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Preparation method of silica-coated iron oxide nano-core-shell structural material

A technology of nano-core-shell and structural materials, applied in the direction of nano-structure manufacturing, iron oxide/hydroxide, silicon dioxide, etc., can solve the problems of complex operation process, serious core agglomeration, and difficulty in scale-up production, and achieve the synthesis process Simple, obvious core-shell structure, easy to enlarge the effect of synthesis

Active Publication Date: 2012-07-25
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the small size of nanoparticles and large specific surface area, the disadvantages of easy aggregation and instability after separation from the preparation system limit the application of nanoparticles. Silica has good biocompatibility and anti-decomposition ability. Nanomaterials with a core-shell structure coated with a layer of silicon dioxide on the surface of iron oxide are not only conducive to the dispersion and stability of iron oxide nanomaterials, but also improve their biocompatibility. The further functionalization of core-shell composite particles has made them widely used in drug controlled release, biological targeting materials, environmental sewage treatment and iron-based catalyst stabilization, and has attracted widespread attention and has become one of the research hotspots in the preparation of new materials. one
[0003] The surface coating methods of nanoparticles mainly include sol-gel method, microemulsion method, aerosol thermal decomposition method, etc. Among these methods, the sol-gel method has the characteristics of large reaction interval, short time and high yield, and is quite popular At present, a considerable part of the related reports on the surface of iron oxide nanoparticles coated with silicon dioxide have obtained composite particle structures that are not ideal. The synthesized core-shell structure has irregular morphology, poor controllability, and core agglomeration. More serious; the operation process is complicated, for example, the patent CN1477082A "method for preparing ferrite-silica core-shell nanoparticles by ultrasonic treatment" requires steps such as ultrasonic treatment of iron oxide nanoparticles, and the serious agglomeration of the core leads to irregular morphology; the process High cost, difficult to scale up production, etc., which all affect the advancement of the later practical process

Method used

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  • Preparation method of silica-coated iron oxide nano-core-shell structural material
  • Preparation method of silica-coated iron oxide nano-core-shell structural material

Examples

Experimental program
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Effect test

Embodiment 1

[0017] 1. Preparation of iron oxide nanoparticles: Dissolve 1.01g of ferric nitrate, 0.5ml of acetic acid and 5g of polyvinylpyrrolidone in 250ml of ethanol solvent, stir and mix evenly, then transfer the solution into a polytetrafluoroethylene reactor and heat to 200°C for reaction , the stirring speed was 100r / min, and a 6nm iron oxide nanoparticle suspension was obtained after reacting for 3 hours.

[0018] 2. Preparation of core-shell structure: Add 520ml of ethanol, 200ml of deionized water, 0.8g of cetyltrimethylammonium bromide to the suspension of iron oxide nanoparticles, and adjust the pH value to 8 with triethanolamine. Under the condition of stirring, 2.5 g of tetraethyl orthosilicate was slowly added to react for 12 hours, filtered and dried, and calcined at 450° C. to obtain a core-shell structure with a coating layer of 5 nm mesoporous silica.

Embodiment 2

[0020] 1. Preparation of iron oxide nanoparticles: Dissolve 0.5g ferrous chloride, 0.5ml acetic acid and 2.02g polyvinylpyrrolidone in 200ml ethanol solvent, stir and mix evenly, then transfer the liquid into a polytetrafluoroethylene reactor and heat to The reaction was carried out at 180° C., and the stirring speed was 80 r / min. After 48 hours of reaction, a suspension of 12 nm nanometer iron oxide particles was obtained.

[0021] 2. Preparation of core-shell structure: Add 200ml of ethanol and 200ml of deionized water to the above-mentioned iron oxide nanoparticle suspension, adjust the pH value to 9 with ammonia water, and slowly add 2.5g of tetraethyl orthosilicate to react under stirring conditions After 24 hours, filter and dry, and bake at 500°C to obtain a core-shell structure with a coating layer of 6.5nm silicon dioxide.

Embodiment 3

[0023] 1. Preparation of iron oxide nanoparticles: Dissolve 1.01g ferric nitrate, 2ml acetic acid and 0.5g polyvinylpyrrolidone in 100ml ethanol solvent, stir and mix evenly, then transfer the solution into a polytetrafluoroethylene reactor and heat to 160°C for reaction , the stirring speed was 40r / min, and after 24 hours of reaction, a suspension of 60nm cubic iron oxide particles was obtained.

[0024] 2. Preparation of the core-shell structure: Add 320ml of ethanol, 400ml of deionized water, 0.2g of cetyltrimethylammonium bromide to the above iron oxide nanoparticle suspension, adjust the pH value to 10 with ammonia water, and stir Slowly add 0.625g of tetraethyl orthosilicate under the conditions of 72 hours, filter and dry, and bake at 550°C to obtain a core-shell structure with a coating layer of 20nm mesoporous silica.

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Abstract

A preparation method of silica-coated iron oxide nano-core-shell structural material includes: dissolving molysite, acetic acid and polyvinylpyrrolidone in ethanol, and mixing well; moving the solution into a polytetrafluoroethylene reactor, allowing the solution to react at the heating temperature of 160-220 DEG C for 3-48 hours and under the mixing speed of 10-100rpm, and obtaining 0.1-8g / L iron oxide nanoparticle suspension; and adding the ethanol and deionized water into the suspension, allowing the volume ratio of the ethanol to water in the suspension system to be 0.5-10 / 1, adjusting pH value to be 7-12, allowing the mass ratio of tetraethoxysilane to iron oxide nanoparticles to be 1:1-40, slowly adding the tetraethoxysilane under mixing, allowing the mixture to react for 12-70 hours, performing filtering and drying, and calcining at 400-600 DEG C to obtain the silica-coated iron oxide nano-core-shell structural material, wherein the molar concentration of the molysite in solution is 0.01-0.1mol / L, the volume ratio of the acetic acid to the ethanol is 0.002-1:1, and the mass concentration of the polyvinylpyrrolidone in the solution is 1.5-20g / L. The preparation method has the advantages that synthetic process is simple, cost is low, operation is simple, and amplification and synthesis are easy.

Description

technical field [0001] The invention relates to a preparation method of a silicon dioxide-coated iron oxide nano core-shell structure material. Background technique [0002] As a cheap and environmentally friendly transition metal oxide, nano-iron oxides have good weather resistance, light resistance, magnetism, and good absorption and shielding effects on ultraviolet rays. They can be widely used in pigments, electronics, high Magnetic recording materials, sensors and catalysts also have good application prospects in the fields of bioengineering and drug release. However, due to the small size of nanoparticles and large specific surface area, the disadvantages of easy aggregation and instability after separation from the preparation system limit the application of nanoparticles. Silica has good biocompatibility and anti-decomposition ability. Nanomaterials with a core-shell structure coated with a layer of silicon dioxide on the surface of iron oxide are not only conducive...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B82B3/00B82Y40/00C01G49/02C01B33/12
Inventor 孙予罕张明伟房克功林明桂魏伟
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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