Production of sodium borohydride from sodium borohydride dihydrate in a fluidized bed dryer

• US 6,231,825 B1
• Filed: 07/29/1999
• Issued: 05/15/2001
• Est. Priority Date: 07/29/1999
• Status: Expired due to Term

• Current Assignee: Ascensus Specialties LLC
• Original Assignee: Rohm and Haas Company (Dow, Inc.)
• Inventors: Mahoney, Lise L., Richardson, Walter A., Eiseman, Austin L., Colby, Richard J.
• Primary Examiner(s): NGUYEN, NGOC YEN M
• Application Number:
  US09/363,103
• Time in Patent Office: 656 Days
• Field of Search: 423/286, 252/188.26, 252/188.22, 252/188.1, 422/139
• US Class Current: 423/286
• CPC Class Codes: C01B 6/21 Preparation of borohydrides of alkali metals, alkaline earth metals, magnesium or beryllium; Addition complexes thereof, e.g. LiBH4.2N2H4, NaB2H7

Abstract

Drying sodium borohydride dihydrate particles in a flowing stream of a chemically inert drying gas results in novel nearly odor-free, dust-free sodium borohydride particles which are free flowing without the need for anti-caking or flow additives. The dihydrate particles are preferably dried in a fluidized bed formed with a flowing stream of nitrogen.

Claims

1. A method of preparing sodium borohydride from sodium borohydride dehydrate particles comprising:

providing a drying gas which is capable of removing water from said particles,

flowing a stream of said drying gas around a plurality of said sodium borohydride dihydrate particles until said particles are converted to sodium borohydride;

wherein said particles are fluidized in said stream of drying gas.

2. The method of claim 1 wherein said drying gas initially has a dew point of less than −

18°

C.

3. The method of claim 1 wherein said drying gas is selected from the group consisting of helium, argon, neon, nitrogen and air.

4. The method of claim 1 wherein said drying gas is nitrogen.

5. The method of claim 1 wherein said stream of drying gas contacts said plurality of particles at a temperature of 31°

C or less.

6. The method of claim 1 wherein said particles initially contact said drying gas at a temperature up to 31°

C. and after they have been partially converted to sodium borohydride said particles contact said drying gas at a temperature in excess of 31°

C.

7. The method of claim 1 including:

recovering said drying gas after it flows around said plurality of particles,

dehydrating said recovered drying gas by removing water therefrom, and

recycling said dehydrated drying gas to further contact a plurality of particles of sodium borohydride dihydrate.

8. The method of claim 7 wherein:

said dehydrating comprises contacting said recovered drying gas with a desiccant capable of absorbing water from said recovered drying gas.

9. A method of drying sodium borohydride dihydrate particles comprising:

providing a plurality of said particles,

flowing nitrogen through said plurality of particles until at least the major portion of said particles have been converted to sodium borohydride;

wherein said nitrogen flows through said plurality of particles at a sufficient velocity to suspend said particles in said nitrogen.

10. The method of claim 9, wherein said nitrogen is provided at a temperature of up to 31°

C.

11. The method of claim 9, comprising:

contacting said plurality of particles with said flowing nitrogen at a first temperature of up to 31°

C. until a portion of said particles have been converted to sodium borohydride, and subsequently

further contacting said plurality of particles with said flowing nitrogen at a second temperature in excess of 31°

C.

12. The method of claim 11 wherein said second temperature is in the range of 32°

C. to 65°

C.

13. The method of claim 9 further comprising:

recovering said nitrogen after it flows through said plurality of particles,

dehydrating said recovered nitrogen by removing water therefrom, and

recycling said dehydrated nitrogen to further contact with a plurality of said particles.

14. The method of claim 13 wherein said step of dehydrating comprises

contacting said recovered nitrogen with a desiccant capable of absorbing water from said recovered nitrogen.

15. The method of claim 14 wherein said desiccant is selected from the group consisting of silica gel, titanium gel, lithium chloride or molecular sieve.

16. The method of claim 9 wherein:

said sodium borohydride dihydrate particles are substantially continuously introduced to said flowing nitrogen, and

substantially continuously withdrawing said converted sodium borohydride particles from said flowing nitrogen.

17. The method of claim 9 wherein said nitrogen is provided at a dew point of less than −

18°

C.

18. The product of the process of claim 9.

19. A free flowing plurality of sodium borohydride particles having a bulk density between 20 and 28 pounds per cubic foot and wherein at least 80% by weight of said particles pass through a 10 mesh screen and are retained on a 60 mesh screen and said plurality of sodium borohydride particles is capable of dissolving in stirred 1-butanol at 5°

C. to form a concentration of sodium borohydride of at least 0.3% by weight in 15 minutes or less.

20. The free-flowing plurality of particles of claim 19 which is free of any flow additives.

21. The plurality of particles of claim 19 wherein at least 98.5% by weight is sodium borohydride.

22. A plurality of particles according to claim 19 wherein less than 5% by weight of the particles pass through a 60 mesh screen.

23. A plurality of particles according to claim 19 wherein less than 0.25% by weight of the particles are capable of passing through a 200 mesh screen.

24. A plurality of particles according to claim 19 wherein a said particles have a smooth, opalescent surface.

25. A plurality of particles according to claim 19 which is capable of substantially retaining its original capacity to flow freely after 9 weeks storage at 22°

C. and 48% relative humidity.

26. A free-flowing plurality of sodium borohydride particles wherein at least 90% by weight of said particles pass through a 10 mesh screen and are retained on a 60 mesh screen and less than 0.25% by weight are capable of passing through a 200 mesh screen, and which is capable of dissolving in stirred 1-butanol at 5°

C. to form a concentration of sodium borohydride of at least 0.3% by weight in 15 minutes or less.