Production method for dipeptide-containing granules

• US 10,683,240 B2
• Filed: 10/01/2018
• Issued: 06/16/2020
• Est. Priority Date: 10/02/2017
• Status: Expired due to Fees

• Current Assignee: Evonik Operations GmbH (Rag-Stiftung)
• Original Assignee: Evonik Operations GmbH (Rag-Stiftung)
• Inventors: Jakob, Harald, Hasselbach, Hans Joachim, Egly, Dominik, Hessberger, Waldemar
• Primary Examiner(s): Langel, Wayne A
• Application Number:
  US16/148,484
• Publication Number:
  US 20190135708A1
• Time in Patent Office: 624 Days
• Field of Search: None
• CPC Class Codes: B01J 2/02 by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
• CPC Class Codes: C05C 3/00 Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
• CPC Class Codes: C05D 1/00 Fertilisers containing potassium C05D7/00 takes precedence
• CPC Class Codes: C05F 11/10 Fertilisers containing plant vitamins or hormones
• CPC Class Codes: C05G 5/12 Granules or flakes
• CPC Class Codes: C05G 5/30 Layered or coated, e.g. dust-preventing coatings
• CPC Class Codes: C12P 13/12 Methionine; Cysteine; Cystine
• CPC Class Codes: Y02E 50/30 Fuel from waste, e.g. synthetic alcohol or diesel
• CPC Class Codes: Y02W 30/40 Bio-organic fraction processing; Production of fertilisers from the organic fraction of waste or refuse

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 sulfate, and use thereof.

Claims

1. A process for producing a particulate composition comprising methionine, methionylmethionine, potassium salt and ammonium sulfate by spray granulation, wherein:

(a) a first aqueous solution or suspension (i), comprising 30 to 40% by weight ammonium sulfate,

a second aqueous solution or suspension (ii), comprising 2 to 6% by weight methionine, 4 to 8% by weight methionylmethionine and 6 to 14% by weight potassium in the form of potassium salt and a gas,

are sprayed via a three-fluid nozzle into a fluidized bed, with simultaneous evaporation of water in the fluidized bed, and with generation of crude particles, and optionally

(b) the crude particles obtained in step (a) are dried.

2. The process according to claim 1, in which a second aqueous solution or suspension (ii), containing 3 to 5% by weight methionine and/or 5 to 7% by weight methionylmethionine and/or 8 to 12% by weight potassium in the form of potassium salt is used.

3. The process according to claim 1, in which the second aqueous solution or suspension (ii) is used in a weight ratio for the first aqueous solution or suspension (i) of 1.0/0.5 to 1.0/3.0.

4. The process according to claim 1, wherein air, nitrogen or CO₂ is used as gas.

5. The process according to claim 1, wherein step (a) of the process is carried out in a fluidized bed at a temperature in the fluidized bed of 60 to 130°

C.

6. The process according to claim 1, further comprising the step of preparing the first aqueous solution or suspension (i), comprising ammonium sulfate, substantially by treating a gas mixture comprising hydrogen cyanide and ammonia, obtained in the production of hydrogen cyanide from methane and ammonia, with aqueous sulfuric acid and subsequently neutralizing the resulting aqueous solution with ammonia.

7. The process according to claim 1, further comprising the step of preparing the second aqueous solution or suspension (ii) by isolating a mother liquor formed in a process for producing methionine that comprises at least the steps of

hydrolysing 5-(2-methylmercaptoethyl)hydantoin with potassium carbonate, potassium hydrogen carbonate to give aqueous potassium methioninate,

neutralizing aqueous potassium methioninate with carbon dioxide to form methionine and subsequently crystallizing the methionine.

8. The process according to claim 1, in which the first aqueous solution or suspension (i) is additionally admixed with an amount of sulfuric acid such that after the spray granulation, a particulate composition is obtained which after dissolution in water has a pH of 3 to 6, measured on a 10% by weight aqueous solution of the particulate composition at room temperature with a glass pH electrode with liquid electrolyte filling in the form of a 3-molar KCl solution.

9. The process according to claim 1, in which, further, the aqueous solution or suspension (ii) used in step (a) is concentrated before step (a) by evaporation of water to give an aqueous suspension having up to 70% by weight solids content.

10. The process according to claim 1, in which an ammonium sulfate shell layer is applied to the particles obtained in step (b) by spraying with an aqueous solution containing 30 to 40% by weight ammonium sulfate with simultaneous evaporation of the water, the proportion of the ammonium sulfate shell layer formed on the particles being 5 to 30% by weight, based on the total weight of the particles formed.

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

12. The process according to claim 11, wherein the potassium salt is at least one potassium salt selected from the group consisting of formic acid, acetic acid, propanoic acid, 2-hydroxypropanoic acid, 2-hydroxy-4-methylthiobutanoic acid, methionine, methionylmethionine, KHCO₃, K₂CO₃, KHSO₄ and K₂SO₄.

13. A fertilizer or fertilizer additive, comprising a composition produced by the process of claim 1.