# US 10,245,576 B1 · Magnetic polymer nanocomposite for removal of divalent heavy metal ions from water

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- Number: US 10,245,576 B1
- Document ID: US10245576B1
- Status: Granted
- Kind: B1
- Application number: 16/137,472
- Filed: 2018-09-20
- Granted: 2019-04-02
- Earliest claimed: 2018-09-20
- Assignees: King Saud University
- Applicants: King Saud University
- Inventors: Ayoub Abdullah Alqadami; Moonis Ali Khan; Zeid Abdullah Alothman; Ibrahim Hotan Alsohaimi; Masoom Raza Siddiqui; Ayman A. Ghfar
- Web page: https://patentgrep.com/patent/US10245576B1

## CPC

- B01J 20/261: {obtained by reactions only involving carbon to carbon unsaturated bonds (macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds per se C08F)}
- B01J 20/06: comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J 20/28009: {Magnetic properties}
- B01J 20/28033: {Membrane, sheet, cloth, pad, lamellar or mat}
- B01J 20/3085: {Chemical treatments not covered by groups B01J20/3007 - B01J20/3078}
- B01J 20/3425: {of sorbents or filter aids comprising organic materials}
- B01J 20/3475: {in the liquid phase}
- C02F 1/288: {using composite sorbents, e.g. coated, impregnated, multi-layered}
- C02F 1/488: {for separation of magnetic materials, e.g. magnetic flocculation}
- C02F 1/66: by neutralisation; pH adjustment (for degassing C02F1/20; using ion-exchange C02F1/42; for flocculation or precipitation of suspended impurities C02F1/52; for removing dissolved compounds C02F1/58)
- H01F 1/0054: {Coated nanoparticles, e.g. nanoparticles coated with organic surfactant}
- H01F 1/42: of organic or organo-metallic materials {, e.g. graphene}(H01F1/44 takes precedence)
- C02F 1/281: {using inorganic sorbents}
- C02F 1/285: {using synthetic organic sorbents}
- C02F 2101/20: Heavy metals or heavy metal compounds
- C02F 2303/16: Regeneration of sorbents, filters
- C02F 2305/08: Nanoparticles or nanotubes
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C02F: TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE (separation in general B01D; special arrangements on waterborne vessels of installations for treating water, waste water or sewage, e.g. for producing fresh water, B63J; adding materials to water to prevent corrosion C23F; treating radioactively-contaminated liquids G21F9/04; regeneration of reactants for recirculation into processes, see the relevant places for the processes)
- H01F: MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES

## Abstract

The magnetic polymer nanocomposite for removal of divalent heavy metal ions from water is magnetic nanocomposite having a core of magnetite (Fe3O4) in a shell of branched polyhydroxystyrene (BHPS), designated as Fe3O4@BHPS. The nanocomposite is synthesized by co-precipitation in alkali solution. Testing showed the nanocomposite reached 93% and 80% Pb(II) and Cd(II) adsorption, respectively, in 30 minutes, attaining equilibrium in 120 minutes. The maximum adsorption capacities of Pb(II) and Cd(II) at 298K were 186.2 and 125 mg/g, respectively. After adsorption, the nanocomposite with the heavy metal(s) adsorbed thereto was easily removed from aqueous solution by application of a magnetic field.

## Claims

### Claim 1

A method of making a magnetic polymer nanocomposite, comprising the steps of:
dissolving FeCl3 and FeCl2 separately in HCl to form an Fe(III) solution and an Fe(II) solution, respectively;
combining the Fe(III) solution and the Fe(II) solution to form a combined solution;
adding a solution of branched polyhydroxystyrene (BPHS) in methanol and a solution of ammonium hydroxide to the combined solution dropwise to form a mixture; and
stirring the mixture under nitrogen atmosphere to precipitate the magnetic polymer nanocomposite as Fe3O4 nanoparticles in a BPHS shell (Fe3O4@ BPHS).

### Claim 2 (depends on 1)

The method of making a magnetic polymer nanocomposite according to claim 1, further comprising the step of removing the precipitated magnetic polymer nanocomposite by application of an external magnetic field.

### Claim 3 (depends on 1)

The method of making a magnetic polymer nanocomposite according to claim 1, wherein said step of adding a solution of branched polyhydroxystyrene (BPHS) in methanol and a solution of ammonium hydroxide to the combined solution dropwise comprises adding a solution of branched polyhydroxystyrene (BPHS) in methanol and a solution of ammonium hydroxide to the combined solution dropwise until a pH of 10 is obtained.

### Claim 4 (depends on 1)

The method of making a magnetic polymer nanocomposite according to claim 1, wherein said step of dissolving FeCl3 and FeCl2 separately in HCl to form an Fe(III) solution and an Fe(II) solution further comprises dissolving the FeCl2 in HCl in the presence of a flow of nitrogen gas to prevent oxidation of Fe(II).

### Claim 5 (depends on 1)

The method of making a magnetic polymer nanocomposite according to claim 1, wherein said solution of ammonium hydroxide comprises a 28% NH4OH solution.