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-10105684-B2
Application number	US-201715453106-A
Country	US
Kind code	B2
Filing date	Mar 8, 2017
Priority date	Mar 17, 2016
Publication date	Oct 23, 2018
Grant date	Oct 23, 2018

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 adamantane carboxylate salt, the method comprising:
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; and
hydrothermally treating the reactant mixture at a reaction temperature for a reaction time to form the transition-metal adamantane carboxylate salt.

2. The method of claim 1 , wherein the diamondoid compound is 1-adamantane carboxylic acid and the transition metal hydroxide has the formula M(OH) 2 , where M is chosen from Co, Cu, and Ni.

3. The method of claim 2 , wherein the transition-metal hydroxide and the 1-adamantane carboxylic acid are mixed in amounts that provide a ratio of M 2+ to 1-adamantane carboxylic acid in the reaction mixture of from 0.5:1 to 1.0:1.

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

5. The method of claim 1 , wherein the transition-metal hydroxide is Ni(OH) 2 and the reaction temperature is 150° 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 temperature is from 100° C. to 180° C.

8. A method for preparing a nanocomposite, the method comprising:
thermally decomposing a transition-metal adamantane carboxylate salt to form the nanocomposite;
the transition-metal adamantane carboxylate salt prepared by:
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; and
hydrothermally treating the reactant mixture at a reaction temperature for a reaction time to form the transition-metal adamantane carboxylate salt.

9. The method of claim 8 , wherein thermally decomposing the transition-metal adamantane carboxylate salt comprises heating the transition-metal adamantane carboxylate salt in air at a decomposition temperature for a decomposition time.

10. The method of claim 9 , wherein the decomposition temperature is at least 450° C.

11. The method of claim 9 , wherein the nanocomposite comprises transition-metal oxide particles dispersed on a carbon support.

12. The method of claim 8 , wherein the 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 nanocomposite.

13. The method of claim 8 , wherein the transition-metal adamantane carboxylate salt comprises Co-AC.

14. The method of claim 13 , wherein the nanocomposite comprises a microporous matrix and crystallites of cobalt oxide.

15. The method of claim 8 , wherein the transition-metal adamantane carboxylate salt comprises Ni-AC.

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

17. The method of claim 8 , wherein the transition-metal adamantane carboxylate salt comprises Cu-AC.

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

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

20. A catalyst system comprising:
(a) a transition-metal adamantane carboxylate salt prepared by:
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; and
hydrothermally treating the reactant mixture at a reaction temperature for a reaction time to form the transition-metal adamantane carboxylate salt;

(b) a nanocomposite prepared by:
thermally decomposing the transition-metal adamantine carboxylate salt of (a) to form the nanocomposite; or
(c) a mixture of (a) and (b).

Assignees

• Saudi Arabian Oil Co
• Univ Durham

Inventors

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

Classifications

• C01G53/04

  Oxides · CPC title

• B01J21/18

  Carbon · CPC title

• C01G53/02

  Carbonyls · CPC title

• C01G3/02

  Oxides; Hydroxides · CPC title

• B01J37/086

  Decomposition of an organometallic compound, a metal complex or a metal salt of a carboxylic acid · CPC title