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-2018333701-A1
Application number	US-201815971634-A
Country	US
Kind code	A1
Filing date	May 4, 2018
Priority date	May 19, 2017
Publication date	Nov 22, 2018
Grant date	—

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

• B01J20/3078

  Thermal treatment, e.g. calcining or pyrolizing · CPC title

• B01D15/08

  Selective adsorption, e.g. chromatography · CPC title

• B01J20/205

  Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs (carbon nanotubes per se C01B32/15) · CPC title

• C09K2208/10

  Nanoparticle-containing well treatment fluids · CPC title

• C01G53/04 Primary

  Oxides · CPC title