Thorn-like silica ball and preparation method thereof

A technology of silica spheres and silica, which is applied in the direction of silica, silica, nanotechnology, etc., can solve the problems that cannot fully meet the application of silica spheres, and the shape is not much, and achieve high pore volume and preparation methods The effect of simplicity and high specific surface area

Active Publication Date: 2017-08-29
WENZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is known that the silica spheres made by the soft template method have few shapes, which cannot fully meet the different applications of silica spheres.

Method used

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  • Thorn-like silica ball and preparation method thereof
  • Thorn-like silica ball and preparation method thereof
  • Thorn-like silica ball and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Weigh 4 g of cetylpyridine bromide and 2 g of urea, mix and dissolve in 100 mL of water to obtain solution A, and take 10 g of tetramethyl orthosilicate, dissolve in 100 mL of cyclohexane and n-pentanol 5 Solution B was obtained from a mixed solution of mL, and while stirring at 500rpm, add solution A dropwise to solution B at a rate of 2-20 mL / min, continue stirring at this stirring speed for 1 h at room temperature, and transfer to the reaction After the still, heat it in a conventional oven at 120°C for 6 h, after cooling, filter, wash, dry, transfer to a muffle furnace and bake at 500°C to obtain highly uniform thorn-like silica balls with a size of 700nm about. SEM image see figure 1 and X - ray diffraction pattern see Figure 15 .

Embodiment 2

[0043]Weigh 4 g of cetylpyridine bromide and 2 g of urea, mix and dissolve in 100 mL of water to obtain solution A, and take 10 g of tetramethyl orthosilicate, dissolve in 100 mL of cyclohexane and n-pentanol 5 The solution B was obtained from the mixed solution of mL. While stirring at 1500rpm, the solution A was added dropwise to the solution B at a rate of 2-20 mL / min. Stirring was continued at room temperature for 1 h at the stirring rate, and transferred to the reaction After the kettle, heat it in a conventional oven at 120°C for 6 hours. After cooling, filter, wash, dry, transfer to a muffle furnace and bake at 500°C to obtain highly uniform thorn-like silica balls with a size of 500nm. about. SEM image see figure 2 .

Embodiment 3

[0045] Weigh 4 g of cetylpyridine bromide and 2 g of urea, mix and dissolve in 100 mL of water to obtain solution A, and take 10 g of tetramethyl orthosilicate, dissolve in 100 mL of cyclohexane and n-pentanol 5 mL of the mixed solution to obtain solution B, while stirring at 2000rpm, add solution A dropwise to solution B at a rate of 2-20 mL / min, continue stirring for 1 h at room temperature at this stirring speed, and transfer to the reaction After the kettle, heat it in a conventional oven at 120°C for 6 h, after cooling, filter, wash, dry, transfer to a muffle furnace and bake at 500°C to obtain highly uniform thorn-like silica balls with a size of 350nm about. SEM image see image 3 .

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Abstract

The invention relates to a thorn-like silica ball and a preparation method thereof. The silica ball has a plurality of thorn-like structures formed by a silica line, and interconnected mesoporous channels are formed between thorns. The preparation method comprises the following steps: 1) emulsification: stirring and dissolving urea, hexadecylpyridinium bromide hydrate and deionized water to form an A solution, mixing n-amyl alcohol, cyclohexane and organic silicate ester to form a B solution, adding dropwise the prepared A solution to the B solution and stirring continuously for 0.5 to 5 hours to obtain a white emulsion; 2) balling: heating the obtained white emulsion in 1) in an oven at 60 to 180 DEG C, standing for 3 to 10 hours to obtain a white precipitate; 3) purification: cooling the white precipitate obtained in 2), performing suction filtration, washing with water and ethanol at least once, and after drying, transferring the white precipitate to a muffle furnace for calcination at 400 to 600 DEG C to obtain a white powdery solid. The prepared silica ball with a thorn-like structure has excellent properties, satisfies more needs, and has a simple preparation method.

Description

technical field [0001] The invention relates to a thorny silica ball and a preparation method thereof. Background technique [0002] Due to its good biocompatibility, chemical stability, high specific area and large pore volume, silica spheres are widely used as templates for drug sustained release, catalysis, adsorption, separation and preparation of other novel structural nanomaterials. [0003] Silica spheres with different particle sizes and shapes have different properties and can meet different applications. Hard template method and soft template method are common methods for preparing silica with special morphology. [0004] Patent CN1511785 discloses a silica mesoporous material, which is composed of hollow silica particles, the walls of which have substantially radially arranged pores, and discloses a method for preparing the above silica mesoporous material: Different forms of calcium carbonate are used as hard templates to grow and synthesize mesoporous material...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18B82Y40/00
CPCC01B33/18C01P2002/72C01P2004/03C01P2004/32C01P2004/62C01P2006/12
Inventor 陈锡安郭大营魏会方黄少铭
Owner WENZHOU UNIVERSITY
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