Process for working up the waste water obtained in the preparation of dinitrotoluene
View Patent ↗The present invention relates to a process for working up or treating aqueous waste waters which are formed during the nitration of toluene to dinitrotoluene with nitrating acid. These aqueous waste waters containing acidic wash water and alkaline wash water from the dinitrotoluene washing step, and distillate from the sulfuric acid concentration step. The process comprises, a) combining the acidic and alkaline waste waters from the washing step and the aqueous distillate from the sulfuric acid concentration step such that the resulting mixture has a pH below 5, b) separating the aqueous and organic phases which are formed by phase separation, c) subjecting the aqueous phase from b) to an extraction step, wherein d) the organic components contained in the aqueous phase from c) are extracted with toluene, and e) introducing the toluene phase enriched with the organic components into the toluene nitration.
1. A process for treating aqueous waste waters formed during the nitration of toluene to dinitrotoluene with nitrating acid, wherein the aqueous waste waters comprise the acidic wash water and alkaline wash water from the dinitrotoluene washing step and the distillate from the sulfuric acid concentration step, comprising
a) combining (1) the acidic and alkaline waste waters from the washing step and (2) the aqueous distillate from the sulfuric acid concentration step such that the resultant mixture has a pH below 5,
b) separating the resultant aqueous and organic phases by phase separation,
c) extracting the organic components present in the aqueous phase resulting from b) with toluene, and
d) introducing the toluene phase enriched with the organic components into the toluene nitration.
2. The process of claim 1 , wherein a) combining of the aqueous waste waters is in a mixer with a venting facility.
3. The process of claim 1 , additionally comprising mixing the combined aqueous phases with mononitrotoluene.
4. The process of claim 1 , additionally comprising recycling the organic phase from b) into the nitration process.
5. The process of claim 1 , wherein the aqueous phase from step b) is mixed with toluene in a static mixer before c) extracting the organic components.
6. The process of claim 1 , wherein the aqueous phase from b) and toluene are introduced into c) in countercurrent fashion for said extraction step and are present in a weight ratio of toluene to aqueous phase of 33:100 to 5:100.
7. The process of claim 1 , wherein c) extracting the organic components with toluene is carried out in stirred multistage extraction columns.
8. The process of claim 1 , additionally comprising steam stripping the aqueous phase resulting from said extraction, thereby removing the toluene from the aqueous phase to yield a water/toluene mixture.
9. The process of claim 8 , wherein the steam stripping is carried out with a stripper column provided with structured or random packing or plates, and the aqueous phase in introduced into the top of the stripper column and the steam is fed into the lower region of the column.
10. The process of claim 8 , additionally comprising recycling the resultant water/toluene mixture c) the extraction or into the nitration process.