IP Library Granted Patent US 11,180,426
Granted Patent B2
US 11,180,426 · App. 16/312,638 · Granted Nov 23, 2021

Dipeptide-containing granular material

Inventors: Martin Koerfer (Kahl, DE); Hans Joachim Hasselbach (Gelnhausen, DE); Gerit Niggemann (Frankfurt, DE); Antje Hansmeier (Antwerp, BE); Hans Christian Alt (Gelnhausen, DE); Dominik Egly (Michelstadt, DE); Peter Schulte (Zuelpich, DE)
Assignee: Evonik Operations GmbH
C05C11/00B01J2/00B01J2/02C05C3/00C05D1/02C05G5/12C05G5/30
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Quick Facts
Patent No.
US 11,180,426
App. No.
16/312,638
Granted
Nov 23, 2021
Kind
B2
Abstract

The present invention relates to a process for producing a particulate composition containing methionine, methionylmethionine, potassium in the form of potassium salt and ammonium sulphate, and use thereof.

Claims (55)

1. A process for producing a particulate composition containing methionine, methionylmethionine, potassium salt and ammonium sulfate, the process comprising:

generating

particles from an aqueous mixture by a forming process with upstream and/or simultaneous evaporation of the water; and

drying the particles to obtain the particulate composition,

wherein the aqueous mixture comprises:

0.5 to 4% by weight of methionine,

0.5 to 5% by weight of methionylmethionine,

1 to 9% by weight of potassium in the form of a potassium salt; and

7 to 35% by weight of ammonium sulfate.

2. The process according to claim 1 , wherein the aqueous mixture comprises:

1 to 3% by weight of the methionine,

1 to 4% by weight of the methionylmethionine,

2 to 7% by weight of the potassium in the form of the potassium salt, and/or

10 to 30% by weight of the ammonium sulfate.

3. The process according to claim 1 , wherein the aqueous mixture is produced by mixing an aqueous solution (i) comprising 30 to 40% by weight of the ammonium sulfate with an aqueous solution (ii) comprising:

2 to 6% by weight of the methionine;

4 to 8% by weight of the methionylmethionine; and

6 to 14% by weight of the potassium in the form of the potassium salt,

such that a ratio of the aqueous solution (ii) to the aqueous solution (i) is from 1.0/0.5 to 1.0/3.0.

4. The process according to claim 3 , wherein:

the aqueous solution (i) comprises 30 to 40% by weight of the ammonium sulfate; and

the aqueous solution (ii) comprises:

3 to 5% by weight of the methionine,

5 to 7% by weight of the methionylmethionine, and/or

8 to 12% by weight of the potassium in the form of the potassium salt.

5. The process according to claim 3 , further comprising:

preparing the aqueous solution (i) comprising the ammonium sulfate primarily by treating a gaseous mixture comprising hydrogen cyanide and ammonia, generated in the production of hydrogen cyanide from methane and ammonia, with sulphuric acid and, subsequent, neutralizing a resulting aqueous solution with ammonia.

6. The process according to claim 3 , further comprising:

preparing the aqueous solution (ii) by separating a mother liquor formed in the reaction of 5-(2-methylmercaptoethyl)hydantoin with potassium carbonate, potassium hydrogen carbonate and carbon dioxide to give the methionine.

7. The process according to claim 1 , wherein the aqueous mixture is additionally treated with sulphuric acid until a pH of 3 to 6 is reached in the aqueous mixture, measured at room temperature with a glass pH electrode filled with liquid electrolyte in the form of a 3 molar KCl solution.

8. The process according to claim 1 , wherein the aqueous mixture is also concentrated, prior to performing the forming process, by evaporation of water to give an aqueous suspension with a solids content of up to 70% by weight.

9. The process according to claim 1 , wherein an ammonium sulfate shell layer is applied to the particles by spraying with an aqueous solution comprising 30 to 40% by weight ammonium sulfate with simultaneous evaporation of water, such that a proportion of the ammonium sulfate shell layer formed on the particles is 5 to 30% by weight based on the total solids content of the particles.

10. The process according to claim 1 , wherein the potassium salt is present as at least one salt of an inorganic or organic acid.

11. The process according to claim 10 , wherein the potassium salt is at least one potassium salt formed from an acid selected from the group consisting of formic acid, acetic acid, propanoic acid, 2-hydroxypropanoic acid, 2-hydroxy-4-methylthiobutanoic acid, KHCO 3 , K 2 CO 3 , KHSO 4 and K 2 SO 4 .

12. The process according to claim 1 , wherein the forming process is carried out as a spray granulation, mix granulation, extrusion or compaction.

13. The process according to claim 12 , wherein the forming process is carried out as a spray granulation with a two-phase nozzle, in which a gas component together with the aqueous mixture is sprayed as a liquid component via the two-phase nozzle.

14. The process according to claim 13 , wherein air or nitrogen are used as a gas component.

15. The process according to claim 13 , wherein the forming process occurs in a fluidized bed at a temperature of 60 to 130° C.

16. A particulate composition, comprising:

5 to 10% by weight of methionine;

2.5 to 9% by weight of methionylmethionine;

4 to 20% by weight of potassium in the form of a potassium salt; and

27 to 80% by weight of ammonium sulfate.

17. The composition according to claim 16 , comprising:

2 to 8% by weight of the methionine,

3 to 7% by weight of the methionylmethionine,

5 to 17% by weight of the potassium in the form of the potassium salt, and/or

30 to 76% by weight of the ammonium sulfate.

18. The composition according to claim 16 , wherein the potassium salt is at least one potassium salt formed from an acid selected from the group consisting of formic acid, acetic acid, propanoic acid, 2-hydroxypropanoic acid, 2-hydroxy-4-methylthiobutanoic acid, KHCO 3 , K 2 CO 3 , KHSO 4 and K 2 SO 4 .

19. The composition according to claim 16 , further comprising:

a binder selected from the group consisting of a porous volcanic silicate rock, a precipitated silica, a fumed silica, and a porous carbonate rock.

20. The composition according to claim 16 , wherein:

particles of the particulate composition have been coated with an ammonium sulfate layer; and

a proportion of the ammonium sulfate layer is 5 to 30% by weight, based on the total solids content of the particles.

21. A fertilizer or fertilizer additives, comprising the particulate composition of claim 16 .

Assignments (2)
CHANGE OF NAME Recorded Jan 31, 2020
From: EVONIK DEGUSSA GMBH
To: EVONIK OPERATIONS GMBH
Reel/Frame 051765/0166 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 31, 2019
From: KOERFER, MARTIN; HASSELBACH, HANS JOACHIM; NIGGEMANN, GERIT; HANSMEIER, ANTJE; ALT, HANS CHRISTIAN; EGLY, DOMINIK; SCHULTE, PETER
To: EVONIK DEGUSSA GMBH
Reel/Frame 049332/0495 →
Priority Claims (1)
EP 16176371 · Jun 27, 2016 · regional
Continuity (1)
Related Publication 20190322600A1 · Oct 24, 2019