Device and process for producing hydrogen peroxide by an anthraquinone process

Patent metadata

Field	Value
Publication number	US-11912571-B2
Application number	US-202117331593-A
Country	US
Kind code	B2
Filing date	May 26, 2021
Priority date	May 28, 2020
Publication date	Feb 27, 2024
Grant date	Feb 27, 2024

Abstract

In a cyclic anthraquinone process for producing hydrogen peroxide, which comprises a distillation unit with vapor compression for concentrating hydrogen peroxide, aqueous condensate from the distillation unit is passed over a bed of a cation exchange resin in its protonated from to provide a purified condensate, and the purified condensate is used as extractant for extracting hydrogen peroxide in the anthraquinone process, as column reflux for the distillation unit or as a diluent for diluting an aqueous hydrogen peroxide solution.

First claim

The invention claimed is:

1. A device for producing hydrogen peroxide by an anthraquinone process, comprising:
a) a hydrogenator for hydrogenating a working solution comprising an alkylanthraquinone and/or an alkyltetrahydroanthraquinone and at least one water immiscible solvent for said alkylanthraquinone and/or alkyltetrahydroanthraquinone with a gas comprising molecular hydrogen in the presence of a hydrogenation catalyst to provide a hydrogenated working solution;
b) an oxidizer for oxidizing the hydrogenated working solution with a gas, comprising molecular oxygen to provide an oxidized working solution containing dissolved hydrogen peroxide, said oxidizer being connected to said hydrogenator to receive said hydrogenated working solution;
c) an extractor for extracting hydrogen peroxide with an aqueous extractant from oxidized working solution containing dissolved hydrogen peroxide to provide a dilute aqueous hydrogen peroxide solution, said extractor being connected to said oxidizer to receive said oxidized working solution containing dissolved hydrogen peroxide;
d) a distillation unit for concentrating an aqueous hydrogen peroxide solution to provide a concentrated aqueous hydrogen peroxide solution and an aqueous condensate, said distillation unit comprising a hydrogen peroxide evaporator, a distillation column receiving vapor from said hydrogen peroxide evaporator and a vapor compressor receiving overhead vapor from said distillation column and passing compressed vapor as heating medium to said hydrogen peroxide evaporator, said distillation unit being connected to said extractor to receive said dilute aqueous hydrogen peroxide solution; and
e) a purification unit comprising a bed of a cation exchange resin in its protonated form for purifying said aqueous condensate to provide a purified condensate, said purification unit being connected to said distillation unit to receive said aqueous condensate as feed and being connected to (i) said extractor, passing purified condensate as aqueous extractant to said extractor, or (ii) said distillation unit, passing purified condensate as a column reflux to said distillation column, or (iii) a hydrogen peroxide dilution device, passing purified condensate as diluent to the hydrogen peroxide dilution device, or (iv) any combination of (i) to (iii); and wherein said purification unit comprises a first filter upstream of said bed of cation exchange resin.

2. The device of claim 1 , wherein the vapor compressor of said distillation unit is a steam driven ejector.

3. The device of claim 1 , wherein the distillation unit comprises a falling film evaporator as hydrogen peroxide evaporator, a separation vessel horizontally partitioned by a demister, connected below the demister to the falling film evaporator to receive a vapor-liquid mixture provided by the hydrogen peroxide evaporator, a conduit connected to the separation vessel above the demister for passing vapor to the distillation column, and a recycle conduit for recycling liquid from the bottom of the separation vessel to the falling film evaporator.

4. The device of claim 1 , wherein the cation exchange resin is a sulfonated polystyrene resin.

5. The device of claim 1 , additionally comprising a buffer vessel connected to said purification unit to receive said purified condensate and connected to said extractor to provide said aqueous extractant.

6. The device of claim 1 , wherein said purification unit comprises a second filter downstream of said bed of cation exchange resin.

7. The device of claim 1 , comprising a heat exchanger transferring heat from said aqueous condensate to said dilute aqueous hydrogen peroxide solution.

8. A process for producing hydrogen peroxide by an anthraquinone process, comprising the steps of:
a) hydrogenating a working solution comprising an alkylanthraquinone and/or an alkyltetrahydroanthraquinone and at least one solvent for said alkylanthraquinone and/or alkyltetrahydroanthraquinone with a gas comprising molecular hydrogen in the presence of a hydrogenation catalyst to provide a hydrogenated working solution;
b) oxidizing hydrogenated working solution of step a) with a gas comprising molecular oxygen to provide an oxidized working solution containing dissolved hydrogen peroxide;
c) extracting hydrogen peroxide from oxidized working solution of step b) with an aqueous extractant to provide a dilute aqueous hydrogen peroxide solution containing from 25 to 50% by weight hydrogen peroxide;
d) concentrating dilute aqueous hydrogen peroxide solution of step c) in a distillation unit comprising a hydrogen peroxide evaporator, a distillation column receiving vapor from the hydrogen peroxide evaporator and a vapor compressor receiving overhead vapor from the distillation column and passing compressed vapor as heating medium to the hydrogen peroxide evaporator to provide a concentrated aqueous hydrogen peroxide solution, containing from 45 to 90% by weight hydrogen peroxide, and an aqueous condensate;
e) purifying aqueous condensate of step d) in a purification unit by passing it through a bed of a cation exchange resin in its protonated form to provide a purified condensate wherein the bed of cation exchange resin is replaced by fresh resin when the concentration of iron, nickel or chromium in said purified condensate increases to a value of more than 0.02 mg/l; and
f) reusing purified condensate of step e) as (i) an aqueous extractant in extracting step c), (ii) a column reflux for the distillation column in concentrating step d), (iii) a diluent in a step of diluting an aqueous hydrogen peroxide solution, or (iv) in any combination of (i) to (iii).

9. The process of claim 8 , wherein in step d), a steam driven ejector is used as vapor compressor.

10. The process of claim 8 , wherein step e) comprises filtering the aqueous condensate of step d) before passing it over the bed of cation exchange resin.

11. The process of claim 8 , wherein part of the purified condensate is passed to the top of the distillation column of step d) to provide a column reflux and the remainder is passed to extracting step c).

12. The process of claim 8 , wherein extracted working solution of step c) is recycled to hydrogenating step a).

13. The process of claim 12 , wherein the extracted working solution of step c) is dried before it is recycled to hydrogenating step a).

14. The device of claim 2 , wherein the distillation unit comprises a falling film evaporator as hydrogen peroxide evaporator, a separation vessel horizontally partitioned by a demister, connected below the demister to the falling film evaporator to receive a vapor-liquid mixture provided by the hydrogen peroxide evaporator, a conduit connected to the separation vessel above the demister for passing vapor to the distillation column, and a recycle conduit for recycling liquid from the bottom of the separation vessel to the falling film evaporator.

15. The device of claim 14 , wherein said purification unit comprises a first filter upstream of said bed of cation exchange resin.

16. The device of claim 15 , wherein the cation exchange resin is a sulfonated polystyrene resin.

17. The device of claim 16 , additionally comprising a buffer vessel connected to said purification unit to receive said purified condensate and connected to said extractor to provide said aqueous extractant.

18. The device of claim 17 , comprising a heat exchanger transferring heat from said aqueous condensate to said dilute aqueous hydrogen peroxide solution.

19. A process for producing hydrogen peroxide

Assignees

• Evonik Operations Gmbh

Inventors

• Seidel Nils Henning
• Kamp Johannes
• Glenneberg Jürgen
• Panz Christian
• Arévalo Saade Eduardo Federico
• Mangalapally Hari Prasad

Classifications

• C01B15/023 Primary

  by the alkyl-anthraquinone process · CPC title

• B01D3/40

  Extractive distillation · CPC title

• C01P2006/82

  water content · CPC title

• C01B15/01 Primary

  Hydrogen peroxide · CPC title

• C07C2603/22

  containing only six-membered rings · CPC title