CaB2O4/PbO/CuO/Pb3O4/PbB2O4/Pb4O(BO3)2 nanocomposite material and method of making

Patent metadata

Field	Value
Publication number	US-12486169-B1
Application number	US-202519037087-A
Country	US
Kind code	B1
Filing date	Jan 25, 2025
Priority date	Jan 25, 2025
Publication date	Dec 2, 2025
Grant date	Dec 2, 2025

Abstract

A multiphase particulate nanocomposite material comprising, as determined by X-ray diffraction: a monoclinic CuO crystalline phase; an orthorhombic CaB 2 O 4 crystalline phase; an orthorhombic PbO crystalline phase; an orthorhombic Pb 4 O(BO 3 ) 2 crystalline phase; a tetragonal Pb 3 O 4 crystalline phase, and, a PbB 2 O 4 crystalline phase. The multiphase particulate nanocomposite material has, based on the total number of atoms in the nanocomposite material: an atomic concentration of boron (B) is from about 1 to about 10 atom %; an atomic concentration of calcium (Ca) is from about 5 to about 15 atom %; an atomic concentration of copper (Cu) is from about 5 to about 15 atom %; and, an atomic concentration of lead (Pb) is from about 5 to about 15 atom %.

First claim

The invention claimed is:

1 . A multiphase particulate nanocomposite material comprising, as determined by X-ray diffraction:
a monoclinic CuO crystalline phase; an orthorhombic CaB 2 O 4 crystalline phase; an orthorhombic PbO crystalline phase; an orthorhombic Pb 4 O(BO 3 ) 2 crystalline phase; a tetragonal Pb 3 O 4 crystalline phase; and, a PbB 2 O 4 crystalline phase,
wherein, based on the total number of atoms in the nanocomposite material:
an atomic concentration of boron (B) is from about 1 to about 10 atom %;
an atomic concentration of calcium (Ca) is from about 5 to about 15 atom %;
an atomic concentration of copper (Cu) is from about 5 to about 15 atom %; and,
an atomic concentration of lead (Pb) is from about 5 to about 15 atom %.

2 . The particulate nanocomposite material according to claim 1 having a volume average crystallite size, as determined by X-ray diffraction, of from about 55 to about 60 nm.

3 . The particulate nanocomposite material according to claim 1 having a volume average crystallite size, as determined by X-ray diffraction, of from about 56 to about 58 nm.

4 . The particulate nanocomposite material according to claim 1 , wherein the nanocomposite material is in the form of particles having a matrix phase with a rough surface and in which sharp-edged plates are embedded and protrude.

5 . The particulate nanocomposite material according to claim 4 , wherein at least a fraction of the sharp-edged plates have a multilayered structure.

6 . The particulate nanocomposite material according to claim 4 , wherein the sharp edged plates have a median volume particle size (Dv50) of from about 5 to about 30 μm, as determined by Scanning Electron Microscopy.

7 . The particulate nanocomposite material according to claim 4 , wherein the sharp edged plates have a Dv90 particle diameter of less than about 50 μm, as determined by Scanning Electron Microscopy.

8 . The particulate nanocomposite material according to claim 4 further comprising granular particles having a median volume particle size (Dv50) of from about 0.1 to about 10 μm, as determined by Scanning Electron Microscopy.

9 . A method for preparing the multiphase particulate nanocomposite material as defined in claim 1 , the method comprising:
forming an aqueous mixture by adding an aqueous solution of a chelating agent to an aqueous solution of a calcium salt, a copper salt, a lead salt and boric acid; adding a polyol into the aqueous mixture to form a gel; heating the gel under stirring at a temperature of from about 200 to about 400° C. for a sufficient duration to form a dry powder; and, calcining the dry powder at a temperature of from about 500 to about 800° C. to form the nanocomposite material.

10 . The method according to claim 9 , wherein the aqueous solution of the chelating agent is added in a dropwise manner into the aqueous solution of the calcium salt, the copper salt, the lead salt and boric acid.

11 . The method according to claim 9 , wherein:
the calcium salt is selected from the group consisting of calcium sulfate (CaSO 4 ), calcium nitrate (Ca(NO 3 ) 2 ), calcium chloride (CaCl 2 ) and calcium acetate (Ca(CH 3 COO) 2 ); the copper salt is selected from the group consisting of copper sulfate (CuSO 4 ), copper nitrate (Cu(NO 3 ) 2 ), copper chloride (CuCl 2 ) and copper acetate (Cu(CH 3 COO) 2 ); and, the lead salt is selected from the group consisting of lead sulfate (PbSO 4 ), lead nitrate (Pb(NO 3 ) 2 ), lead chloride (PbCl 2 ) and lead acetate (Pb(CH 3 COO) 2 ).

12 . The method according to claim 9 , wherein:
the calcium salt is calcium nitrate (Ca(NO 3 ) 2 ); the cobalt salt is copper nitrate (Cu(NO 3 ) 2 ); and, the lead salt is lead nitrate (Pb(NO 3 ) 2 ).

13 . The method according to claim 9 , wherein the chelating agent comprises at least one hydroxyalkyl carboxylic acid selected from the group consisting of citric acid, tartaric acid, malic acid, mandelic acid and 12-hydroxystearic acid.

14 . The method according to claim 9 , wherein the chelating agent consists of tartaric acid.

15 . The method according to claim 9 , wherein the polyol is added in a dropwise manner into the aqueous mixture.

16 . The method according to claim 9 , wherein the polyol has a number average molecular weight of from about 200 to about 5000 g/mol. and an hydroxyl number of from about 25 to about 500 mg KOH/g.

17 . The method according to claim 9 , wherein the polyol is selected from the group consisting of: polyester polyols; polyether polyols; poly(ether-ester) polyols; poly(alkylene carbonate) polyols; and, mixtures thereof.

18 . The method according to claim 9 , wherein the polyol comprises a polyoxy(C 2 -C 3 )alkylene polyol.

19 . The method according to claim 18 , wherein the polyol comprises a polyoxy(C 2 -C 3 )alkylene polyol having a number average molecular weight of from about 200 to about 5000 g/mol. and an hydroxyl number of from about 25 to about 500 mg KOH/g.

20 . A method of immobilizing inorganic contaminants disposed in an aqueous medium, the method comprising contacting the aqueous medium with the multiphase particulate nanocomposite material as defined in claim 1 .

Assignees

• Imam Mohammad Ibn Saud Islamic Univ

Inventors

• Ahmed Ehab Abdelhamed Abdelrahman
• Algethami Faisal Khuwayshan Lafi

Classifications

• C01P2002/60

  Compounds characterised by their crystallite size · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• C01P2004/61

  Micrometer sized, i.e. from 1-100 micrometer · CPC title

• C01P2004/30

  extending in three dimensions · CPC title

• C01P2004/51

  Particles with a specific particle size distribution · CPC title