# US 10,369,526 B2 · Carbon nanotube membranes

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- Number: US 10,369,526 B2
- Document ID: US10369526B2
- Status: Granted
- Kind: B2
- Application number: 15/651,306
- Filed: 2017-07-17
- Published: 2017-11-02
- Granted: 2019-08-06
- Earliest claimed: 2015-10-21
- Assignees: King Fahd University of Petroleum and Minerals
- Applicants: King Fahd University of Petroleum and Minerals
- Inventors: Muataz Ali Atieh; Ihsanullah; Tahar Laoui
- Web page: https://patentgrep.com/patent/US10369526B2

## CPC

- B01D 67/0083: {Thermal after-treatment}
- B01D 69/141: {Heterogeneous membranes, e.g. containing dispersed material; Mixed matrix membranes}
- B01D 67/0041: {by agglomeration of particles in the dry state}
- B01D 67/00411: {by sintering}
- B01D 69/04: Tubular membranes
- B01D 69/12: Composite membranes; Ultra-thin membranes
- B01D 69/14111: {with nanoscale dispersed material, e.g. nanoparticles}
- B01D 71/021: {Carbon}
- B01D 71/024: {Oxides}
- C02F 1/288: {using composite sorbents, e.g. coated, impregnated, multi-layered}
- 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)}
- B01D 2323/08: Specific temperatures applied
- B01D 2323/21813: Metal oxides
- B01D 2323/46: Impregnation
- B01D 2325/02: Details relating to pores or porosity of the membranes
- C02F 2101/10: Inorganic compounds
- C02F 2103/08: Seawater, e.g. for desalination
- C02F 2305/08: Nanoparticles or nanotubes
- 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)
- 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)

## Abstract

A process for making an iron oxide impregnated carbon nanotube membrane. In this template-free and binder-free process, iron oxide nanoparticles are homogeneously dispersed onto the surface of carbon nanotubes by wet impregnation. The amount of iron oxide nanoparticles loaded on the carbon nanotubes range from 0.25-80% by weight per total weight of the doped carbon nanotubes. The iron oxide doped carbon nanotubes are then pressed to form a carbon nanotube disc which is then sintered at high temperatures to form a mixed matrix membrane of iron oxide nanoparticles homogeneously dispersed across a carbon nanotube matrix. Methods of characterizing porosity, hydrophilicity and fouling potential of the carbon nanotube membrane are also described.

## Claims

### Claim 1

An iron oxide impregnated carbon nanotube disc membrane, comprising:
a matrix comprising a plurality of carbon nanotubes;
wherein:
the plurality of carbon nanotubes is randomly oriented along a two-dimensional singular axis and is impregnated with iron oxide nanoparticles on the surface;
wherein iron oxide impregnated carbon nanotube disc is obtained by die-pressing the matrix to form a die-pressed disc and sintering the die-pressed disc at temperature of from 1,000 to 1,500° C., and
the iron oxide impregnated carbon nanotube disc is binder-free.

### Claim 2 (depends on 1)

The iron oxide impregnated carbon nanotube disc membrane of claim 1, having an iron oxide nanoparticle content of 0.25-80% by weight per total weight of the carbon nanotube membrane.

### Claim 3 (depends on 1)

The iron oxide impregnated carbon nanotube disc membrane of claim 1, wherein no iron oxide nanoparticles are embedded in the inner wall of the plurality of carbon nanotubes.

### Claim 4 (depends on 1)

The iron oxide impregnated carbon nanotube disc membrane of claim 1, having a carbon nanotube density of at least 1010 cm−2.

### Claim 5 (depends on 1)

The iron oxide impregnated carbon nanotube disc membrane of claim 1, having a porosity of 50-80%.

### Claim 6 (depends on 1)

The iron oxide impregnated carbon nanotube disc membrane of claim 1, having a total pore volume of 0.05-0.5 cm3/g.

### Claim 7 (depends on 1)

The iron oxide impregnated carbon nanotube disc membrane of claim 1, having an average pore diameter of 0.05-10 μm.

### Claim 8 (depends on 2)

The iron oxide impregnated carbon nanotube disc membrane of claim 2, wherein the iron oxide nanoparticle content is at least 20% and the iron oxide nanoparticles partially aggregate to form pores having an average diameter of 0.05-20 μm on the iron oxide impregnated carbon nanotube disc membrane.

### Claim 9 (depends on 1)

The iron oxide impregnated carbon nanotube disc membrane of claim 1, having a water contact angle of 5-75°.

### Claim 10 (depends on 1)

The iron oxide impregnated carbon nanotube disc membrane of claim 1, having a water flux of 20-2000 Lm−2h−1.

### Claim 11 (depends on 1)

A method for desalinating and/or treating an aqueous sample, comprising:
contacting the aqueous sample with the iron oxide impregnated carbon nanotube disc membrane of claim 1.

### Claim 12 (depends on 1)

A water desalination or treatment system comprising one or more of the iron oxide impregnated carbon nanotube disc membranes of claim 1.