IP Library Granted Patent US 9,994,472
Granted Patent B2
US 9,994,472 · App. 15/296,421 · Granted Jun 12, 2018

Treatment of the wastewater from isophorone production comprising neutralization, filtration and a downstream chemical oxidation process and subsequent reduction

Inventors: Yue Chang (Darmstadt, DE); Manfred Kreczinski (Herne, DE); Martin Maier (Herne, DE); Matthias Woyciechowski (Langenselbold, DE)
Assignee: Evonik Degussa GmbH
C02F9/00B01D61/00C02F1/004C02F1/66C02F1/70C02F1/76B01D2325/02C02F1/44C02F2101/34C02F2103/36C02F2209/02C02F2209/06C02F2303/185
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Quick Facts
Patent No.
US 9,994,472
App. No.
15/296,421
Granted
Jun 12, 2018
Kind
B2
Abstract

Treatment of the wastewater from isophorone production comprising neutralization, filtration and a downstream chemical oxidation process and subsequent reduction. The invention relates to treatment of the wastewater from isophorone (IP) production comprising neutralization, filtration and a downstream chemical oxidation process and subsequent reduction.

Claims (18)

1. A method of treating the wastewater from isophorone production by

A) neutralization of the alkaline wastewater from isophorone production to a pH of 6.5 to 8.5;

B) filtration of the mixture of liquid and solids obtained from the neutralization;

C) oxidation of the filtrate obtained from the filtration;

D) reduction of an oxidant in the wastewater from the oxidation C).

2. The method according to claim 1 , wherein the neutralization A) is carried out by an in-line method or by a stationary neutralization method.

3. The method according to claim 1 , wherein the neutralization A) is carried out by a stationary neutralization method, wherein the acids are admixed to the wastewater in a container using a stirrer.

4. The method according to claim 1 , wherein the neutralization A) is carried out at atmospheric pressure in the temperature range of 20-40° C. and at pH 7 to 7.5.

5. The method according to claim 1 , wherein in the neutralization A) the metering of acids is effected in two stages such that the first metering stage is carried out with concentrated acid just above the vertex of the pH lowering which as per the operating state is between pH 11-10.5 and in the second metering stage dilute acid is then used to slowly approach pH 7-7.2.

6. The method according to claim 1 , wherein in the neutralization A) the metering of acids is effected in two stages such that the first metering stage is carried out with 90-96 wt % H 2 SO 4 or 30-35 wt % HCl just above the vertex of the pH lowering which as per the operating state is between pH 11-10.5 and in the second metering stage preferably 5-15 wt % H 2 SO 4 or 5-10 wt % HCl is then used to slowly approach pH 7-7.2.

7. The method according to claim 1 , wherein the filtration B) is carried out at atmospheric pressure or superatmospheric pressure at temperatures of 15° C. to 45° C.

8. The method according to claim 1 , wherein the filtration B) is carried out at atmospheric pressure at temperatures of 20° C. to 30° C. using a filter with a pore size below 10 μm, in particular of 1 μm.

9. The method according to claim 1 , wherein the reaction pH range during the oxidation C) varies between pH 7-8 and the reaction temperature varies between 20-45° C.

10. The method according to claim 1 , wherein the oxidation C) is carried out by a 5-15 wt % solution comprising at least one oxidant.

11. The method according to claim 1 , wherein the oxidation is carried out by a 5-15 wt % solution comprising sodium hypochlorite.

12. The method according to claim 1 , wherein the oxidation C) is carried out in continuous fashion as a multistage through-flow process.

13. The method according to claim 1 , wherein the oxidant is reduced with Na 2 SO 3 in step D).

14. The method according to claim 1 , wherein wastewaters from the production of isophoronenitrile (IPN) and/or isophoronediamine (IPDA) are fed with the isophorone wastewater from step B) into the oxidation C), the oxidation being effected at pH>9.5.

Assignments (2)
CHANGE OF NAME Recorded Nov 18, 2019
From: EVONIK DEGUSSA GMBH
To: EVONIK OPERATIONS GMBH
Reel/Frame 051045/0872 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 28, 2017
From: CHANG, YUE; KRECZINSKI, MANFRED; MAIER, MARTIN; WOYCIECHOWSKI, MATTHIAS
To: EVONIK DEGUSSA GMBH
Reel/Frame 041400/0001 →
Priority Claims (1)
EP 15190324 · Oct 19, 2015 · regional
Continuity (1)
Related Publication 20170107133A1 · Apr 20, 2017