Alkali metal ion source with moderate rate of ion release and methods of forming

• US 10,196,317 B2
• Filed: 04/27/2016
• Issued: 02/05/2019
• Est. Priority Date: 05/06/2013
• Status: Active Grant

• Current Assignee: Massachusetts Institute of Technology
• Original Assignee: Massachusetts Institute of Technology
• Inventors: Skorina, Taisiya, Allanore, Antoine
• Primary Examiner(s): Langel, Wayne A
• Application Number:
  US15/139,456
• Publication Number:
  US 20160311727A1
• Time in Patent Office: 1,014 Days
• Field of Search: None
• CPC Class Codes: C01B 33/26 Aluminium-containing silicates , i.e. silico-aluminates
• CPC Class Codes: C01B 33/32 Alkali metal silicates C01B33/24 , C01B33/26 take precedence
• CPC Class Codes: C01B 33/36 having base-exchange properties but not having molecular sieve properties regeneration thereof B01J49/00
• CPC Class Codes: C01P 2004/61 Micrometer sized, i.e. from 1-100 micrometer
• CPC Class Codes: C01P 2006/12 Surface area
• CPC Class Codes: C05D 1/00 Fertilisers containing potassium C05D7/00 takes precedence
• CPC Class Codes: C05D 1/04 from minerals or volcanic rocks
• CPC Class Codes: C05D 3/02 from limestone, calcium carbonate, calcium hydrate, slaked lime, calcium oxide, waste calcium products
• CPC Class Codes: C05D 9/00 Other inorganic fertilisers
• CPC Class Codes: C05D 9/02 containing trace elements
• CPC Class Codes: C05G 1/00 Mixtures of fertilisers belonging individually to different subclasses of C05

Abstract

An alkali metal ion source with a moderate rate of release of the ion (e.g. potassium) is formed by a method that includes: 1) combining an particulate ore that contains at least one of an alkali metal ion-bearing framework silicate (e.g. syenite ore) with at least one of an oxide and hydroxide of at least one of an alkali metal and alkaline earth metal such as calcium hydroxide; 2) milling the mixture of these two components optionally, with water, optionally, milling the dry components separately and blended thereafter, optionally, with water; 3) forming a mixture by adding water to the solid mixture after milling, if water was not added before milling; 4) exposing the mixture to an elevated temperature and pressure to form a gel that includes silica and the alkali metal of the framework silicate.

Claims

1. A method, comprising:

milling a combination which comprises i) a particulate alkali metal ion bearing framework silicate; and

ii) a metal oxide and/or a metal hydroxide; and

after milling the combination, hydrothermally processing the combination to provide a gel,

wherein milling the combination reduces the size of the particulate alkali metal ion bearing framework silicate so that at least about 50% by weight of the particles of the particulate alkali metal ion bearing framework silicate have a diameter of equal to or less than 5 μ

m as measured by laser-based particle-size distribution analysis.

2. The method of claim 1, wherein the particulate alkali metal ion bearing framework silicate comprises at least one member selected from the group consisting of lithium, sodium and potassium.

3. The method of claim 1, wherein the particulate alkali metal ion-bearing framework silicate comprises potassium.

4. The method of claim 1, when the particulate alkali metal ion bearing framework silicate comprises an aluminosilicate.

5. The method of claim 1, wherein the particulate alkali metal ion bearing framework silicate comprises at least one member selected from the group consisting of potassium feldspar (KAlSi₃O₈), leucite (KAlSi₂O₆), kalsilite (KAlSiO₄) and nepheline (Na₃KAl₄Si₄O₁₆).

6. The method of claim 1, wherein the particulate alkali metal ion bearing framework silicate comprises at least about 5% by weight of an equivalent amount of K₂O.

7. The method of claim 1, wherein the particulate alkali metal ion bearing framework silicate comprises at least one member selected from the group consisting of syenite, nepheline syenite, and granite.

8. The method of claim 1, wherein the metal oxide and/or a metal hydroxide comprises at least one member selected from the group consisting of an alkali metal oxide, an alkali metal hydroxide, an alkaline earth oxide and an alkaline earth hydroxide.

9. The method of claim 1, wherein hydrothermally processing the combination comprises heating the combination to a temperature of between about 100°

C. and about 350°

C.

10. The method of claim 1, wherein hydrothermally processing the combination heating the combination comprises at a pressure of between about 100 PSIG and about 500 PSIG.

11. The method of claim 1, wherein hydrothermally processing the combination comprises exposing the combination to a pressure of between about 100 PSIG and about 500 PSIG.

12. The method of claim 1, further comprising combining the gel with soil.

13. The method of claim 1, comprising at least one member selected from the group consisting of dry milling the combination and wet milling the combination.

14. An alkali metal ion source formed by the method of claim 1,

wherein the alkali metal ion source has a Brunauer-Emmett-Teller (BET) specific surface area between about 3 m²/g and about 10 m²/g.

15. The alkali metal ion source of claim 14, wherein the particulate alkali metal ion bearing framework silicate comprises at least one member selected from the group consisting of lithium, sodium and potassium.

16. The alkali metal ion source of claim 14, wherein the particulate alkali metal ion bearing framework silicate comprises potassium.

17. The alkali metal ion source of claim 14, wherein the particulate alkali metal ion bearing framework silicate comprises an aluminosilicate.

18. The alkali metal ion source of claim 14, wherein the particulate alkali metal ion bearing silicate framework comprises at least one member selected from the group consisting of potassium feldspar (KAlSi₃O₈), leucite (KAlSi₂O₆), kalsilite (KAlSiO₄) and nepheline (Na₃KAl₄Si₄O₁₆).

19. The alkali metal ion source of claim 14, wherein the particulate alkali metal ion bearing framework silicate comprises at least about 5% by weight of an equivalent amount of K₂O.

20. The alkali metal ion source of claim 14, wherein the particulate alkali metal ion bearing framework silicate comprises at least one member selected from the group consisting of syenite, nepheline syenite, and granite.