Process for working up waste water from nitrobenzene preparation

Patent metadata

Field	Value
Publication number	US-9771291-B2
Application number	US-201414784699-A
Country	US
Kind code	B2
Filing date	Apr 14, 2014
Priority date	Apr 18, 2013
Publication date	Sep 26, 2017
Grant date	Sep 26, 2017

Abstract

The invention relates to a process for working up alkaline waste water which is formed during washing of crude nitrobenzene obtained by nitration of benzene, wherein
(i) the alkaline waste water is heated under an increased pressure with respect to atmospheric pressure with exclusion of oxygen and is then cooled and expanded; (ii) the waste water obtained in (i) is purified further by stripping with a stripping gas and the stripping gas stream loaded with impurities is then cooled to a temperature of from 10° C. to 60° C.; and (iii) the liquid process product obtained in (ii) by cooling the stripping gas stream loaded with impurities is separated into an aqueous and an organic phase and the organic phase is used further in an aniline production process.

First claim

The invention claimed is:

1. A process for working up alkaline waste water which is formed during washing of crude nitrobenzene obtained by nitration of benzene, comprising:
(i) heating the alkaline waste water to a temperature of from 150° C. to 500° C. under an increased pressure with respect to atmospheric pressure with exclusion of oxygen, wherein the heated alkaline waste water is then cooled and expanded;
(ii) further purifying the waste water obtained in (i) by stripping with a stripping gas and then cooling the stripping gas stream loaded with impurities is then cooled to a temperature of from 10° C. to 60° C.; and
(iii) separating the liquid process product obtained in (ii) into an aqueous and an organic phase and further using the organic phase obtained thereby in an aniline production process.

2. The process of claim 1 , comprising sending the organic phase obtained in step (iii) to the educt stream of an aniline production plant.

3. The process of claim 1 , comprising sending the organic phase obtained in step (iii) to the product stream of an aniline production plant.

4. The process of claim 1 , comprising heating of the alkaline waste water in step (i) under an absolute pressure of from 50 bar to 350 bar.

5. The process of claim 1 , comprising heating the alkaline waste water in step (i) is carried out for a period of from 5 minutes to 120 minutes.

6. The process of claim 1 , comprising, after the heating, cooling the alkaline waste water to a temperature of from 60° C. to 100° C.

7. The process of claim 1 , comprising partially recycling the aqueous phase obtained in step (iii) into the stripping of step (ii) and sending the remaining part which is not recycled to a biological treatment plant without further purification steps.

8. The process of claim 1 , in which the alkaline waste water used in step (i) originates from step c) or step d) of the following process steps:
a) nitration of benzene with nitric acid or a mixture of nitric acid and sulfuric acid and separating off of the aqueous phase;
b) washing of the organic process product obtained in step a);
c) alkaline washing of the washed organic process product obtained in step b); and
d) optional separation of benzene and/or nitrobenzene out of the alkaline waste water obtained in step c).

9. The process of claim 8 , in which in the alkaline wash in step c) the base is used in an excess of from 0.5% to 5.0% of theory, based on the nitrophenols contained in the waste water after step b).

Assignees

• Covestro Deutschland Ag

Inventors

• Knauf Thomas
• Mairata Antoni
• Sluyts Erik
• Van Tricht Jan

Classifications

• 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

• C02F2301/046

  Recirculation with an external loop · CPC title

• C07C205/06

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

• C07C209/36

  by reduction of nitro groups bound to carbon atoms of six-membered aromatic rings {in presence of hydrogen-containing gases and a catalyst} · CPC title

• C02F2101/322

  Volatile compounds, e.g. benzene · CPC title