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A kind of silicon dioxide egg yolk-eggshell structure material containing large spacing flower-shaped core and its preparation method

A technology of silicon dioxide and structural materials, applied in the direction of silicon dioxide, silicon oxide, chemical instruments and methods, etc., can solve the problem that the smooth surface is not conducive to loading or controlled release of guest molecules, is not conducive to increasing the specific surface area of ​​materials, etc. The process is not easy to control and other problems, to achieve the effect of easy implementation of process operation, novel structure and low cost

Active Publication Date: 2019-06-14
QILU UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The experimental process of this method is relatively complicated, and the etching process is not easy to control. It is difficult to control the size of the egg yolk and eggshell of the material, and the structure of the egg yolk is a regular spherical shape, which is not conducive to increasing the specific surface area of ​​the material. At the same time, the smooth surface is not conducive to loading. or controlled release of guest molecules

Method used

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  • A kind of silicon dioxide egg yolk-eggshell structure material containing large spacing flower-shaped core and its preparation method
  • A kind of silicon dioxide egg yolk-eggshell structure material containing large spacing flower-shaped core and its preparation method
  • A kind of silicon dioxide egg yolk-eggshell structure material containing large spacing flower-shaped core and its preparation method

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preparation example Construction

[0042] As introduced in the background technology, the preparation method of the silicon dioxide material with egg yolk-eggshell structure in the prior art has certain deficiencies. In order to overcome the deficiencies of the prior art, the present invention provides a flower-shaped The preparation method of inner silicon dioxide egg yolk-eggshell structure comprises the following steps:

[0043] (1) Cetyltrimethylammonium bromide (CTAB) and polyvinylpyrrolidone (PVP) are fully dissolved in water and ethanol mixed solution, and it is formed into a transparent and uniform solution by stirring;

[0044] Wherein, the stirring temperature is 25-40° C., and the stirring speed is 400-600 r / min.

[0045] The molar ratio of CTAB and PVP is 1:(0.028-0.065).

[0046] The addition ratio of the CTAB, water and ethanol is 1 g: (300-320) mL: (180-200) mL.

[0047] (2) Ultrasonic dispersion of tetraethyl orthosilicate (TEOS) in cyclohexane;

[0048] Wherein, the addition amount ratio of ...

Embodiment 1

[0058] Add 0.08g CTAB and 0.4g PVP into a 100mL beaker and place it on a magnetic stirrer, add 25mL deionized water and 15mL ethanol to raise the temperature to 35°C, adjust the rotation speed to 500r / min to completely dissolve and form a uniform solution; gTEOS was ultrasonically dispersed in 3mL cyclohexane solution and the mixture was quickly added to the above solution under stirring, and 0.6mL ammonia water with a mass concentration of 23%-25% was added to the solution, followed by stirring reaction for 4h. The obtained white suspension was transferred to a 100mL reaction kettle, and placed in a thermostat at 160°C for 24h. After cooling, the white precipitate was filtered, and the obtained precipitate was repeatedly filtered and washed with distilled water. The obtained precipitate was dried at 55° C. for 10 h, and then the precipitate was calcined in a tubular calciner at 550° C. for 4 h to obtain a silica yolk-eggshell structure containing a flower-like core with large...

Embodiment 2

[0061] Add 0.08g CTAB and 0.4g PVP into a 100mL beaker and place it on a magnetic stirrer, add 25mL deionized water and 15mL ethanol to raise the temperature to 35°C, adjust the rotation speed to 500r / min to completely dissolve and form a uniform solution; The gTEOS was ultrasonically dispersed in 5 mL of cyclohexane solution and the mixture was quickly added to the above solution under stirring, and 0.6 mL of ammonia water with a mass concentration of 23%-25% was added to the solution, followed by a stirring reaction for 4 h. The obtained white suspension was transferred to a 100mL reaction kettle, and placed in a thermostat at 160°C for 24h. After cooling, the white precipitate was filtered, and the obtained precipitate was repeatedly filtered and washed with distilled water. The obtained precipitate was dried at 55°C for 10 hours, and then calcined in a tubular calciner at 550°C for 4 hours to obtain a silica egg yolk-eggshell structure with a flower-like core at large inte...

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Abstract

The invention discloses a silica yolk-eggshell structure material containing a large-spacing flower-like core and a preparation method of the silica yolk-eggshell structure material. The preparation method comprises the following steps: (1) fully dissolving CTAB (Cetyltrimethyl Ammonium Bromide) and PVP (Polyvinyl Pyrrolidone) in a mixed solution of water and ethanol to form a transparent and uniform solution; (2) dispersing TEOS (Tetraethyl Orthosilicate) in cyclohexane; (3) adding the mixture in the step (2) into a solution in the step (1), adding ammonium hydroxide, stirring to obtain white suspension, and adding the white suspension to perform solvent thermal treatment; and (4) filtering, washing, drying, grinding, and calcining the white precipitate subjected to solvent thermal treatment in the step (3), thereby obtaining the product. The silica material prepared in the method disclosed by the invention is uniform in dispersion, and has the particle size of 500-650nm, the shell layer thickness of 25nm and the yolk-eggshell spacing of 100-200nm, and the yolk is of a flower-like structure, has the size of 300-450nm and has rich pore passage structures. Meanwhile, the material is large in void volume, so that the material can be widely applied to the fields of enzyme catalysis, substance adsorption and the like.

Description

technical field [0001] The invention relates to a silicon dioxide egg yolk-eggshell structure material with a flower-like inner core at large intervals and a preparation method thereof, belonging to the technical field of nanomaterial synthesis. Background technique [0002] In recent years, mesoporous silica has attracted widespread attention in the field of nanomaterials science because of its high chemical stability and biocompatibility, adjustable pore size, controllable shape, convenient synthesis, and low cost. The advantages make it show the unparalleled superiority and application potential of other porous materials in many fields such as macromolecular adsorption and separation, enzyme catalysis, chemical sensors, drug controlled release and environmental protection. Among them, egg yolk-eggshell silica not only has the advantages of mesoporous silica, but also provides large pore volume and uniform pore size distribution, and the inner hollow part creates an enviro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/12
CPCC01B33/126C01P2004/04C01P2004/32C01P2004/51C01P2004/62C01P2004/64C01P2006/12
Inventor 周国伟郑玉洁王丹丹张敬
Owner QILU UNIV OF TECH
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