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(12) Patent Application Publication (10) Pub. No.: US 2017/0113189 A1 ATIEH Et Al US 20170113189A1 (19) United States (12) Patent Application Publication (10) Pub. No.: US 2017/0113189 A1 ATIEH et al. (43) Pub. Date: Apr. 27, 2017 (54) FABRICATION OF CARBON NANOTUBE (52) U.S. Cl. MEMBRANES CPC ....... BOID 67/0083 (2013.01); B0ID 71/024 (2013.01); B0ID 71/021 (2013.01); B0ID (71) Applicant: King Fahd University of Petroleum 69/04 (2013.01); C02F I/288 (2013.01); B0ID and Minerals, Dhahran (SA) 69/12 (2013.01); B01D 2325/02 (2013.01); B01D 2323/46 (2013.01); B01D 2323/08 (72) Inventors: Muataz Ali ATIEH, Dahran (SA): (2013.01); C02F 2101/10 (2013.01) Ihsanullah, Dhahran (SA); Tahar Laoui, Dhahran (SA) (57) ABSTRACT (73) Assignee: King Fahd University of Petroleum A process for making an iron oxide impregnated carbon and Minerals, Dhahran (SA) nanotube membrane. In this template-free and binder-free process, iron oxide nanoparticles are homogeneously dis (21) Appl. No.: 14/919,331 persed onto the Surface of carbon nanotubes by wet impreg nation. The amount of iron oxide nanoparticles loaded on the (22) Filed: Oct. 21, 2015 carbon nanotubes range from 0.25-80% by weight per total Publication Classification weight of the doped carbon nanotubes. The iron oxide doped carbon nanotubes are then pressed to form a carbon nano (51) Int. Cl. tube disc which is then sintered at high temperatures to form BOLD 67/00 (2006.01) a mixed matrix membrane of iron oxide nanoparticles homo BOLD 69/12 (2006.01) geneously dispersed across a carbon nanotube matrix. Meth CO2F I/28 (2006.01) ods of characterizing porosity, hydrophilicity and fouling BOID 71/02 (2006.01) potential of the carbon nanotube membrane are also BOLD 69/04 (2006.01) described. {x Water Tolecule Eron oxide particles Carbor ranotubes N ion oxide impregnated C3rton anothe intenniae Patent Application Publication Apr. 27, 2017. Sheet 1 of 8 *….......…«**-* Patent Application Publication Apr. 27, 2017. Sheet 2 of 8 US 2017/0113189 A1 g is N S. g S. Patent Application Publication Apr. 27, 2017. Sheet 3 of 8 US 2017/0113189 A1 G. 33 FG, 3C FG. 3 F. 3 Patent Application Publication Apr. 27, 2017. Sheet 4 of 8 US 2017/0113189 A1 8 -: g s x: 8 S * 8 M SS . SO ---------------------------------------------------------------------------------------------------------------------------------------------------- 38 AO Si 8 iron oxide content % 8 ran oxide context% F.G. 5 Patent Application Publication Apr. 27, 2017. Sheet 5 of 8 US 2017/0113189 A1 FG. A F. 63 G. SC FG. 6 F.C. s. Patent Application Publication Apr. 27, 2017. Sheet 6 of 8 US 2017/0113189 A1 sap?uedappiouol? Patent Application Publication Apr. 27, 2017. Sheet 7 of 8 US 2017/0113189 A1 Patent Application Publication Apr. 27, 2017. Sheet 8 of 8 US 2017/0113189 A1 M&M, C-3% for xide M& CN.8% for oxide ...:... CN-23% iro: Oxide: ^x-CN.30% iror oxide • CN-SO% iro: Oxide 2 { &x s: ----- 8. •&s -% or oxide {{ . w& CN:-30% if c oxie: & . --- CN-2%-3% or x8& xxx CN-33% in oxide 28 . X& C.5% of xidia .....................;....................................................................................................... 2 40 6 80 . intensin} F. US 2017/0113189 A1 Apr. 27, 2017 FABRICATION OF CARBON NANOTUBE iron oxide magnetic composites for Ni(II) and Sr(II). J MEMBRANES Hazard Mater 2009. 64:923-928; DiZ C, Li YH, Laun Z K, Liang J. Adsorption of chromium(VI) ions from water by BACKGROUND OF THE INVENTION carbon Nanotubes. Adsorpt SciTechnol 2004. 22:467-474; 0001 Technical Field Wang S G, Gong W X, Liu X W. Yao Y W. Gao BY, Yue 0002 The present invention relates to a manufacturing QY. Removal of lead(II) from aqueous solution by adsorp process in the field of nanotechnology. More particularly, the tion onto manganese oxide-coated carbon nanotubes. Sep present invention relates to a process for preparing carbon Purif Technol 2007. 58:17-23 each incorporated herein by nanotube membranes that are impregnated with iron oxide. reference in its entirety. Various experimental studies have The carbon nanotube membranes prepared by this process reported the adsorption of heavy metal ions, Small molecules are Suitable for water desalination and purification applica like hydrogen and oxygen, organic chemicals and radionu tions. Membranes containing iron oxide-impregnated car clides on different CNTs (closed- or open-ended CNTs, bon nanotubes and an iron oxide binder and/or matrix are single walled or multiwalled) Li Y H. Ding J, Luan Z. Di also included in the invention. Z, Zhu Y. Xu C, Wu D. Wei B. Competitive adsorption of 0003. Description of the Related Art Pb", Cu" and Cd" ions from aqueous solutions by mul 0004. The “background description provided herein is tiwalled carbon nanotubes. Carbon 2003. 4:2787-2792: for the purpose of generally presenting the context of the Chen C. Wang X. Adsorption of Ni(II) from aqueous solu disclosure. Work of the presently named inventors, to the extent it is described in this background section, as well as tion using oxidized multiwall carbon nanotubes. Ind Eng aspects of the description which may not otherwise qualify Chem Res 2006. 45:9144-9149; Chen C L. Wang X K, as prior art at the time of filing, are neither expressly or Nagatsu M. Europium adsorption on multiwall carbon nano impliedly admitted as prior art against the present invention. tube/iron oxide magnetic composite in the presence of 0005 Water is the non-substitutional natural resource and polyacrylic acid. Environ SciTechnol 2009. 43:2362-2367: most essential substance for all life on earth. Reliable access Chen C H., Huang C C. Hydrogen adsorption in defective to clean and affordable water is considered to be one of the carbon nanotubes. Sep Purif Technol 2009. 65:305-310; most basic humanitarian goals, and remains a major chal Gaur A, Shim M. Substrate-enhanced O. adsorption and lenge for the 21 century. Good quality water (i.e. pollutant complexity in the Raman G-band spectra of individual free water) is not only crucial for human health but also as metallic carbon nanotubes. Phys Rev B 2008. 78:1254221 an essential feedstock for various industries including pet 7: Varlot K M, McRae E. Pavlovsky N. D. Comparative rochemicals, oil and gas, food and pharmaceuticals. adsorption of simple molecules on carbon nanotubes depen 0006 Our current water supply faces massive challenges, dence of the adsorption properties on the nanotube morphol both old and new. Worldwide, some 780 million people still ogy. Appl Surf Sci 2002. 196: 209-215: Goering J, Kadossov lack access to safe drinking water (WHO, 2012) Qu X, E. Burghaus U. Adsorption kinetics of alcohols on single Alvarez, PJ J. Li Q. Applications of nanotechnology in water wall carbon nanotubes: an ultrahigh vacuum surface chem and wastewater treatment. Water Res 2013. 47: 3931 istry study. J Phys Chem C2008. 112:1.0114-10124; Hyung 3946 incorporated herein by reference in its entirety. H. Kim J H. Natural organic matter (NOM) adsorption to Water use has been growing at more than twice the rate of multi-walled carbon nanotubes: effect of NOM characteris population increase in the last century. As per a report from tics and water quality parameters. Environ SciTechnol 2008. the United Nations (UN), by 2025, 1800 million people will 42: 4416-4421—each incorporated herein by reference in its be facing absolute water scarcity, and two-thirds of the entirety. world population could be under stress conditions Qu X, 0009 CNTs have recently attracted considerable atten Alvarez, PJ J. Li Q. Applications of nanotechnology in water tion for synthesis of novel membranes with attractive fea and wastewater treatment. Water Res 2013. 47: 3931-3946; tures for water purification Iijima S. Ichihashi, T. Ando Y. Kar S. Bindal R C, Tewari P. K. Carbon nanotube mem Pentagons, heptagons and negative curvature in graphite branes for desalination and water purification: Challenges microtubule growth. Nature 1992. 356:776-778; Holt J K, and opportunities. Nano Today 2012. 7: 385-389—each Noy A, Huser T. Eaglesham D. Bakajin O. Fabrication of a incorporated herein by reference in its entirety. carbon Nanotube-embedded silicon nitride membrane for 0007 Nanotechnology has great potential in wastewater studies of nanometer-scale mass transport. Nano Lett 2004. treatment for providing environmentally acceptable water. 4:224.5-2250—each incorporated herein by reference in its Nanomaterials have many key physicochemical properties entirety. CNTs can also be used as direct filters and effective that make them suitable for water treatment. On mass fillers to improve the membrane performance. CNTs have balance they have higher Surface area than bulk materials. proven to be excellent filler in membrane due to improved Thus they are ideal building blocks for developing high permeability, rejection, disinfection and antifouling behav capacity sorbents with the ability to be functionalized to ior. The flux through CNTs has been estimated to be 3-4 enhance their affinity and selectivity. orders of magnitude faster than predicted by the Hagen 0008 Various nanostructured materials like Zeolites, Poiseuille equation Li S, Liao G, Liu Z, Pan Y. Wu Q, Weng metal/metal-oxide nanoparticles, dendrimers and carbon Y. Zhang X, Yang Z, Tsuid O KC. Enhanced water flux in nanotubes (CNTs) have been widely employed in water vertically aligned carbon nanotube arrays and polyetherSul purification. However, carbon nanotubes are considered as a fone composite membranes. J Mater Chem A 2014. 2:12171 versatile and unique material due to their extraordinary 12176; Majumder M, Chopra N, Andrews R, Hinds B J. electrical, thermal and mechanical properties. CNTs have Nanoscale hydrodynamics: Enhanced flow in carbon nano been widely employed for the removal of various contami tubes. Nature 2005. 438:44; Holt J.
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