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A kind of preparation method of interlocking microcapsule of hierarchical pore structure of inorganic silicon material

A technology of graded pores and inorganic silicon, which is applied in the fields of inorganic, organic and polymer materials, can solve the problems of complex preparation process, achieve the effect of simple and easy preparation process, good industrial development prospects, and improved mass transfer rate.

Inactive Publication Date: 2016-08-24
HEBEI UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2014, the patents of our research group (CN103933911 A30-30, CN103933912 A30-30) proposed the use of atom transfer radical polymerization to form polymers on the surface of functionalized, regularly arranged silica colloidal crystal templates and perform cross-linking. After the hole, the template is removed, and the interlocking microcapsule of the polymer-based hierarchical pore structure is obtained. The preparation process is complicated. In the process of surface-induced atom transfer radical polymerization, a high temperature of 100 ° C and harsh reaction conditions of anhydrous and oxygen are required to form The process of hierarchical pore structure requires complex cross-linking porogenic technology

Method used

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  • A kind of preparation method of interlocking microcapsule of hierarchical pore structure of inorganic silicon material
  • A kind of preparation method of interlocking microcapsule of hierarchical pore structure of inorganic silicon material
  • A kind of preparation method of interlocking microcapsule of hierarchical pore structure of inorganic silicon material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Preparation of 500nm cross-linked polystyrene colloidal crystal template

[0034] Take 80mL of water into a 250mL three-necked flask, stir stably, pour in argon, heat to 70℃, stir for 30min, add 11mL of monomer (a mixture of 10mL of styrene and 1mL of divinylbenzene) into the reaction system, and then Dissolve 0.04 g of potassium persulfate in 10 mL of water and add it to the reaction system. The stirring speed is controlled at 300r / min. After 30 hours of reaction, the reaction is stopped. The obtained emulsion is removed and allowed to stand. The solvent evaporates naturally at room temperature to obtain an average particle size of 500 nm. Cross-linked polystyrene colloidal crystal template;

[0035] Attached figure 2 It was obtained by scanning the cross-linked polystyrene colloidal crystal template with the model FEI Nano SEM 450 electron scanning electron microscope. It can be seen from the figure that the cross-linked polystyrene colloidal crystal template prepared...

Embodiment 2

[0045] (1) Preparation of 200nm cross-linked polystyrene colloidal crystal template

[0046] Add 0.1g NaHCO to a 500mL four-necked bottle 3 , 0.3g sodium dodecyl sulfonate (SDS) and 120mL water, heated to 70℃ in a water bath, argon gas was introduced, and mechanical stirring, and then mixed monomers (20mL styrene and 2mL divinylbenzene) were added to the reaction system Then, 0.5g potassium persulfate dissolved in 30mL water was added dropwise to the previous reactor. After 1h, the dripping was completed. The stirring speed was 180r / min, and the reaction was kept at 70℃ for 13h. The obtained emulsion was removed and allowed to stand. The solvent was kept at room temperature. It evaporates naturally, and a cross-linked polystyrene colloidal crystal template with a particle size of 200 nm is obtained;

[0047] (2) Surface functionalization of cross-linked polystyrene colloidal crystal template (CLPS)

[0048] The dried 1g cross-linked polystyrene colloidal crystal template was immerse...

Embodiment 3

[0053] (1) Preparation of 900nm cross-linked polystyrene colloidal crystal template

[0054] In a 250mL four-neck flask, add 2g polyvinylpyrrolidone, 95mL absolute ethanol and 10mL water. The stirring speed is controlled at 110r / min. After argon gas is introduced for 15min, it is placed in a 75℃ water bath for later use, and another 20mL is added to the beaker. Styrene, 2mL divinylbenzene, 0.2g azobisisobutyronitrile were mixed uniformly and added to a four-neck flask, protected by argon, and reacted at a constant temperature for 15 hours. The resulting emulsion was removed and allowed to stand, and the solvent was naturally evaporated at room temperature to obtain Cross-linked polystyrene colloidal crystal template with a particle size of 900 nm;

[0055] (2) Surface functionalization of cross-linked polystyrene colloidal crystal template (CLPS)

[0056] The dried 0.5g cross-linked polystyrene colloidal crystal template was immersed in 10mL concentrated sulfuric acid and reacted at...

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Abstract

The invention is a method for preparing interlocking microcapsules with hierarchical pore structure of inorganic silicon materials. The method includes: (1) preparation of cross-linked polystyrene colloidal crystal template; (2) surface of cross-linked polystyrene colloidal crystal template Functionalization; (3) Preparation of CLPS@SiO2 core-shell composite materials; (4) Removal of cross-linked polystyrene in CLPS@SiO2 core-shell composite materials. Compared with polymer-based hierarchical pore structure interlocking microcapsules, the present invention has the advantages of simple preparation process, mild reaction conditions, no need for subsequent cross-linking porogenic technology, and the obtained product has good thermal stability and excellent Biocompatibility makes it have huge potential application value in the fields of high-temperature supported catalysis and bioloaded catalysis.

Description

Technical field [0001] The technical scheme of the present invention relates to the field of inorganic, organic and polymer materials, and specifically relates to a method for preparing interlocking microcapsules with a hierarchical pore structure of inorganic silicon materials. Background technique [0002] Microcapsule refers to a miniature container with a hollow structure and a shell of polymer materials, inorganic materials or organic-inorganic hybrid materials. Microcapsules have the functions of protecting the core material in the capsule core, changing the weight, volume, state and surface properties of the material, isolating the active ingredients, and controlling the slow release of the core material. At the end of the 1970s, Narty et al. (Narty JJ, et al. Nanoparticles a new colloidal drug delivering system. Pharmaceutica Acta Helvetiae, 1978, 53: 17-23.) proposed the concept of nanocapsules (Nanocapsules) and expanded the microcapsules into A new type of material wi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/14B01J21/08B01J32/00B01J35/10
CPCB01J13/14B01J21/08B01J35/653B01J35/651
Inventor 张旭顾金艳王小梅刘盘阁
Owner HEBEI UNIV OF TECH