfuric acid, 1 wt % nitric acid, 0.5 wt % dinitrotoluene and the remainder being water was fed into a first evaporation stage having a feed temperature of 135 C. The first evaporation stage was operated at a pressure of 1 bar and a bottom temperature of 180 C.

[0076] The thus obtained first concentrated sulfuric acid was withdrawn at the bottom of the first evaporation stage and fed into a second evaporation stage having a feed temperature of 180 C. The second evaporation stage was operated at a pressure of 0.09 bar and a bottom temperature of 160 C. At the bottom of the second evaporation stage a second concentrated sulfuric acid was obtained which then was fed into the third evaporation stage with a feed temperature of 160 C. The third evaporation stage was operated at a pressure of 0.09 bar and a bottom temperature of 180 C. and the concentrated sulfuric acid obtained in the bottom of the third evaporation stage was withdrawn as product.

[0077] In this example, 5 g of 99.8% nitric acid per kg feed stream were added into the third stage as oxidizing agent.

[0078] The TOC of the product was 0.042, the density of the product 1.823 g/ml and the concentration of the sulfuric acid 94 wt %. No solids were observed in the product and the product was colorless.

Example 3

[0079] Diluted sulfuric acid comprising 71 wt % sulfuric acid, 1 wt % nitric acid, 0.5 wt % dinitrotoluene and the remainder being water was fed into a first evaporation stage having a feed temperature of 135 C. The first evaporation stage was operated at a pressure of 1 bar and a bottom temperature of 180 C.

[0080] The thus obtained first concentrated sulfuric acid was withdrawn at the bottom of the first evaporation stage and fed into the third evaporation stage having a feed temperature of 180 C. The third evaporation stage was operated at a pressure of 0.09 bar and a bottom temperature of 210 C. and the concentrated sulfuric acid obtained in the bottom of the third evaporation stage was withdrawn as product.

[0081] In this example, 5 g of 99.8% nitric acid per kg of the feed stream were added into the third stage as oxidizing agent.

[0082] The TOC of the product was 0.024, the density of the product 1.826 g/ml and the concentration of the sulfuric acid 95 wt %. No solids were observed in the product and the product was colorless.