Preparation method of large-particle-size porous high-specific-surface silicon dioxide microspheres

A technology of high specific surface area and silicon dioxide, applied in the direction of silicon dioxide and silicon oxide, can solve the problems of narrow particle size control range, poor structure controllability, cumbersome process, etc., and achieve good uniformity, low cost, and easy preparation The effect of simple process

Active Publication Date: 2018-03-13
NORTHWESTERN POLYTECHNICAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to avoid the deficiencies of the prior art, the present invention proposes a method for preparing silica microspheres with large particle size, porous and high specific surface area, which solves the existing problems in the preparation process of porous silica such as high cost, cumbersome process, poor structure Problems such as poor controllability and narrow particle size control range (mainly manifested in the difficulty of preparing large particle sizes above the micron level)

Method used

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  • Preparation method of large-particle-size porous high-specific-surface silicon dioxide microspheres
  • Preparation method of large-particle-size porous high-specific-surface silicon dioxide microspheres
  • Preparation method of large-particle-size porous high-specific-surface silicon dioxide microspheres

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Embodiment 1

[0024] Example 1: Large particle size porous high specific surface silica microspheres

[0025] Take porous polystyrene microspheres, put them into a reaction bottle, and add tetraethyl orthosilicate to it until the liquid level does not exceed the porous polystyrene microspheres; vacuumize until no bubbles overflow in tetraethyl orthosilicate, and filter to obtain Porous polystyrene / tetraethyl orthosilicate composite microspheres; the obtained porous polystyrene / tetraethyl orthosilicate composite microspheres were transferred to a three-neck flask, and ammonia water was added thereto, stirring was started, and the porous polystyrene The volume ratio of tetraethyl orthosilicate composite microspheres to ammonia water is 1:5, and the pH of ammonia water is 10; after reacting at room temperature for 60 minutes, filter to obtain porous polystyrene / SiO 2 Composite microspheres; the resulting porous polystyrene / SiO 2 The composite microspheres were vacuum carbonized at 500 °C for ...

Embodiment 2

[0026] Example 2: Large particle size porous high specific surface silica microspheres

[0027] Take porous polymethyl methacrylate microspheres, put them into a reaction bottle, and add methyl orthosilicate to it until the liquid level does not exceed the porous polymethyl methacrylate microspheres; After the bubbles overflowed, filter to obtain porous polymethyl methacrylate / orthosilicate composite microspheres; transfer the obtained porous polymethyl methacrylate / orthosilicate composite microspheres to a three-necked flask, Add sodium hydroxide aqueous solution to it, start stirring, wherein the volume ratio of porous polymethyl methacrylate / orthosilicate composite microspheres and sodium hydroxide aqueous solution is 1:7, and the pH of sodium hydroxide aqueous solution is 12; room temperature reaction After 40min, filter to obtain porous polymethyl methacrylate / SiO 2 Composite microspheres; the resulting porous polymethylmethacrylate / SiO 2 The composite microspheres were...

Embodiment 3

[0028] Example 3: Large particle size porous high specific surface silica microspheres

[0029] Take porous polyacrylonitrile microspheres, put them into a reaction bottle, and add propyl orthosilicate to it until the liquid level does not exceed the porous polyacrylonitrile microspheres; vacuumize until no bubbles overflow in the propyl orthosilicate, and filter to obtain Porous polyacrylonitrile / orthopropyl silicate composite microspheres; transfer the obtained porous polyacrylonitrile / orthopropyl silicate composite microspheres into a three-neck flask, and add potassium hydroxide aqueous solution to it, start stirring, and the porous polyacrylonitrile The volume ratio of polyacrylonitrile / propyl orthosilicate composite microspheres to potassium hydroxide aqueous solution is 1:6, and the pH of potassium hydroxide aqueous solution is 14; after reacting at room temperature for 30 minutes, filter to obtain porous polyacrylonitrile / SiO 2 Composite microspheres; the resulting por...

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Abstract

The invention relates to a preparation method of a large-particle-size porous high-specific-surface silicon dioxide microspheres. The preparation method comprises the following steps of: taking industrialized macroporous large-particle-size resin as a template and organic silicon as a silicon source, 'filling' the silicon source into a porous resin channel under a vacuum condition, hydrolyzing thesilicon source under an alkaline condition, then carrying out calcination, and preparing large-particle-size high-specific-surface silicon dioxide microspheres by a method of replacing holes and walls. In the first step, silicon oxide is filled into pore channels of the template resin for one-step carbonization, and the framework of the template resin is carbonized to further bring pore channelssecond filling, thereby ensuring the framework strength of the product namely silicon dioxide microspheres and enrich the pore channels. The silicon dioxide microspheres prepared by the method have the advantages of high specific surface area, easy control of pore channels and particle sizes, good uniformity, simple preparation process, low cost, suitability for large-scale preparation and potential application value in the field of adsorption separation.

Description

technical field [0001] The invention belongs to the field of inorganic porous materials and relates to a method for preparing silicon dioxide microspheres with large particle diameter, porous and high specific surface area. Background technique [0002] Due to its high specific surface area, good stability and strong adsorption capacity, porous silica has a wide range of applications in the fields of catalysis, environment and biomedicine. Therefore, it is of great significance to develop a method for preparing porous silica with low cost, simple process and easy industrialization. [0003] At present, the preparation methods of porous silica mainly include surfactant template method, sol-gel method and spray drying method. The surfactant template method uses surfactant as a template, and utilizes the difference in the morphology of surfactant micelles at different concentrations to hydrolyze organosiloxane under alkaline conditions to obtain silica materials with different...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12
CPCC01B33/12
Inventor 张宝亮王继启呼延钰张秋禹张和鹏
Owner NORTHWESTERN POLYTECHNICAL UNIV
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