Mixed nitrate salt heat transfer medium and process for providing the same

• US 4,430,241 A
• Filed: 07/01/1982
• Issued: 02/07/1984
• Est. Priority Date: 07/01/1982
• Status: Expired due to Fees

• Current Assignee: OLIN Corporation
• Original Assignee: OLIN Corporation
• Inventors: Fiorucci, Louis C.
• Primary Examiner(s): Kittle, John E.
• Assistant Examiner(s): Wax, Robert A.
• Application Number:
  US06/394,192
• Time in Patent Office: 586 Days
• Field of Search: 252/70, 23/293 R, 23/293 A, 23/302 T, 23/313 FB, 423/182, 423/183, 423/201, 423/395, 423/641, 423/659, 71/58, 71/59, 264/3 C, 264/3 D, 149/41, 149/46
• US Class Current: 252/70
• CPC Class Codes: C09K 5/063 Materials absorbing or liberating heat during crystallisation; Heat storage materials

Abstract

A process for producing particles of a non-friable eutectic mixture of sodium nitrate and potassium nitrate for solar power station use is disclosed. In one embodiment of the invention, the particles are produced by shock chilling a molten stream of mixed nitrate material and crushing the resulting flakes to a size range of between about -5 mesh and about +30 mesh. In a second embodiment, particles of this size are produced by spray granulation of a concentrated solution of mixed nitrate salts onto a fluidized bed to produce dry, free-flowing, solid spheres. In both embodiments, the particles are extremely hard, resistant to moisture pickup and adaptable to being readily shipped by bulk containers.

Claims

1. A process for preparing particles of a non-friable, eutectic mixture of sodium nitrate and potassium nitrate for use as a heat transfer and thermal storage medium for solar power stations comprising steps of:

(a) preparing a fluid mixture of between about 70% and about 30% by weight sodium nitrate and about 30% and about 70% by weight potassium nitrate, wherein said fluid mixture has a combined level of sulfates, oxides, carbonates and chlorides of no more than about 0.7% by weight and with the chloride being no more than about 0.2% by weight;

(b) granulating said fluid mixture by a process selected from the group consisting of shock chilling and spray graining to form substantially homogeneous particles of said mixture; and

(c) recovering a salt product comprised of particles having a predetermined mesh size.

2. The process of claim 1 wherein said fluid mixture is formed by:

(a) admixing granular NaNO₃ and granular KNO₃ to produce a dry blended substantially homogeneous salt mix; and

(b) heating said salt mix while agitating it until it fuses to form a molten mass.

3. The process of claim 2 wherein said salt mix is heated to a temperature in the range of from about 220°

C. to about 300°

C.

4. The process of claim 3 wherein said salt mix is heated to a temperature in the range of from about 220°

C. to about 245°

C.

5. The process of claim 2 wherein said particles are formed by a shock chilling process which comprises:

(a) pouring said molten mass onto a chilled surface to form a solid, amorphous homogeneous sheet; and

(b) breaking up said sheet to form said particles.

6. The process of claim 5 wherein said solid sheet is between about 0.20" and about 1.25" thick.

7. The process of claim 5 wherein said solid sheet is between about 0.25" and about 0.75" thick.

8. The process of claim 1 wherein said fluid mixture is an aqueous solution of sodium nitrate and potassium nitrate.

9. The process of claim 8 wherein said aqueous solution has a total salt concentration of between about 60% and about 75% by weight.

10. The process of claim 8 wherein said aqueous solution is at a temperature of between about 95°

C. and about 120°

C.

11. The process of claim 8 wherein said granulation step is carried out by spray graining in a process which comprises:

(a) spraying said aqueous solution into a drying chamber and contacting said sprayed solution with a heated gas flowing through said chamber to form a dried fine particulate product, said fine particulate product being fluidized by said flowing gas; and

(b) agglomerating said fluidized fine particulate product by contacting it with additional aqueous solution which is being sprayed into said drying chamber for a time sufficient to form agglomerated particles of a predetermined mesh size.

12. The process of claim 10 wherein said heated gas is at a temperature of between about 160°

C. and about 200°

C.

13. The process of claim 5 or claim 11 wherein said recovery step comprises screening said agglomerated particles to separate out salt particles having an acceptable size range from those which are oversized or undersized.

14. The process of claim 13 wherein said acceptable salt particles are in the range of between about -5 mesh to about +30 mesh.

15. The process of claim 13 wherein oversized particles of said mix are crushed and rescreened.

16. The process of claim 13 wherein undersized particles of said mix are recycled to form a part of the feedstock for said fluid mixture.

17. The process of claim 13 wherein said salt particles are comprised of between about 65% and about 55% by weight sodium nitrate and about 35% to about 45% by weight potassium nitrate.

18. A process for making non-friable, dried salt particles for use as a heat transfer medium for solar power stations, said salt particles being a eutectic mixture of between about 70% and about 30% by weight sodium nitrate and between about 30% and about 70% by weight potassium nitrate, said particles being further characterized by having a maximum combined chloride, sulfate, oxide and carbonate content of about 0.7% by weight with the maximum chloride content being about 0.2%, said salt particles having been produced by a method comprising the steps of:

(a) admixing granular NaNO₃ and granular KNO₃ to produce a dry blended substantially homogeneous salt mix;

(b) heating said salt mix to a temperature in the range of about 220°

C. to about 300°

C. while agitating it until it fuses to form a molten mass;

(c) pouring said molten mass onto a chilled surface at a rate sufficient to form a solid, amorphous homogeneous sheet of between about 0.20" and about 1.25" thick;

(d) breaking up said sheet to form said particles; and

(e) classifying said particles to recover a final product.

20. The process of claim 18 or 19 wherein said acceptable salt particles are in the range of between about -5 mesh to about +30 mesh.

21. The process of claim 20 wherein oversized particles of said mix in size are crushed and reclassified.

22. The process of claim 20 wherein undersized particles of said mix are recycled to form a part of the feedstock for said fluid mixture.

19. A process for making non-friable, dried salt particles for use as a heat transfer medium for solar power stations, said salt particles being a eutectic mixture of between about 70% and about 30% by weight sodium nitrate and between about 30% and about 70% by weight potassium nitrate, said particles being further characterized by having a maximum combined chloride, sulfate, oxide and carbonate content of about 0.7% by weight with the maximum chloride content being about 0.2%, said salt particles having been produced by a method comprising the steps of:

(a) forming an aqueous solution of sodium nitrate and potassium nitrate, said solution having a total salt content of between about 60% and about 75% combined salt by weight at a temperature of between about 95°

C. and about 120°

C.;

(b) spraying said aqueous solution into a drying chamber and contacting said sprayed solution with a heated gas flowing through said chamber to form a dried fine particulate product, said fine particulate product being fluidized by said flowing gas;

(c) agglomerating said fluidized fine particulate product by contacting it with additional aqueous solution which is being sprayed into said drying chamber for a time sufficient to form said particles; and

(d) classifying said particles to recover a final product.

23. Non-friable, dried salt particles for use as a heat transfer medium for solar power stations, said salt particles being a eutectic mixture of between about 70% and about 30% by weight sodium nitrate and between about 30% and about 70% by weight potassium nitrate, said particles being further characterized by having a maximum combined chloride, sulfate, oxide and carbonate content of about 0.7% by weight with the maximum chloride content being about 0.2%.

24. The salt product of claim 23 wherein said salt particles are comprised of between about 65% and about 55% by weight sodium nitrate and about 35% to about 45% by weight potassium nitrate.

25. The salt product of claim 23 wherein said acceptable salt particles are in the range of between about -5 mesh to about +30 mesh.