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Preparation method for controllable hollow mesoporous silicon dioxide nanospheres

A technology of mesoporous silica and silica, applied in silica, silica, nanotechnology and other directions, can solve the problems of high cost and complicated preparation process, achieve complete morphology, simple synthesis process and cheap raw materials Effect

Active Publication Date: 2012-08-15
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, for the preparation of hollow silica, how to overcome the shortcomings of complex preparation process, strict process conditions and high cost, and precisely control the parameters of hollow spheres such as size, geometric uniformity and shell thickness are still the main problems faced by people.

Method used

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  • Preparation method for controllable hollow mesoporous silicon dioxide nanospheres
  • Preparation method for controllable hollow mesoporous silicon dioxide nanospheres

Examples

Experimental program
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Effect test

Embodiment 1

[0019] 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.

[0020] 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.

[0021] 3. Etching of the hard template: immerse the core-shell structure material obtained above in 10% HCl solution a...

Embodiment 2

[0023] 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., the stirring speed was 80 r / min, and a suspension of 12 nm nanometer iron oxide particles was obtained 48 hours after the reaction.

[0024] 2. Preparation of the core-shell structure: Add 200ml of ethanol, 200ml of deionized water, 0.8g of cetyltrimethylammonium bromide to the above iron oxide nanoparticle suspension, adjust the pH value to 9 with ammonia water, and stir Slowly add 2.5g tetraethyl orthosilicate to react for 24 hours, filter and dry, and bake at 500°C to obtain a core-shell structure with a coating layer of 6.5nm silica.

[0025] 3. Etching of the hard template: immerse the core-shell structure material obtained above in 15% HCl solution and etch for 20 minutes, dissolv...

Embodiment 3

[0027] 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 a suspension of 60nm cubic iron oxide particles was obtained 24 hours after the reaction.

[0028] 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.

[0029] 3. Etching of the hard template: immerse the core-shell structure material obtained above into 15% HNO 3 Etching in the solution for 80 min, d...

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Abstract

The invention provides a preparation method for controllable hollow mesoporous silicon dioxide nanospheres. The method comprises the following steps of: dissolving iron salt, acetic acid and polyvinylpyrrolidone in ethanol, and uniformly stirring and mixing, then transferring the solution into a polytetrafluoroethylene reaction kettle, and reacting while heating to obtain an iron oxide nanoparticle suspension; adding ethanol, deionized water and cetyl trimethyl ammonium bromide into the iron oxide nanoparticle suspension, adding alkali to adjust the pH value to be 7-12, slowly adding tetraethoxysilane in a stirring condition so as to for 12-72 hours, filtering, drying, and roasting at 400-600 DEG C, thus obtaining a mesoporous silicon dioxide-coated iron oxide nanomaterial with a core-shell structure; and completely soaking the obtained mesoporous silicon dioxide-coated iron oxide nanomaterial with the core-shell structure in a prepared acidic etching solution, dissolving an iron oxide used as a hard template, and washing with the deionized water and the ethanol, filtering and drying, thus obtaining the hollow mesoporous silicon dioxide nanospheres. The preparation method for the controllable hollow mesoporous silicon dioxide nanospheres disclosed by the invention has the advantages of being simple in synthesis process, moderate in operation condition, cheap in raw material and easy in acquisition of raw materials, and easy in enlargement and synthesis.

Description

technical field [0001] The invention relates to a preparation method of controllable hollow mesoporous silica nanospheres. Background technique [0002] Hollow silica microspheres have extremely broad application prospects because of their non-toxic and side-effect-free properties, low density, and high thermal and mechanical stability. They can not only be widely used as microcapsule materials in the controllable transport and release system of drugs, dyes, cosmetics, sensitive reagents such as enzymes, proteins, etc., but also can be used as lightweight fillers, highly selective catalysts or catalyst carriers, and in Artificial cells, disease diagnosis, etc. will also have extremely important value. In addition, the design of physical and chemical properties can be effectively realized by adjusting the size of microspheres, cavities and wall thicknesses, which has broad application prospects in industry. [0003] There are many methods to synthesize hollow nanospheres, su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12B82Y40/00
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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