Method for the continuous production of nitrobenzene

Patent metadata

Field	Value
Publication number	US-9227909-B2
Application number	US-201314046068-A
Country	US
Kind code	B2
Filing date	Oct 4, 2013
Priority date	Oct 10, 2012
Publication date	Jan 5, 2016
Grant date	Jan 5, 2016

Abstract

The present invention relates to a method for producing nitrobenzene, in which the waste gas streams accruing in the process and containing benzene and (traces of) nitrobenzene, possibly low- and medium-boiling components, possibly non-condensable gases and possibly water, optionally after removal of nitrogen oxides, are scrubbed in an absorption column with nitrobenzene, which comprises only very small amounts (maximum 50 ppm) of benzene and is distributed by means of a liquid distributor at a rate of 50 to 200 drip points per square meter, preferably 60 to 120 drip points per square meter, wherein (i) a liquid stream containing benzene and nitrobenzene, possibly organic low- and medium-boiling components and additionally containing sulfuric acid if sulfuric acid is used as the scrubbing agent and (ii) waste gas depleted in benzene and possibly in organic low- and medium-boiling components are obtained. A waste gas purified by the method according to the invention is particularly suitable for burning in a thermal exhaust air treatment process.

First claim

What is claimed is:

1. A method for producing nitrobenzene, comprising
a) nitrating benzene with nitric acid or mixtures of nitric acid and sulfuric acid and subsequent phase separation into an aqueous phase and crude nitrobenzene,
b) scrubbing the crude nitrobenzene from step a) with an aqueous scrubbing solution in at least three scrubbing stages, each stage followed by separation of the scrubbing solution wherein following separation of the scrubbing solution used in the final scrubbing stage a pre-purified nitrobenzene mixture is obtained which comprises at least benzene and water in addition to nitrobenzene,
c) removing benzene and water from the pre-purified nitrobenzene mixture from step b) by distillation in a distillation apparatus to give purified nitrobenzene,

wherein waste gas streams accrue in steps a) to c) which contain benzene and nitrobenzene, and
d) scrubbing the waste gas streams countercurrently in an absorption column with nitrobenzene, which has a benzene content of <50 ppm, relative to the total mass of nitrobenzene, and is distributed by means of a liquid distributor at a rate of 50 to 200 drip points per square meter, wherein (i) a liquid stream containing benzene and nitrobenzene and (ii) a nitrobenzene-depleted waste gas are obtained.

2. The method according to claim 1 , wherein step d) is performed under an absolute pressure of about 900 mbar to about 980 mbar.

3. The method according to one of claims 1 or 2 , wherein purified nitrobenzene from step c) is used as the scrubbing solution in step d).

4. The method according to claim 3 , wherein the distillation in step c) is operated under an absolute pressure at the top of the distillation column of about 220 mbar to about 480 mbar and at a temperature at the bottom of the distillation column of about 100° C. to about 200° C.

5. The method according to claim 3 , wherein the distillation in step c) is operated under an absolute pressure at the top of the distillation column of about 270 mbar to about 430 mbar and at a temperature at the bottom of the distillation column of about 120° C. to about 190° C., and wherein the purified nitrobenzene used as the scrubbing solution in step d) has a benzene content of <20 ppm, relative to the total mass of purified nitrobenzene.

6. The method according to claim 3 , wherein the distillation in step c) is operated under an absolute pressure at the top of the distillation column of about 320 mbar to about 380 mbar and at a temperature at the bottom of the distillation column of about 160° C. to about 180° C., and wherein the purified nitrobenzene used as the scrubbing solution in step d) has a benzene content of <10 ppm, relative to the mass of purified nitrobenzene.

7. The method according to one of claims 3 to 6 , wherein the nitrobenzene from step c) used as the scrubbing solution in step d) has a temperature of about 20° C. to about 75° C.

8. The method according to one of claims 1 to 7 , wherein the absorption column is operated in such a way that the gaseous vapours that are discharged have a temperature of about 20° C. to about 75° C.

9. The method according to one of claims 1 to 8 , wherein the liquid distributor used in step d) has a drip point density of about 60 to about 120 drip points per square meter.

10. The method according to one of claims 1 to 9 , further comprising
e) distilling the liquid stream obtained in step d) so as to obtain a liquid selected from the group consisting of benzene, nitrobenzene and a mixture of benzene and nitrobenzene.

11. The method according to claim 10 , further comprising
f) returning the mixture of benzene and nitrobenzene to step b.

Assignees

• Bayer Materialscience Ag
• Covestro Deutschland Ag

Inventors

• Knauf Thomas
• Munnig Jurgen
• Schmiedler Joerg

Classifications

• C07C201/08 Primary

  by substitution of hydrogen atoms by nitro groups · CPC title

• C07C201/16

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

• C07C205/06

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