High aspect ratio layered double hydroxide materials and methods for preparation thereof

Patent metadata

Field	Value
Publication number	US-2017267623-A1
Application number	US-201715449207-A
Country	US
Kind code	A1
Filing date	Mar 3, 2017
Priority date	Mar 17, 2016
Publication date	Sep 21, 2017
Grant date	—

Abstract

Embodiments are directed to adamantane-intercalated layered double-hydroxide (LDH) particles and the methods of producing adamantane-intercalated LDH particles. The method comprises adding to an aqueous solution a first precursor and a second precursor to form an initial mixture, where the first precursor is Al(OH) 3 or Al 2 O 3 , the second precursor is a hydroxide M(OH) 2 or an oxide MO, where M is a metal of oxidation state +2; and the initial mixture has a M/Al molar ratio of from 1 to 5. The method also comprises adding to the initial mixture an amount of adamantane to form a reaction mixture having an Al/adamantane molar ratio of from 0.5 to 2; and heating the reaction mixture to produce adamantane-intercalated LDH particles, where the adamantane-intercalated LDH particles have aspect ratios greater than 100.

First claim

What is claimed is:

1 . A method for preparing adamantane-intercalated layered double-hydroxide (LDH) particles, the method comprising:
adding to an aqueous solution a first precursor and a second precursor to form an initial mixture, where:
the first precursor is Al(OH) 3 or Al 2 O 3 ;
the second precursor is a hydroxide M(OH) 2 or an oxide MO, where M is a metal of oxidation state +2; and
the initial mixture has a M/Al molar ratio from 1 to 5;
the initial mixture has a solid loading of less than 10 weight % solids, based on a total weight of the initial solution;
adding to the initial mixture an amount of adamantane to form a reaction mixture having an Al/adamantane molar ratio from 0.5 to 2; and heating the reaction mixture to produce the adamantane-intercalated LDH particles, where the adamantane-intercalated LDH particles have an aspect ratio greater than 100, the aspect ratio defined by a width of an adamantane-intercalated LDH particle divided by a thickness of the adamantane-intercalated LDH particle.

2 . The method of claim 1 further comprising stirring the reaction mixture.

3 . The method of claim 1 where the adamantane is added as a carboxylic acid.

4 . The method of claim 1 where the heating step occurs at a reaction temperature from 110° C. to 180° C. for a reaction time of 12 hours to 48 hours.

5 . The method of claim 1 where M is chosen from Mg, Ca, Co, Ni, Cu, or Zn.

6 . The method of claim 1 where the second precursor is Mg(OH) 2 , Ca(OH) 2 , Co(OH) 2 , Ni(OH) 2 , Cu(OH) 2 , or Zn(OH) 2 .

7 . The method of claim 1 where the second precursor is Mg(OH) 2 or MgO.

8 . The method of claim 1 where the second precursor is Mg(OH) 2 and the first precursor is Al(OH) 3 .

9 . The method of claim 1 where the Al/adamantane molar ratio is from 0.8 to 1.2.

10 . The method of claim 1 where 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.

11 . The method of claim 1 where M is Mg.

12 . The method of claim 1 where the initial mixture has less than 5 weight % solids, based on the total weight of the initial mixture.

13 . The method of claim 1 where the aspect ratio is greater than 125.

14 . The method of claim 1 where the adamantane-intercalated LDH particle have a particle diameter of 5 to 10 μm.

15 . An adamantane-intercalated layered double-hydroxide (LDH) material in a form of adamantane-intercalated LDH particles, where the adamantane-intercalated LDH particles comprise:
a general formula defined by [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 defined by a width of an adamantane-intercalated LDH particle divided by a thickness of the adamantane-intercalated LDH particle.

16 . The adamantane-intercalated LDH material of claim 15 where M is Mg.

17 . The adamantane-intercalated LDH material of claim 15 where the aspect ratio is greater than 125.

18 . The adamantane-intercalated LDH material of claim 15 where the adamantane-intercalated LDH particles have a particle diameter of 5 to 10 μm.

Assignees

• Saudi Arabian Oil Co
• Univ Durham

Inventors

• Veerabhadrappa Manohara Gudiyor
• Greenwell Hugh Christopher
• Alabedi Gasan Selman
• Hall John Adrian
• Al-Shahrani Abdullah A
• Whiting Andrew

Classifications

• B01J21/10

  Magnesium; Oxides or hydroxides thereof · CPC title

• C07C61/135 Primary

  having three rings · CPC title

• C09C1/407

  Aluminium oxides or hydroxides · CPC title

• B01J31/04

  containing carboxylic acids or their salts {(B01J31/0277 - B01J31/0298 take precedence; multi-metal carboxylate complexes like Pd (II) acetate, i.e. Pd3 (OAc) 6 or Cr(II)acetate, i.e. Cr2(OAc)4 B01J31/2226)} · CPC title

• C09K21/06

  Organic materials · CPC title