IP Library Granted Patent US 12,441,614
Granted Patent B2
US 12,441,614 · App. 17/783,375 · Granted Oct 14, 2025

Method of cleaning an apparatus used in the concentration of a mineral acid

Inventors: Bernd Pennemann (Bergisch Gladbach, DE); Kameh Tajvidi (Neuss, DE)
Assignee: Covestro Deutschland AG
C01B17/88B01B1/005B01D3/148B01D53/263B01D53/28C01B21/44C07C201/08F28G9/00
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Quick Facts
Patent No.
US 12,441,614
App. No.
17/783,375
Granted
Oct 14, 2025
Kind
B2
Abstract

The present invention relates to a method for preparing an apparatus (or a plant comprising a plurality of apparatuses), for example a heat exchanger, a vaporizer or a distillation column, for use in a process (in particular a continuously operated process) for concentrating a mineral acid by evaporation of water, wherein the apparatus or the plant comprises (at least) a device which is resistant to the mineral acid and the device is flushed with an aqueous alkali metal hydroxide solution having a concentration by mass of alkali metal hydroxide in the range from 1% to 30% at a temperature in the range from 40° C. to 90° C. for a time of from 2 hours to 7 days.

Claims (21)

1. A method for preparing and using an apparatus comprising an acid-resistant device,

wherein the acid-resistant device has a coating comprising steel enamel, silicon carbide, glass, tantalum, niobium, a perfluorinated polymer, or a composite of two or more thereof,

or

wherein the acid-resistant device is made of one of steel enamel, silicon carbide, glass, tantalum, niobium, a perfluorinated polymer, or a composite of two or more thereof,

the method comprising:

(a) flushing the acid-resistant device with an aqueous alkali metal hydroxide solution having a concentration by mass of alkali metal in the range from 1% to 30% at a temperature in the range from 40° C. to 90° C. for a time of from 2 hours to 7 days; and then subsequently

(b) using the apparatus comprising the acid-resistant device flushed in step (a) in a process of concentrating a mineral acid by evaporation of water, wherein said process comprises contacting the acid-resistant device with the mineral acid during the concentrating of the mineral acid or wherein said process comprises contacting the acid-resistant device with the mineral acid while the mineral acid has a concentration that was increased as a result of said concentrating of the mineral acid.

2. The method as claimed in claim 1 , wherein the alkali metal hydroxide solution comprises sodium hydroxide solution, potassium hydroxide solution, or a mixture thereof.

3. The method as claimed in claim 1 , wherein the flushing is carried out for a time of from 8 hours to 30 hours.

4. The method as claimed in claim 1 , wherein the acid-resistant device comprises a heat exchanger for heating the mineral acid, a distillation apparatus for removing organic compounds from the mineral acid, a vaporization apparatus, a heat exchanger for cooling the mineral acid after the mineral acid has been concentrated and/or a vessel for accommodating the mineral acid after the mineral acid has been concentrated.

5. The method as claimed in claim 4 , wherein the acid-resistant device is a heat exchanger which is designed for heating the mineral acid and/or for cooling the mineral acid after the mineral acid has been concentrated.

6. The method as claimed in claim 4 , wherein the acid-resistant device comprises a heat exchanger for cooling the mineral acid after the mineral acid has been concentrated and a vessel downstream thereof for accommodating the mineral acid after the mineral acid has been concentrated.

7. The method as claimed in claim 1 , wherein the mineral acid comprises sulfuric acid, nitric acid, or a mixture thereof.

8. The method as claimed in claim 7 , wherein the process of concentrating the mineral acid by evaporation of water comprises concentrating sulfuric acid that is used as a catalyst and diluent in a nitration of an aromatic compound with nitric acid to obtain an aromatic nitro compound.

9. The method as claimed in claim 8 , wherein the aromatic nitro compound comprises nitrobenzene or dinitrotoluene.

10. The method as claimed in claim 7 , wherein the process of concentrating the mineral acid by evaporation of water is used for concentrating sulfuric acid that has been diluted by use of the sulfuric acid as a desiccant for drying a gas.

11. The method as claimed in claim 10 , wherein the gas comprises chlorine.

12. The method as claimed in claim 1 , wherein the acid-resistant device comprises a coating comprising a perfluorinated polymer or wherein the acid-resistant device is made at least partly of a perfluorinated polymer, where the perfluorinated polymer is mechanically stabilized with an inert material.

13. The method as claimed in claim 1 , wherein the acid-resistant device comprises a coating comprising steel enamel, silicon carbide, glass, niobium and/or tantalum or wherein the acid-resistant device is made at least partly of steel enamel, silicon carbide, glass, niobium and/or tantalum.

14. The method as claimed in claim 1 , wherein the acid-resistant device is not disassembled for the purpose of carrying out the flushing.

15. The method as claimed in claim 14 , wherein the apparatus is not disassembled for the purpose of carrying out the flushing of the acid-resistant device.

Assignments (2)
MERGER Recorded Oct 29, 2024
From: COVESTRO INTELLECTUAL PROPERTY GMBH & CO. KG
To: COVESTRO DEUTSCHLAND AG
Reel/Frame 069272/0414 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 21, 2022
From: PENNEMANN, BERND; TAJVIDI, KAMEH
To: COVESTRO INTELLECTUAL PROPERTY GMBH & CO. KG
Reel/Frame 060578/0555 →
Priority Claims (1)
EP 19217596 · Dec 18, 2019 · regional
Continuity (1)
Related Publication 20230016848A1 · Jan 19, 2023
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