High temperature layered mixed-metal oxide materials with enhanced stability

Patent metadata

Field	Value
Publication number	US-10252245-B2
Application number	US-201715453056-A
Country	US
Kind code	B2
Filing date	Mar 8, 2017
Priority date	Mar 17, 2016
Publication date	Apr 9, 2019
Grant date	Apr 9, 2019

Abstract

Embodiments of the present disclosure are directed towards methods for preparing mixed-metal oxide particles by heating adamantane-intercalated layered double-hydroxide (LDH) particles at a reaction temperature of from 400° C. to 800° C. to form mixed-metal oxide particles. The adamantane-intercalated LDH particles have a general formula [M 1-x Al x (OH) 2 ](A) x .mH 2 O, where x is from 0.14 to 0.33, m is from 0.33 to 0.50, M is chosen from Mg, Ca, Co, Ni, Cu, or Zn, and A is adamantane carboxylate, and an aspect ratio greater than 100. The aspect ratio is defined by the width of an adamantane-intercalated LDH particle divided by the thickness of the adamantane-intercalated LDH particle. The mixed-metal oxide particles comprise a mixed-metal oxide phase containing M, Al or Fe, and carbon.

First claim

What is claimed is:

1. A method for preparing mixed-metal oxide particles comprising:
heating adamantane-intercalated layered double-hydroxide (LDH) particles to a reaction temperature of from 400 ° C. to 800 ° C. to form mixed-metal oxide particles,

where:
the adamantane-intercalated LDH particles have
a length and a width;
a general formula [M 1 - x Al x (OH) 2 ](A) x .mH 2 O, where x is from 0.14 to 0.33, m is from 0.33 to 0.50, M is chosen from Mg, Ca, Co, Ni, Cu, or Zn, and A is adamantane carboxylate; and
an aspect ratio greater than 100 where the aspect ratio is defined by the width of an adamantane-intercalated LDH particle divided by the thickness of the adamantane-intercalated LDH particle; and

the mixed-metal oxide particles comprise a mixed-metal oxide phase containing M, Al, and carbon.

2. The method of claim 1 where the mixed-metal oxide particles further comprise an oxide phase having a formula MO.

3. The method of claim 1 where the mixed-metal oxide particles comprises less than 5 wt %, by weight of the mixed-metal oxide particles, of spinel-phases having a formula MAl 2 O 4 .

4. The method of claim 1 where the mixed-metal oxide particles do not include any spinel-phases having a formula MAl 2 O 4 .

5. The method of claim 1 where the mixed-metal oxide particles consist essentially of the mixed-metal oxide phase and an oxide phase having a formula MO, and the mixed-metal oxide particles do not include any spinel-phase having a formula MAl 2 O 4 .

6. The method of claim 5 where the mixed-metal oxide phase is positioned between chains of the oxide phase.

7. The method of claim 1 where the heating up to the reaction temperature is at a heating rate of 4 to 6° C/min.

8. The method of claim 7 where the heating involves holding at the reaction temperature for at least 4 hours.

9. The method of claim 7 , where M is Mg.

10. The method of claim 1 where the heating of the adamantane-intercalated layered double-hydroxide (LDH) particles is from an initial temperature of 20° C. to 30° C. to the reaction temperature of 400° C. to 800° C.

Assignees

• Saudi Arabian Oil Co
• Univ Durham

Inventors

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

Classifications

• B01J20/28028

  Particles immobilised within fibres or filaments · CPC title

• B01J2220/46

  Materials comprising a mixture of inorganic and organic materials (materials coated or impregnated on a carrier B01J20/32) · CPC title

• B01D2255/20753

  Nickel · CPC title

• B01D2255/20792

  Zinc · CPC title

• B01J31/069

  Hybrid organic-inorganic polymers, e.g. silica derivatized with organic groups (nitrogen containing groups on mineral substrates B01J31/0254; organometallic polymers B01J31/123; coordination complexes immobilised on an inorganic support B01J31/1616; coordination polymers, e.g. metal-organic frameworks B01J31/1691) · CPC title