Cyanuric acid production by controlled pyrolysis of biuret

• US 4,894,452 A
• Filed: 04/18/1988
• Issued: 01/16/1990
• Est. Priority Date: 04/18/1988
• Status: Expired due to Fees

• Current Assignee: Lenroc Company
• Original Assignee: Lenroc Company
• Inventors: Stephan, Kurt F.
• Primary Examiner(s): Schwartz, Richard A.
• Assistant Examiner(s): Whittenbaugh, Robert C.
• Application Number:
  US07/182,504
• Time in Patent Office: 638 Days
• Field of Search: 544/192
• US Class Current: 544/192
• CPC Class Codes: C07D 251/32 Cyanuric acid; Isocyanuric acid

Abstract

The process of producing from urea a reaction product which is predominantly cyanuric acid, which process involves only the application of heat without use of solvents or catalysts. The process in its first stage involves heating molten urea for a time and at a temperature to convert the urea to a first stage reaction product comprising less than 40% urea and at least 30% biuret, then cooling and comminuting the first stage reaction product, then as a second stage of the process, passing hot air through the comminuted first stage reaction product at temperatures progressively increasing but maintained below the melting point of the reaction, such solid phase heating of the reaction product during the second stage of the process being maintained until the cyanuric acid content is at least about 50% of the final reaction product and is preferably at least about 70%.

Claims

1. A process in which urea is pyrolytically converted to cyanuric acid, said process comprising heating, in dry, particulate, and essentially solid state, a partially pyrolyzed reaction product containing less than about 40% urea by weight an at least from about 30% biuret by weight, the heating of such feedstock occurring while maintaining the particles in essentially solid phase and at a temperature substantially at or slightly below the softening temperature of the particles with forced hot gas flow interstitially through the particles for a sufficient time to increase the cyanuric acid content thereof until the reaction product is principally cyanuric acid, partly by conversion of urea to biuret and in turn by conversion of biuret to cyanuric acid.

2. The process of claim 1, comprising heating the particles at a temperature of between 100°

C. to 200°

C.

3. The process of claim 1, comprising heating the particulate reaction product with forced air circulation herethrough for a time sufficient to product a cyanuric acid content greater than about 70% by weight.

4. The process of claim 3, wherein the particle size of the feedstock is about 1 mesh or less.

5. The process of claim 3, wherein the particle size of the feedstock is in the range of about 4 mesh to about 16 mesh.

6. The process according to claim 3, comprising arranging the particulate feedstock in a bed to a depth of up to about 5 feet, and causing forced air circulation vertically or horizontally therethrough.

7. The process of claim 1, wherein the partially pyrolyzed reaction product comprising the feedstock for the process is prepared by subjecting urea to a pyrolyzation for a time and temperature, in generally inverse reaction, of between about 15 minutes at about 220°

C. and about 24 hours at about 135°

C., followed by cooling of the resulting partially pyrolyzed reaction product to solid form, and by comminuting same.

8. The process of claim 7, comprising promoting crystallization and accelerating cooling of the partially pyrolyzed reaction product by adding thereto a seed material in powder form.

9. The process of pyrolytically producing from urea a reaction product which is predominantly cyanuric acid without use of solvents or catalysts, said process comprising heating molten urea for a time and at a temperature to convert the urea to an intermediate reaction product comprising less than about 40% urea and at least about 30% biuret by weight, cooling and comminuting such intermediate reaction product, passing hot gas through the comminuted product at progressively increasing temperatures maintained near but below the melting point of the product so that the product is maintained in essentially solid phase, and continuing such heating of the product until the cyanuric acid content thereof is at least about 50% by weight.

10. The process of claim 9, wherein the heating of the molten urea is under conditions resulting in an intermediate realistic product comprising less than about 30% urea and at least about 40% biuret by weight.

11. The process of claim 10, comprising continuing the solid phase heating of the product until the cyanuric acid content thereof is at least about 70% by weight.

12. The process of claim 9, comprising continuing the solid phase heating of the product until the cyanuric acid content thereof is at least about 70% by weight.