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Method for preparing small-size meso-porous hollow carbon sphere

A hollow carbon sphere, small-sized technology, applied in chemical instruments and methods, medical preparations of non-active ingredients, pharmaceutical formulations, etc., can solve the problem of inability to control the size of mesoporous hollow carbon spheres, complex synthesis process steps, time-consuming and High cost and other issues, to achieve the effect of controllable size, large pore volume, and easy operation

Active Publication Date: 2010-01-06
中国科学院上海硅酸盐研究所苏州研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, mesoporous carbon materials are mainly prepared by hard template and soft template methods in the prior art, but the existing preparation methods mainly have the following disadvantages: 1. The synthesis process steps are complicated, time-consuming and costly; 2. Using existing The mesoporous hollow carbon spheres synthesized by existing technologies are all larger than 200nm, which greatly limits the application of mesoporous hollow carbon spheres as drug carriers in the field of medicine; 3. The size of the synthesized mesoporous hollow carbon spheres cannot be easily and effectively regulated

Method used

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  • Method for preparing small-size meso-porous hollow carbon sphere
  • Method for preparing small-size meso-porous hollow carbon sphere
  • Method for preparing small-size meso-porous hollow carbon sphere

Examples

Experimental program
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Effect test

Embodiment 1

[0050]First prepare aluminum-doped mesoporous silica core-shell spheres with a size of 260-280nm: 6.28mL ammonia water (14% by mass), 74mL absolute ethanol and 10mL deionized water, add 6mL orthosilicic acid at 30°C Stir for 1 h after ethyl ester; then add 5 mL of tetraethyl orthosilicate and 2 mL of octadecyltrimethoxysilane, and 1 mL of aluminum sulfate aqueous solution with a concentration of 0.45 mol / L to continue the reaction for 1 h; centrifuge the resultant, wash and After drying, calcining at 550° C. for 6 h to remove the template, thereby preparing aluminum-doped mesoporous silica core-shell spheres. Take 0.5g of the above powder and put it into a small beaker, drop 0.6mL of furfuryl alcohol into the powder at a rate of 0.3mL / min to make the furfuryl alcohol fully wet the powder; then put the small beaker into a vacuum oven at 60°C for heating After 3h, start vacuuming and maintain the vacuum state for 10h; put the obtained powder into the atmosphere furnace, raise it...

Embodiment 2

[0052] First prepare aluminum-doped mesoporous silica core-shell spheres with a size of 160-180nm: 3.14mL ammonia water (30% by mass), 74mL absolute ethanol and 10mL deionized water, add 6mL orthosilicic acid at 30°C Stir for 1 h after ethyl ester; then add 5 mL of tetraethyl orthosilicate and 2 mL of octadecyltrimethoxysilane, and 1 mL of aluminum sulfate aqueous solution with a concentration of 0.45 mol / L to continue the reaction for 1 h; centrifuge the resultant, wash and After drying, calcining at 550° C. for 6 h to remove the template, thereby preparing aluminum-doped mesoporous silica core-shell spheres. Intuitive description see figure 1 . Take 0.5g of the above powder and put it into a small beaker, drop 0.6mL of furfuryl alcohol into the powder at a rate of 0.3mL / min to make the furfuryl alcohol fully wet the powder; then put the small beaker into a vacuum oven at 60°C for heating After 3h, start vacuuming and maintain the vacuum state for 10h; put the obtained powd...

Embodiment 3

[0054] According to the process described (same as Example 1), first prepare aluminum-doped mesoporous silica core-shell spheres with a size of 80-100 nm: 3.14 mL of ammonia water (22% by mass), 148 mL of absolute ethanol and 20 mL of dehydrated Add 6 mL of tetraethyl orthosilicate to ionic water at 30°C and stir for 1 hour; then add 5 mL of tetraethyl orthosilicate and 2 mL of octadecyltrimethoxysilane, and 1 mL of aqueous aluminum sulfate solution with a concentration of 0.45 mol / L The reaction was continued for 1 hour; the resultant was centrifuged, washed and dried, and calcined at 550° C. for 6 hours to remove the template, thereby preparing aluminum-doped mesoporous silica core-shell spheres. Intuitive shape attached image 3 . Take 0.5g of the above powder and put it into a small beaker, drop 0.6mL of furfuryl alcohol into the powder at a rate of 0.3mL / min to make the furfuryl alcohol fully wet the powder; then put the small beaker into a vacuum oven at 60°C for heatin...

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Abstract

The invention belongs to the field of the compounding of inorganic nano materials, in particular to a method for preparing a small-size meso-porous hollow carbon sphere. The method comprises the following steps: preparing an aluminum-doped meso-porous silicon dioxide nuclear shell structure sphere, polymerizing the sphere by furfuryl alcohol, carbonizing the sphere and removing a silicon dioxide template. The method for preparing the small-size meso-porous hollow carbon sphere has simple condition and is easy to operate, and the meso-porous hollow carbon sphere prepared by the method has the characteristics of controllable size, even pore diameter, large specific surface area and pore volume, and the like and can be applied to the field of adsorbing agent or drug carrier.

Description

technical field [0001] The invention belongs to the field of synthesis of inorganic nanometer materials, and in particular relates to a preparation method of small-sized mesoporous hollow carbon spheres. Background technique [0002] Mesoporous materials are widely used in related fields such as adsorbents, catalyst supports and drug carriers due to their many excellent properties. In the past two decades, various studies on the synthesis and control of mesoporous structures and morphologies have been reported. Mainly through continuous improvement of existing synthesis methods or adoption of some new synthesis techniques. As a kind of mesoporous materials, ordered mesoporous carbon materials are widely used in catalysis, electrode materials, sensors, Adsorbents and hydrogen storage materials have broad application prospects. There have been many reports of mesoporous carbon materials as adsorbents and catalyst supports (eg: 2009, 21, 706-716, Chemistry of Materials), and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82B3/00A61K47/04B01J20/20
Inventor 郭利民何前军崔香枝施剑林
Owner 中国科学院上海硅酸盐研究所苏州研究院
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