Synthesis of transition-metal adamantane salts and oxide nanocomposites, and systems and methods including the salts or the nanocomposites

Patent metadata

Field	Value
Publication number	US-10906028-B2
Application number	US-201815971634-A
Country	US
Kind code	B2
Filing date	May 4, 2018
Priority date	May 19, 2017
Publication date	Feb 2, 2021
Grant date	Feb 2, 2021

Abstract

A method for preparing a transition-metal adamantane carboxylate salt is presented. The method includes mixing a transition-metal hydroxide and a diamondoid compound having at least one carboxylic acid moiety to form a reactant mixture, where M is a transition metal. Further, the method includes hydrothermally treating the reactant mixture at a reaction temperature for a reaction time to form the transition-metal adamantane carboxylate salt.

First claim

What is claimed is:

1. A method for preparing a transition metal nanocomposite, the method comprising:
mixing a transition metal hydroxide and a diamondoid compound having at least one carboxylic acid moiety to form a reactant mixture;
hydrothermally treating the reactant mixture at a reaction temperature for a reaction time to form a transition-metal adamantane carboxylate salt; and
thermally decomposing the transition-metal adamantane carboxylate salt in a reducing atmosphere at a decomposition temperature for a decomposition time to form the transition metal nanocomposite.

2. The method of claim 1 , wherein the diamondoid compound is 1-adamantane carboxylic acid and the transition metal hydroxide has an oxidation state of M+2, where M is chosen from cobalt (Co), copper (Cu), or combinations of cobalt and copper.

3. The method of claim 2 , wherein the transition metal hydroxide and the 1-adamantane carboxylic acid are mixed in amounts that provide a molar ratio of M 2+ to 1-adamantane carboxylic acid in the reaction mixture of from 0.5:1 to 1:1.

4. The method of claim 1 , wherein the reaction temperature is from 100° C. to 180° C.

5. The method of claim 1 , wherein the transition metal hydroxide is Co(OH) 2 and the reaction temperature is 110° C.

6. The method of claim 1 , wherein the transition-metal hydroxide is Cu(OH) 2 and the reaction temperature is 110° C.

7. The method of claim 1 , wherein the reaction time is at least 12 hours.

8. The method of claim 1 , wherein thermally decomposing the transition-metal adamantane carboxylate salt further comprises heating the transition-metal adamantane carboxylate salt from room temperature to the decomposition temperature at a rate of 5° C. per minute, and wherein the decomposition temperature is at least 450° C.

9. The method of claim 1 , wherein the decomposition time is at least 4 hours.

10. The method of claim 1 , wherein the transition metal nanocomposite comprises transition metal oxide particles.

11. The method of claim 10 , wherein the transition metal nanocomposite comprises from 70 wt. % to 80 wt. % metal oxide and from 20 wt. % to 30 wt. % carbon, based on the total weight of the transition metal nanocomposite.

12. The method of claim 1 , wherein the transition-metal adamantane carboxylate salt comprises cobalt adamantane carboxylate.

13. The method of claim 12 , wherein the cobalt adamantane carboxylate comprises CoO, Co 3 O 4 , or a mixture of CoO and Co 3 O 4 .

14. The method of claim 1 , wherein the transition-metal adamantane carboxylate salt comprises Ni-AC.

15. The method of claim 14 , wherein the transition metal nanocomposite comprises crystallites of NiO configured as porous nanowhiskers.

16. The method of claim 1 , wherein the transition-metal adamantane carboxylate salt comprises Cu-AC.

17. The method of claim 16 , wherein the transition metal nanocomposite comprises carbon sheets and nanoparticles of copper oxide supported on carbon sheets.

18. The method of claim 17 , wherein the copper oxide comprises CuO, Cu 2 O, or a mixture of CuO and Cu 2 O.

19. A method for catalyzing a chemical reaction between at least one first reactant and at least one second reactant, the method comprising:
reacting the at least one first reactant and at least one second reactant in the presence of a catalyst system comprising the transition metal nanocomposite prepared according to claim 1 .

20. An electrode comprising the transition metal nanocomposite prepared according to claim 1 .

Assignees

• Saudi Arabian Oil Co
• Univ Durham

Inventors

• Veerabhadrappa Manohara Gudiyor
• Greenwell Hugh Christopher
• Whiting Andrew
• Hall John Adrian
• Alabedi Gasan

Classifications

• B01J35/45

  Nanoparticles · CPC title

• H01B1/14

  Conductive material dispersed in non-conductive inorganic material · CPC title

• C01P2004/04

  obtained by TEM, STEM, STM or AFM · CPC title

• C01P2004/03

  obtained by SEM · CPC title

• C01P2002/82

  by IR- or Raman-data · CPC title