Method for preparing nanocomposite material by assembling ferriferrous oxide in halloysite tube

A nano-composite material, ferric oxide technology, applied in the direction of iron oxide/hydroxide, magnetic materials, nanotechnology, etc., to achieve the effect of improving biocompatibility and strong application advantages

Active Publication Date: 2018-05-22
CENT SOUTH UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Based on the above literature research, published patents and literature, involving SiO 2 Coated Fe 3 o 4 , Fe 3 o 4 Composite materials with halloysite, montmori

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  • Method for preparing nanocomposite material by assembling ferriferrous oxide in halloysite tube

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Embodiment 1

[0023] A preparation of halloysite tube assembled Fe by high temperature pyrolysis 3 o 4 The method for nanocomposite material, its specific preparation steps are:

[0024] Step 1. Take 10g of halloysite and disperse it in 500mL of deionized water. Stir magnetically at room temperature for 3 hours to obtain a cloudy liquid. Suction filter it. Under drying for 8 hours, the coarse halloysite was obtained;

[0025] Step 2. Put 22mL of concentrated nitric acid, 14mL of concentrated sulfuric acid, 4g of ammonium chloride and 2g of sodium chloride into a beaker, add 714mL of deionized water into the beaker, and stir at 60°C for 0.5h with a magnetic stirrer. Obtain mixed solutions such as mixed acids and strong ionic salts for subsequent use;

[0026] Step 3: Take 750mL of the mixed solution of mixed acid and strong ionic salt prepared in Step 3 and 10g of rough-selected Halloysite obtained in Step 1 respectively, and put them into a beaker. After magnetically stirring at room te...

Embodiment 2

[0034] A preparation of halloysite tube assembled Fe by high temperature pyrolysis 3 o 4 The method for nanocomposite material, its specific preparation steps are:

[0035] Step 1, the method similar to embodiment 1, obtains the halloysite powder of purification and tube expansion;

[0036] Step 2: Weigh 1.5 g of sodium oleate and add it to 300 mL of citric acid solution (2 wt %) and stir until the sodium oleate is completely dissolved. Then add 3g of expanded HNTs powder into the sodium oleate solution and sonicate for 30min to obtain a homogeneous mixture. Stirring was continued at 60°C for 2 hours, and then collected by centrifugation to obtain oleate-modified halloysite nanotubes (BHNTs), which were washed three times with deionized water. The BHNTs were then dried at 60°C for 12 hours and ground through a 200-mesh sieve in an agate mortar;

[0037] Step 3, according to the method of embodiment 1, by Fe(acac) 3 : Oleylamine: The molar ratio of oleic acid and trioctylp...

Embodiment 3

[0041] A preparation of halloysite tube assembled Fe by high temperature pyrolysis 3 o 4 The method for nanocomposite material, its specific preparation steps are:

[0042] Step 1, the method similar to embodiment 1, obtains the halloysite powder of purification and tube expansion;

[0043] Step 2. Disperse 3 g of the tube-expanded HNTs sample obtained in Step 1 in 600 mL of deionized water to obtain a HNTs suspension (5 mg / mL). After sonication for 0.5 h the pH of the suspension was adjusted to 8.5 by tris. Then 1.2mg of dopamine powder was added to the HNTs suspension and stirred at 30°C. The gray DHNTs product was obtained after the final mixture was stirred for 3 h. The gray product was separated by centrifugation and washed repeatedly with distilled water until the filtrate became colorless and transparent;

[0044] Step 3, according to the method of embodiment 1, by Fe(acac) 3 : The molar ratio of oleylamine: oleic acid and polyvinylpyrrolidone is 1:10:4:0.5 to pre...

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Abstract

The invention provides a method for preparing a nanocomposite material by assembling ferriferrous oxide in a halloysite tube, and belongs to the technical field of deep processing of nonmetallic minerals. The method comprises the following four steps: (1) pretreatment, tube expansion and purification of the halloysite minerals; (2) modification in the halloysite tube; (2) preparation of Fe3O4 magnetic nanoparticles through a mixed hydrothermal solution technology; and (4) vacuum impregnation for obtaining the compoiste material with the nano-Fe3O4 assembled in the halloysite tube. The halloysite/Fe3O4 composite material prepared in the invention has no residual magnetization or coercive force, and has a typical paramagnetic performance. The material prepared through the method has good biocompatibility, and broadens the application prospect of mineral magnetic materials in the fields of biomedicines and composite magnetic materials.

Description

[0001] Ouyang Jing, Yang Huaming, Mu Dawei, Guo Binbin, Zhang Yi technical field [0002] The invention relates to a preparation method of a mineral-based composite functional material, in particular to a composite functional material in which nano ferric oxide particles are assembled in a halloysite tube by a two-step method. Background technique [0003] The chemical composition of halloysite is Al[Si 2 o 5 ](OH) 4 2H 2 O, a silicate mineral with hydrous layered structure in the monoclinic system. It is in the shape of a straight tube, and under a transmission electron microscope (TEM), it shows a natural nano-hollow tube shape. The outer diameter of the tube is 50-100nm, the inner diameter is 16-30nm, and the tube length ranges from tens to hundreds of nanometers. It is often used to prepare high-quality white ceramic materials, and some methods including physical and chemical modification, surface and structural modification make halloysite have good application pros...

Claims

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Application Information

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IPC IPC(8): C01G49/08C01B33/26B82Y30/00H01F1/00H01F1/01H01F41/00
CPCB82Y30/00C01B33/26C01G49/08C01P2004/04C01P2004/82C01P2006/42H01F1/0018H01F1/01H01F41/00
Inventor 欧阳静杨华明穆大伟郭斌斌张毅
Owner CENT SOUTH UNIV
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