Methods for preparing compositions which comprise magnesium borohydride, and related materials
View Patent ↗Disclosed herein is a method for preparing magnesium borohydride. The method includes the step of reacting a metal borohydride with a metal salt composition in a solvent, to form a reaction mixture. The metal salt composition comprises at least one magnesium salt. The metal borohydride and the metal salt composition are insoluble in the solvent. The method further includes the step of grinding the reaction mixture to produce a composition that includes magnesium borohydride; and removing the solvent from the composition. Another embodiment of this invention relates to a new material. The material is an orthorhombic crystal phase of magnesium borohydride.
1. A method for preparing magnesium borohydride, comprising the following steps:
reacting a metal borohydride with a metal salt composition in a solvent to form a reaction mixture, wherein the metal salt composition comprises at least one magnesium salt; and both the metal borohydride and the metal salt composition are insoluble in the solvent;
grinding the reaction mixture to produce a composition that comprises magnesium borohydride;
removing the solvent from the composition that comprises magnesium borohydride; and
heating the composition that comprises magnesium borohydride to a temperature of from about 180° C. to about 250° C.
2. The method of claim 1 , further comprising separating the composition that comprises magnesium borohydride from insoluble reactants and reaction products.
3. The method of claim 1 , wherein the grinding is conducted using ball milling, milling in a Wiley mill, hammer milling, rod milling, semi autogenous milling, autogenous milling, pebble milling, milling using high pressure grinding rolls, milling in a Buhrstone mill, or a combination comprising at least one of the foregoing grinding operations.
4. The method of claim 3 wherein the ball milling is carried out in a rolling ball mill or in a planetary ball mill.
5. The method of claim 1 , wherein removal of the solvent is carried out in a vacuum.
6. The method of claim 1 , wherein the metal borohydride is selected from the group consisting of sodium borohydride, potassium borohydride, calcium borohydride, strontium borohydride, and combinations comprising at least one of the foregoing metal borohydrides.
7. The method of claim 1 , wherein the magnesium salt is selected from the group consisting of chloride salts, sulfate salts, phosphates, triflates, and combinations thereof.
8. The method of claim 1 , wherein the magnesium salt comprises at least two metals, one of which is magnesium.
9. The method of claim 8 , wherein the at least two metals includes lithium.
10. The method of claim 1 , wherein the metal salt composition comprises magnesium chloride.
11. The method of claim 1 , wherein the molar ratio of the borohydride (BH 4 ) group in the metal borohydride to the magnesium salt in the metal salt composition is about 2:1 to about 6:1.
12. The method of claim 11 , wherein the molar ratio of the borohydride (BH 4 ) group in the metal borohydride to the magnesium salt in the metal salt composition is about 2:1 to about 3:1.
13. The method of claim 1 , wherein a molar ratio of the solvent to the sum of the metal borohydride and the metal salt composition is about 50:1 to about 100:1.
14. The method of claim 1 , wherein the solvent comprises an alkyl ether.
15. The method of claim 14 , wherein the alkyl ether is selected from the group consisting of methyl ether, ethyl ether, propyl ether, and combinations comprising at least one of the foregoing alkyl ethers.
16. The method of claim 1 , wherein the solvent comprises an alkyl amine.
17. The method of claim 1 , wherein removing the solvent is carried out by a technique which comprises evaporation in vacuum.