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-2017266643-A1
Application number	US-201715453106-A
Country	US
Kind code	A1
Filing date	Mar 8, 2017
Priority date	Mar 17, 2016
Publication date	Sep 21, 2017
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 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 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

• C01P2002/82

  by IR- or Raman-data · CPC title

• C07C51/412 Primary

  by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part · CPC title

• B01J37/04

  Mixing {(B01J37/0009, B01J37/0018 take precedence)} · CPC title

• B01J21/18

  Carbon · CPC title

• C07C2603/74

  Adamantanes · CPC title