Process for forming a sintered iron oxide impregnated carbon nanotube membrane

Patent metadata

Field	Value
Publication number	US-10272391-B2
Application number	US-201715651688-A
Country	US
Kind code	B2
Filing date	Jul 17, 2017
Priority date	Oct 21, 2015
Publication date	Apr 30, 2019
Grant date	Apr 30, 2019

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.

First claim

The invention claimed is:

1. A process for forming a sintered iron oxide impregnated carbon nanotube membrane, comprising:
dispersing iron oxide nanoparticles onto the surface of carbon nanotubes by wet impregnation to produce iron oxide impregnated carbon nanotube particles comprising from 1 to 50 wt. % iron oxide based on the total weight of the iron oxide impregnated carbon nanotube particles;
pressing the iron oxide impregnated carbon nanotube particles with a die to form an iron oxide impregnated carbon nanotube disc; and
sintering the carbon nanotube disc to produce the sintered iron oxide impregnated carbon nanotube membrane having a thickness of 1 to 5 mm.

2. The process of claim 1 , wherein the wet impregnation comprises:
dissolving a ferric salt in a first alcohol solvent to form a ferric salt solution having a concentration of 1-600 mM;
dissolving carbon nanotubes in a second alcohol solvent to form a carbon nanotube solution having a concentration of 25-100 g/L;
mixing and ultrasonicating the ferric salt solution and the carbon nanotube solution for 1-5 h to form a homogeneous carbon nanotube-ferric salt mixture; and
evaporating alcohol from the carbon nanotube-ferric salt mixture and calcinating the carbon nanotube-ferric salt mixture at 300-450° C. to produce the iron oxide impregnated carbon nanotube particles;
wherein the ferric salt solution and the carbon nanotube solution are of equal volumes or of volumes that differ by no more than 20-25%.

3. The process of claim 1 , wherein 0.25% to 80% of the iron oxide nanoparticles by weight per total weight of the iron oxide impregnated carbon nanotube particles are dispersed onto the surface of the carbon nanotubes.

4. The process of claim 2 , wherein during the calcinating,
ferric ions in the ferric salt solution are oxidized to form the iron oxide nanoparticles; and
the iron oxide nanoparticles are attached to and homogeneously dispersed across the surface of the carbon nanotubes.

5. The process of claim 1 , wherein the iron oxide impregnated carbon nanotube particles are pressed at 50-500 MPa.

6. The process of claim 1 , wherein the carbon nanotube disc is sintered at 1000-1500° C. for 3-8 h at a heating rate of 5-20° C./min.

7. The process of claim 1 , wherein the process excludes the use of a non-metallic binder.

8. The process of claim 1 , wherein the process excludes the use of a template.

Assignees

• Univ King Fahd Pet & Minerals

Inventors

• Atieh Muataz Ali
• Ihsanullah
• Laoui Tahar

Classifications

• B01D69/12

  Composite membranes; Ultra-thin membranes · CPC title

• B01D71/024

  Oxides · CPC title

• B01D2323/08

  Specific temperatures applied · CPC title

• B01D2325/02

  Details relating to pores or porosity of the membranes · CPC title

• B01D71/021

  Carbon · CPC title