# US 10,870,088 B1 · Composite photocatalysts embedded in microporous membranes

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- Number: US 10,870,088 B1
- Document ID: US10870088B1
- Status: Granted
- Kind: B1
- Application number: 16/594,783
- Filed: 2019-10-07
- Granted: 2020-12-22
- Earliest claimed: 2019-10-07
- Assignees: King Abdulaziz University
- Applicants: King Abdulaziz University
- Inventors: Iqbal M. I. Ismail; Abdul Hameed; Muhammad Aslam; Mohammad H. Albeirutty
- Web page: https://patentgrep.com/patent/US10870088B1

## CPC

- B01D 69/145: {containing embedded catalysts}
- B01D 67/00793: {Dispersing a component, e.g. as particles or powder, in another component}
- B01D 69/1411: {containing dispersed material in a continuous matrix}
- B01D 69/148: {Organic/inorganic mixed matrix membranes}
- B01D 71/024: {Oxides}
- B01D 71/16: Cellulose acetate
- B01J 23/10: of rare earths
- B01J 23/22: Vanadium
- B01J 23/28: Molybdenum
- B01J 23/30: Tungsten
- B01J 23/34: Manganese
- B01J 23/72: Copper
- B01J 23/80: with zinc, cadmium or mercury
- B01J 35/39: Photocatalytic properties
- B01J 35/395: {Thickness of the active catalytic layer}
- B01J 35/59: Membranes
- B01J 35/643: {less than 2 nm}
- B01J 37/031: {Precipitation}
- B01J 37/04: Mixing {(B01J37/0009, B01J37/0018 take precedence)}
- B01J 37/06: Washing {(B01J37/0009, B01J37/0018 take precedence)}
- B01J 37/08: Heat treatment {(B01J37/0009, B01J37/0018 take precedence)}
- C02F 1/32: with ultraviolet light
- C02F 1/44: by dialysis, osmosis or reverse osmosis {(general membrane separation processes B01D61/00, membrane modules B01D63/00, electrodialysis C02F1/4693, combination of membrane modules and bioreactors C02F3/1268)}
- C02F 1/725: {by catalytic oxidation}
- B01J 2235/30: Scanning electron microscopy; Transmission electron microscopy
- C02F 2101/345: {Phenols}
- C02F 2101/36: containing halogen
- C02F 2101/38: containing nitrogen
- C02F 2303/04: Disinfection
- C02F 2305/10: Photocatalysts
- Y02W 10/37: using solar energy
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- 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)
- Y02W: CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT

## Abstract

Photocatalytic materials with a composite photocatalyst of a metal oxide impregnated with elemental metal particles, can be embedded into a hydrophilic polymer having pores with diameters of less than 2 nm, to provide a useful water remediation and/or purification product. The metal oxide may be WO3, Ce2, Bi2O3, NiO, TiO2, and/or ZnO, and the elemental metal particles, impregnated or compounded into the metal oxide, may be Fe, Co, Ni, Cu, Ag, Ce, Mn, Mo, V, Bi, Sn, W, Nb, Pd, and/or Pt. The photocatalytic materials may be easily removed and/or retrieved after use, and can effectively combat both chemical and biological contamination and/or fouling of water as well as the membranes composed of the photocatalytic material.

## Claims

### Claim 1

A photocatalytic material, comprising:
a composite photocatalyst comprising a metal oxide impregnated with elemental metal particles; and
a hydrophilic polymer membrane having pores with diameters of less than 2 nm, wherein the hydrophilic polymer membrane comprises a hydrophilic polymer,
wherein the composite photocatalyst is dispersed within the hydrophilic polymer membrane, wherein at least 95 wt % of the composite photocatalyst is completely enveloped within the hydrophilic polymer membrane,
wherein the metal oxide comprises WO3, CeO2, Bi2O3, and/or ZnO, and
wherein the elemental metal particles comprise at least one elemental metal selected from the group consisting of Cu, Ce, Mn, Mo, V, and W.

### Claim 2 (depends on 1)

The material of claim 1, wherein the hydrophilic polymer comprises cellulose acetate, polyether sulfone, polysulfone, and/or polyvinylidene difluoride.

### Claim 3 (depends on 2)

The material of claim 2, wherein the hydrophilic polymer is present in the hydrophilic polymer membrane in an amount of at least 90 wt. % of all polymers present in the hydrophilic polymer membrane.

### Claim 4 (depends on 1)

The material of claim 1, wherein the metal oxide is impregnated with the elemental metal particles in an amount in a range of 0.1 to 50 wt. % of a total composite photocatalyst weight.

### Claim 5 (depends on 1)

The material of claim 1, wherein at least 95 wt. % of metal present in the elemental metal particles is in a zero oxidation state.

### Claim 6 (depends on 1)

The material of claim 1, wherein the composite photocatalyst comprises a single metal oxide.

### Claim 7 (depends on 1)

The material of claim 1, wherein the composite photocatalyst comprises a single elemental metal.

### Claim 8 (depends on 1)

The material of claim 1, wherein the composite photocatalyst comprises:
at least 95 wt. % of a single metal oxide, relative to all metal oxide present in the photocatalyst; and
at least 95 wt. % of a single elemental metal, relative to all elemental metal present in the photocatalyst.

### Claim 9 (depends on 1)

A method of preparing the material of claim 1, the method comprising:
(a) heating an aqueous solution comprising an acid, a metal salt, and miscible organic solvent to produce metal oxide comprising WO3, CeO2, Bi2O3, and/or ZnO;
(b) mixing an aqueous solution of a precursor of at least one metal selected from the group consisting of Cu, Ce, Mn, Mo, V, and W and the metal oxide to form a mixture comprising the metal embedded in the metal oxide;
(c) heating and/or calcining the mixture to form a photocatalyst;
(d) blending the photocatalyst with a solution comprising a polymer in a solvent to form a solution and/or compounding the photocatalyst with the polymer to form a compounded melt, in a mass relationship of the photocatalyst in a range of from 0.1 to 100 wt. % of a weight of the polymer, wherein the polymer is hydrophilic and comprises pores having diameters up to 2 nm; and
(e) forming a membrane.

### Claim 10 (depends on 9)

The method of claim 9, wherein the heating (a) is at a temperature in a range of from 80 to 160° C.

### Claim 11 (depends on 9)

The method of claim 9, wherein the heating (a) is for a time in a range of 2 to 24 hours.

### Claim 12 (depends on 9)

The method of claim 9, wherein the acid in the heating (a) comprises at least 25 wt. % acetic acid, relative to all acids in the mixture.

### Claim 13 (depends on 9)

The method of claim 9, wherein the solvent in the heating (a) is an alcohol.

### Claim 14 (depends on 9)

The method of claim 9, wherein the forming (e) comprises casting the solution or extruding the compounded melt.

### Claim 15 (depends on 9)

The method of claim 9, wherein the heating (c) comprises bringing the mixture to dryness, adding a flammable liquid, and igniting to form the photocatalyst.

### Claim 16 (depends on 1)

A method of preparing the material of claim 1, the method comprising:
blending the photocatalyst with a solution comprising a polymer in a solvent and/or compounding the photocatalyst with the polymer; and
forming a membrane.

### Claim 17 (depends on 1)

A method of inactivating at least one biological contaminant in water, the method comprising:
while irradiating with a source of UV and/or visible light, contacting the material of claim 1 with contaminated water.

### Claim 18 (depends on 1)

The material of claim 1, wherein the metal oxide is ZnO.

### Claim 19 (depends on 2)

The material of claim 2, wherein the hydrophilic polymer is cellulose acetate.

### Claim 20 (depends on 1)

The material of claim 1, wherein the hydrophilic polymer membrane consists of cellulose acetate.