Process for producing biuret from urea

Patent metadata

Field	Value
Publication number	US-12030837-B2
Application number	US-202118037704-A
Country	US
Kind code	B2
Filing date	Aug 31, 2021
Priority date	Nov 18, 2020
Publication date	Jul 9, 2024
Grant date	Jul 9, 2024

Abstract

A process for the production of biuret from urea wherein: a urea aqueous solution ( 24 ) withdrawn from the recovery section of a urea plant is processed to remove water and obtain a concentrated urea melt ( 25 ); said urea melt is processed under biuret-forming conditions to decompose urea into biuret and ammonia and obtain a high-biuret urea melt ( 26 ); said high-biuret urea melt ( 26 ) is diluted with water or with an aqueous stream obtaining a solution ( 28 ); the solution ( 28 ) is subject to crystallization and precipitation of a solid phase containing biuret which is separated from the aqueous phase.

First claim

What is claimed is:

1. A process for the production of biuret from urea comprising:
a) ammonia and carbon dioxide are reacted in a synthesis section at a synthesis pressure to form urea and obtaining a reaction effluent containing urea, water and unconverted reagents;
b) said reaction effluent is processed in a recovery section to recover unconverted reagents contained therein;
c) a urea aqueous solution, withdrawn from the recovery section, is processed to remove water and obtain a concentrated urea melt; said urea aqueous solution containing no more than 100 ppm by weight of formaldehyde;
d) said urea melt is processed under biuret-forming conditions to decompose urea into biuret and ammonia and obtain a biuret urea melt;
e) said biuret urea melt is diluted with water or with an aqueous stream obtaining a solution;
f) the solution obtained at step e) is subject to a process of crystallization including precipitation of a solid phase containing biuret and obtaining a slurry including precipitated solid phase and a mother liquor;
g) the slurry obtained at step f) is processed to obtain a biuret-containing solid product and a mother liquor.

2. The process according with claim 1 , wherein the step g) includes separation of a solid phase from the slurry and further processing of said solid phase to remove residual water.

3. The process according to claim 1 , wherein the solid product obtained after step g) contains at least 55% by weight of biuret.

4. The process according to claim 1 , wherein the sum of biuret and urea in the solid product obtained after step g) is at least 80% by weight.

5. The process according to claim 1 , wherein step d) is performed by maintaining the urea melt in a reaction space.

6. The process according to claim 5 , wherein the biuret-forming conditions of step d) include one or more of:
a reaction temperature in the reaction space of 160° C. to 180° C.;
a residence time in the reaction space that ranges from 30 min to 100 min;
a pressure in the reaction space which is atmospheric pressure or slightly below atmospheric pressure.

7. The process according to claim 1 , wherein the urea aqueous solution of step c) is free of formaldehyde.

8. The process according to claim 1 , wherein:
the urea aqueous solution of step c) is a first portion of a solution obtained from the recovery section;
a second portion of urea aqueous solution from the recovery section is processed to remove water, separately from the first portion, obtaining a urea melt;
said urea melt obtained from the second portion of the solution is processed for the production of low-biuret urea.

9. The process according to claim 1 , wherein the solution obtained after dilution of step e) contains by weight 40% to 60% of water.

10. The process according to claim 1 , wherein gaseous ammonia obtained at step d) is condensed obtaining an ammonia solution and ammonia contained in said solution is recycled to the urea process.

11. The process according to claim 10 , wherein said gaseous ammonia is condensed with process condensate from a waste water treatment section and the ammonia solution is recycled to said waste water treatment section.

12. The process according to claim 10 , wherein the ammonia solution is subject to ammonia stripping in a dedicated ammonia stripper, thus obtaining an aqueous process condensate and a carbonate recycle solution;
said recycle solution is sent to the urea recovery section;
a first portion of said process condensate is used for condensation of said gaseous ammonia.

13. The process according to claim 12 , wherein: a waste water obtained at step c) is treated in said ammonia stripper and a second portion of said process condensate is used in step e) to dilute the biuret urea melt.

14. The process according to claim 1 , wherein the mother liquor obtained at step f) is treated by adding an acid or carbon dioxide to reduce the pH of the liquor, and cause the precipitation of cyanuric acid contained in the liquor, and the precipitated cyanuric acid is removed.

15. The process according to claim 14 , wherein the mother liquor is treated by absorption of gaseous carbon dioxide and the absorption is performed under pressure.

16. The process according to claim 1 , wherein the mother liquor of step f) is mixed with the urea solution of step c) before the water removal step.

17. The process according to claim 1 , wherein said urea aqueous solution contains no more than 50 ppm by weight of formaldehyde.

18. The process according to claim 1 , wherein the solid product obtained after step g) contains at least 70% by weight of biuret.

19. The process according to claim 1 , wherein step d) is performed by maintaining the urea melt in a reaction space in a continuously stirred condition.

20. The process according to claim 5 , wherein the biuret-forming conditions of step d) include one or more of:
a reaction temperature in the reaction space of 160° C. to 170° C.;
a residence time in the reaction space that ranges from 30 min to 100 min;
a pressure in the reaction space which is atmospheric pressure or slightly below atmospheric pressure.

21. The process according to claim 5 , wherein the biuret-forming conditions of step d) include one or more of:
a reaction temperature in the reaction space of 165° C.;
a residence time in the reaction space that ranges from 30 min to 100 min;
a pressure in the reaction space which is atmospheric pressure or slightly below atmospheric pressure.

22. The process according to claim 1 , wherein the solution obtained after dilution of step e) contains by weight 50% of water.

23. The process according to claim 1 , wherein the mother liquor obtained at step f) is treated by adding an acid or carbon dioxide to reduce the pH of the liquor to 7.2 or less, and cause the precipitation of cyanuric acid contained in the liquor, and the precipitated cyanuric acid is removed.

24. The process according to claim 14 , wherein the mother liquor is treated by absorption of gaseous carbon dioxide and the absorption is performed at a pressure of about 5 bar abs.

25. The process according to claim 1 , wherein the mother liquor of step f), after removal of cyanuric acid, is mixed with the urea solution of step c) before the water removal step.

Assignees

• Casale Sa

Inventors

• Marrone Leonardo
• Benedetti Alberto
• Biasi Pierdomenico
• Pizzolitto Cristina

Classifications

• Y02P20/582

  Recycling of unreacted starting or intermediate materials · CPC title

• C07C273/189

  Purification, separation, stabilisation, use of additives · CPC title

• C07C275/62 Primary

  Y being a nitrogen atom, e.g. biuret · CPC title

• C07C273/1881 Primary

  from urea · CPC title