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Preparation method of mesoporous silica microsphere

A technology of mesoporous silica and silica, applied in chemical instruments and methods, separation methods, alkali metal oxides/hydroxides, etc., can solve the problem of wide size distribution of mesoporous silica microspheres and synthesis parameters Difficult to control, uneven appearance and other problems, to achieve the effect of easy to realize industrial production, good physical and chemical properties, and good industrial development prospects

Inactive Publication Date: 2018-09-28
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

(Lu B W, Endo A, Inagi Y, etal.Synthesis and characterization of mono-dispersed mesoporous spheres[J].Journal of Materials Science,2009,44(24):6463.) However, due to the difficulty in controlling the synthesis parameters, the prepared Mesoporous silica microspheres have problems such as wide size distribution, uneven appearance, narrow pore size distribution, particle agglomeration, and harsh synthesis conditions.

Method used

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  • Preparation method of mesoporous silica microsphere
  • Preparation method of mesoporous silica microsphere
  • Preparation method of mesoporous silica microsphere

Examples

Experimental program
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Effect test

Embodiment 1

[0046] (1) The preparation of polystyrene microspheres with a degree of crosslinking of 2%

[0047] Take 0.1g NaHCO 3 , 0.2g of sodium dodecylsulfonate (SDS) was dissolved in 120mL of distilled water, the solution was transferred to a reaction kettle, nitrogen gas was introduced, mechanically stirred, the temperature was raised to 70°C, and 20mL of monomers (19.6mL of styrene and 0.4 mL of a mixture of divinylbenzene) was added to the reaction system, and 0.32 g of potassium persulfate was weighed and dissolved in 30 mL of distilled water, and added to the reaction system, the stirring speed was controlled at 180 r / min, and the reaction was stopped after 13 hours of reaction, and the obtained emulsion was removed and left to stand. The solvent evaporates naturally at room temperature to obtain polystyrene microspheres with a crosslinking degree of 2%;

[0048] attached figure 2 It is obtained by scanning polystyrene microspheres with a cross-linking degree of 2% with a mode...

Embodiment 2

[0060] (1) preparation of polystyrene microspheres with a degree of crosslinking of 3%

[0061] In a 500mL four-necked bottle, add 0.1g NaHCO successively 3 , 0.3g sodium dodecylsulfonate (SDS) and 120mL water, heated to 70°C in a water bath, introduced argon, mechanically stirred, and then added mixed monomers (19.4mL styrene and 0.6mL diethylene benzene mixture), while dissolving 0.5g of potassium persulfate in 30mL of water and heating to 70°C, and then dropwise adding it to the previous reactor. The emulsion was left standing, and the solvent evaporated naturally at room temperature to obtain polystyrene microspheres with a crosslinking degree of 3%.

[0062] (2) Sulfonation of polystyrene microspheres

[0063] Submerge 1 g of dry cross-linked polystyrene microspheres in 30 mL of concentrated sulfuric acid, and react at a constant temperature of 40 ° C for 13 h. After the reaction, discard the liquid, wash with water until the pH value of the supernatant remains unchange...

Embodiment 3

[0068] (1) preparation of polystyrene microspheres with a degree of crosslinking of 20%

[0069] In a 250mL four-neck flask, add 1g of polyvinylpyrrolidone, 95mL of absolute ethanol and 10mL of water, control the stirring speed at 100r / min, put it in a water bath at 75°C after passing through argon, and add 16mL of benzene to the beaker. Ethylene, 4mL divinylbenzene, and 0.2g azobisisobutyronitrile were mixed evenly and added to a four-neck flask, protected by argon, and reacted at a constant temperature for 15 hours. Polystyrene microspheres with a joint degree of 20%;

[0070] (2) Sulfonation of polystyrene microspheres

[0071] Submerge 0.5 g of dry cross-linked polystyrene microspheres in 10 mL of concentrated sulfuric acid, and react at a constant temperature of 40 ° C for 20 h. After the reaction, discard the liquid, wash with water until the pH of the supernatant remains unchanged, and freeze-dry the obtained product , to obtain cross-linked polystyrene microspheres w...

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Abstract

The invention relates to a preparation method of a mesoporous silica microsphere. The method comprises the following steps that 1, a polystyrene microsphere is prepared; 2, the polystyrene microsphereis subjected to sulfonation; 3, a polystyrene / silicon dioxide composite microsphere is prepared; 4, polystyrene in the polystyrene / silicon dioxide composite microsphere is removed, and finally the mesoporous silica microsphere is obtained. According to the prepared mesoporous silica microsphere, by adjusting the cross-linking degree of a polystyrene template, the particle size of generated nano silicon dioxide can be controlled, therefore, the mesoporous size generated after particles are stacked is controlled, and pore diameter adjustable excellent performance is achieved. No expensive pore-forming agent is needed, and then the mesoporous silica microsphere which is uniform in pore diameter and high in specific surface area can be obtained.

Description

technical field [0001] The technical solution of the present invention relates to the field of organic, inorganic and polymer materials, in particular to a preparation method of mesoporous silica microspheres. Background technique [0002] The International Union of Pure and Applied Chemistry divides porous materials into three categories according to their pore sizes: microporous materials with pore diameters less than 2 nm, macroporous materials with pore diameters greater than 50 nm, and mesoporous materials with pore diameters in between. hole material. In 1992, Kresge et al. of Mobil Corporation reported for the first time that M41S series mesoporous silica was successfully synthesized by nanometer self-assembly technology. The study of silica has aroused a research upsurge of scholars at home and abroad, making the preparation and application of mesoporous silica develop rapidly. [0003] Mesoporous silica microspheres have a larger pore size than microporous materia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30B01D53/02
CPCB01D53/02B01J20/103B01J20/261B01J20/28021B01J20/28083
Inventor 张旭张新潮王小梅
Owner HEBEI UNIV OF TECH
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