Hollow silicon dioxide microsphere with pores in graded distribution as well as preparation method and application thereof

A silica, gradient distribution technology, applied in the field of porous materials, to achieve the effect of optimizing performance, increasing adsorption speed, and increasing adsorption capacity

Inactive Publication Date: 2012-03-21
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In particular, hollow microspheres change from the outside to the inside, and the pores in the shell layer are gradient (such as from small to large or from large to small) microspheres that have not been reported.

Method used

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  • Hollow silicon dioxide microsphere with pores in graded distribution as well as preparation method and application thereof
  • Hollow silicon dioxide microsphere with pores in graded distribution as well as preparation method and application thereof
  • Hollow silicon dioxide microsphere with pores in graded distribution as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Prepare hollow silica microspheres coated with two layers of silica shells. The molar ratio of raw materials required for each layer of silica shells is: ethanol: water: pore former: TEOS: NH 3 ·H 2 O=58:144:0.3:1:10. The preparation method is as follows:

[0023] 1. Disperse PS microspheres in EtOH and H 2 In the mixed solution of O, after stirring for 30 minutes, add CTAB, after stirring for another 30 minutes, add TEOS and NH 3 ·H 2 O, continue to stir and react for 1 hour, then the reaction ends, filter with suction, wash with water, and obtain PS / CTAB-SiO 2 Composite microspheres, that is, composite microspheres coated with a layer of silica shell;

[0024] 2. The above PS / CTAB-SiO 2 The composite microspheres were dispersed in EtOH and H according to the same ratio 2 In the mixed solution of O, after stirring for 30 minutes, add TTAB, after stirring for another 30 minutes, add TEOS and NH 3 ·H 2 O, continue to stir and react for 1 hour, then the reaction ...

Embodiment 2

[0028] Prepare hollow silica microspheres coated with three layers of silica shells. The molar ratio of raw materials required for each layer of silica shells is: ethanol: water: pore former: TEOS: NH 3 ·H 2 O=58:144:0.3:1:10. The preparation method is as follows:

[0029] 1. Disperse PS microspheres in EtOH and H 2 In the mixed solution of O, after stirring for 30 minutes, add CTAB, after stirring for another 30 minutes, add TEOS and NH 3 ·H 2 O, continue to stir and react for 1 hour, then the reaction ends, filter with suction, wash with water, and obtain PS / CTAB-SiO 2 Composite microspheres, that is, composite microspheres coated with a layer of silica shell;

[0030] 2. Follow the same method and ratio as step 1 in PS / CTAB-SiO 2 A layer of silica shell is coated on the composite microspheres. The difference is that the pore-forming agent used is TTAB, and finally PS / CTAB-SiO 2 / TTAB-SiO 2 Composite microspheres;

[0031] 3. Mix PS / CTAB-SiO with the same ratio as s...

Embodiment 3

[0035] Preparation of coated two-layer SiO 2 shell hollow SiO 2 The microspheres, method and proportioning are the same as in Example 1, except that the second layer uses DTAB as a pore-forming agent.

[0036] The resulting hollow SiO 2 The thickness of the microsphere shell is 91nm, and the specific surface area of ​​the sample is 654m 2 / g, the pore volume is 0.3888ml / g, the outer pore diameter is 1.72nm, and the inner pore diameter is 2.19nm.

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Abstract

The invention discloses a hollow SiO2 (silicon dioxide) microsphere with pores in graded distribution as well as a preparation method and an application thereof. The preparation method comprises the steps that: polrvinyl benzene microspheres, ethyl orthosilicate, ammonia water, ethanol, water and alkyl ammonium bromide are used as raw materials, a sol-gel method is adopted for preparing the hollow SiO2 microsphere, during the preparation, the polrvinyl benzene microspheres are used as a hollow template, the alkyl ammonium bromide is used as pore formers, two to three layers of SiO2 cases are covered on the polrvinyl benzene microspheres to form composite microspheres, the carbon numbers of the pore formers used during the covering of each layer of SiO2 cases are different, and the hollow SiO2 microsphere with pores in graded distribution is finally obtained through calcination. The use performance of the hollow SiO2 microsphere is optimized, the hollow SiO2 microsphere with different case layer thicknesses, specific surface area, pore volume and apertures, and the pores of the hollow SiO2 microsphere are distributed in a gradually increased way from outside to inside in the radialdirection of a case layer. The microsphere obtained by the method has the advantages that the adsorption speed is accelerated, the adsorption quantity is increased, and good application is realized in the aspects of aquatic dye molecule adsorption and food preservative load.

Description

technical field [0001] The invention relates to a hollow silica microsphere and its preparation method and application, in particular to a hollow silica microsphere with gradient distribution of pores on a spherical shell, its preparation method and application, and belongs to the technical field of porous materials. Background technique [0002] Hollow silica (SiO 2 ) Microspheres can be used in catalyst and preservative carrier, adsorption and separation, microreactor, chromatographic separation and other fields. Combining sol-gel and double-template (polystyrene as a hollow template, surfactant as a pore-forming template) method is a common method for preparing hollow microspheres with nanopores on the shell. That is, polystyrene (PS) microspheres are used as templates, and SiO is coated on them. 2 Spherical shell, and then calcined to remove the PS template to obtain hollow SiO 2 Microspheres. In SiO 2 The formation of nanopores in silica spherical shells can greatl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30C02F1/28A23L3/3454
Inventor 刘世权邱芹王海霞
Owner UNIV OF JINAN
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