Method for cleaning aqueous wastewater streams loaded with nitrobenzene

Patent metadata

Field	Value
Publication number	US-12129187-B2
Application number	US-202117996954-A
Country	US
Kind code	B2
Filing date	Apr 24, 2021
Priority date	Apr 27, 2020
Publication date	Oct 29, 2024
Grant date	Oct 29, 2024

Abstract

A process for purifying nitrobenzene-contaminated wastewater stream WW 1 includes stripping WW 1 with stripping gas SG 1 in a stripping column to obtain wastewater stream WW 2 containing reduced concentration of nitrobenzene relative to WW 1 (c NB,WW2 ), and purifying WW 2 in a wastewater treatment plant, wherein a target value (c NB,WW2,TARGET ) is specified for the nitrobenzene concentration in WW 2 . A set of linear mathematical relationships is stored in a database for a combination of boundary conditions of nitrobenzene concentration in WW 1 , temperature of WW 1 , and temperature of SG 1 . This set defines a range of concentrations of nitrobenzene in WW 2 and includes a mathematical relationship corresponding to c NB,WW2,TARGET , a mathematical relationship for a value of c NB,WW2 corresponding to 98% of c NB,WW2,TARGET , and a linear mathematical relationship for a value of c NB,WW2 corresponding to 102% of c NB,WW2,TARGET . The concentration of nitrobenzene is controlled in WW 2 (c NB,WW2 ) by adjusting the flow rate of SG 1.

First claim

The invention claimed is:

1. A process for purifying a wastewater stream WW 1 contaminated with nitrobenzene which contains nitrobenzene in a concentration c NB,WW1 , comprising:
(I) stripping WW 1 with a stripping gas SG 1 in a continuously operated stripping column to obtain a wastewater stream WW 2 which contains nitrobenzene in a concentration c NB,WW2 in which c NB,WW2 <c NB,WW1 and a stripping gas SG 2 laden with nitrobenzene, wherein WW 1 is supplied to the stripping column at a flow rate {dot over (m)} WW1 and a temperature T WW1 and SG 1 is supplied to the stripping column at a flow rate {dot over (m)} SG1 and a temperature T SG1 , and wherein c NB,WW2 is measured at a measuring point continuously or at intervals; and
(II) purifying WW 2 in a wastewater treatment plant to obtain a purified wastewater stream WW 3 which contains nitrobenzene in a concentration c NB,WW3 in which c NB,WW3 <c NB,WW2 ,
wherein c NB,WW2 does not exceed a predetermined maximum value c NB,WW2,MAX and a target value c NB,WW2,TARGET is specified for c NB,WW2 which is greater than zero and is specified to a value within a target range defined by the condition
0.50· c NB,WW2,MAX ≤c NB,WW2,TARGET ≤0.95· c NB,WW2,MAX ;

wherein the operation of the stripping column comprises:
(i) continuously supplying SG 1 and WW 1 to the stripping column, wherein for at least one combination of boundary conditions (a) c NB,WW1 , (b) the temperature T WW1 , and (c) the temperature T SG1 , a set of linear mathematical relationships corresponding to:
{dot over (m)} SG1 =x·{dot over (m)} WW1 ,

is stored in a database, each of which linear mathematical relationships corresponds to a concentration c NB,WW2 , so that the set of linear mathematical relationships defines a range of concentrations c NB,WW2 , wherein the set of linear mathematical relationships comprises, in addition to a mathematical relationship (0) which corresponds to c NB,WW2,TARGET , at least a first linear mathematical relationship (1) for a first value of c NB,WW2 , which corresponds to 98% of c NB,WW2,TARGET , and a second linear mathematical relationship (2) for a second value of c NB,WW2 , which corresponds to 102% of c NB,WW2,TARGET , and
wherein {dot over (m)} SG1 is selected for a flow rate {dot over (m)} WW1 (t i ) occurring at a time t i in such a way that {dot over (m)} SG1 is within a range of values ( AB ) that is generated by the first mathematical relationship (1) and the second mathematical relationship (2) at the flow rate {dot over (m)} WW1 (t i ) occurring at the time t i ; and
(ii) controlling c NB,WW2
by reducing {dot over (m)} SG1 in the event that an actual concentration c NB,WW2,ACTUAL of nitrobenzene in the wastewater WW 2 measured at the measuring point is equal to or less than 0.98·c NB,WW2,TARGET and
by increasing {dot over (m)} SG1 in the event that c NB,WW2,ACTUAL measured at the measuring point is equal to or less than 1.02·c NB,WW2,TARGET .

2. The process as claimed in claim 1 , wherein steam and/or nitrogen is used as the stripping gas.

3. The process as claimed in claim 1 , wherein a value for c NB,WW2 is determined independently at two or more measuring points and the obtained measured values are used to form an average which is used as the value for c NB,WW2,ACTUAL .

4. The process as claimed in claim 3 , wherein in the event of failure of one or more of the two or more measuring points, but not of all of the measuring points, only the at least one measuring point remaining functional is used, wherein the process comprises at least one such failure during the continuously performed stripping.

5. The process as claimed in claim 1 , wherein in the event of failure of each measuring point, the last value for the reduced or increased flow rate {dot over (m)} SG1 to be supplied to the stripping column according to the controlling of step (ii) that was determined from the measured value of a measuring point before its failure, is increased by 5% to 10% and maintained until at least one of the measuring points is functional again.

6. The process as claimed in claim 1 , wherein in step (i) {dot over (m)} SG1 is selected for {dot over (m)} WW1 (t i ) in such a way that {dot over (m)} SG1 is within a range of values that is generated by the mathematical relationship (0), which corresponds to c NB,WW2,TARGET , and the second mathematical relationship (2) at {dot over (m)} WW1 (t i ) occurring at the time t i .

7. The process as claimed in claim 1 , wherein in step (i) {dot over (m)} SG1 is selected {dot over (m)} WW1 (t i ) occurring at the time t i in such a way that {dot over (m)} SG1 is within a range of values that is generated by the mathematical relationship (0), which corresponds to c NB,WW2,TARGET , and the first mathematical relationship (1) at {dot over (m)} WW1 (t i ) occurring at the time t i .

8. The process as claimed in claim 1 , wherein the set of linear mathematical relationships includes a third linear mathematical relationship for a third value of c NB,WW2 , which corresponds to 99% of c NB,WW2,TARGET , and a fourth linear mathematical relationship for a fourth value of c NB,WW2 , which corresponds to 101% of c NB,WW2,TARGET , wherein in step (i) {dot over (m)} SG1 is selected for {dot over (m)} WW1 (t i ) occurring at the time t i in such a way that {dot over (m)} SG1 is within a range of values that is generated by the third mathematical relationship and the fourth mathematical relationship at {dot over (m)} WW1 (t i ) occurring at the time t i .

9. The process as claimed in claim 1 , wherein a set of linear mathematical relationships is stored for each of at least two combinations of boundary conditions of (a) c NB,WW1 , (b) T WW1 and (c) T SG1 , wherein at least T SG1 differs in the at least two combinations of boundary conditions.

10. The process as claimed in claim 1 , wherein the wastewater stream to be purified is obtained in the washing of a nitrobenzene phase, wherein the nitrobenzene phase is obtained by nitration of benzene with nitric acid in the presence of sulfuric acid followed by separation of an aqueous sulfuric acid phase.

11. The process as claimed in claim 10 , wherein the washing of the nitrobenzene phase comprises three stages, wherein the first stage comprises washing with water, the second stage comprises washing with an aqueous base solution and the third stage comprises washing with water, wherein wastewater is generated in each of the three stages and at least one of these is purified in the stripping column as WW 1 .

12. The process as claimed in claim 1 , wherein c NB,WW2,MAX is in the range from 2.0 ppm to 10 ppm based on the total mass of WW 2 .

13. The process as claimed in claim 1 , wherein c NB,WW2 is measured continuously or at intervals of not more than 6 hours.

Assignees

• Covestro Deutschland Ag

Inventors

• Rosin Thomas
• Drinda Peter
• Pilarczyk Klaus

Classifications

• C02F2101/38

  containing nitrogen · CPC title

• C02F1/10

  by direct contact with a particulate solid or with a fluid, as a heat transfer medium · CPC title

• B01D3/42

  Regulation; Control · CPC title

• B01D3/38

  Steam distillation · CPC title

• B01D3/346 Primary

  the gas being used for removing vapours, e.g. transport gas · CPC title