Preparation method for polymer-based hierarchical porous structure interlocking microcapsule

A polymer, graded pore technology, applied in the preparation of microspheres, microcapsule preparations, etc., can solve the problems of cumbersome preparation, high price, unstable pore structure, etc.

Active Publication Date: 2014-07-23
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its limitations are: (1) In the double-template method, the template should have obvious interfacial interaction or form a strong interaction force (such as hydrogen bond) with the skeleton material, complete self-assembly in the skeleton material, and remove the template Pores can be formed. At present, polymer compounds with special structures are mostly used in the double-template method. This type of polymer has high requirements for the composition of segmental structural units and molecular weight, and the preparation is cumbersome and expensive. At the same time, the choice of skeleton material is only melamine. Forming polymers with strong hydrogen bond

Method used

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  • Preparation method for polymer-based hierarchical porous structure interlocking microcapsule
  • Preparation method for polymer-based hierarchical porous structure interlocking microcapsule
  • Preparation method for polymer-based hierarchical porous structure interlocking microcapsule

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0062] Example one:

[0063] (1) Preparation of 600nm silica colloidal crystal template

[0064] At room temperature, add 145g of absolute ethanol, 34.1g of 25% ammonia water, and 35.0g of deionized water to a 500mL three-necked flask equipped with mechanical stirring. After stirring evenly, quickly add 15.4g of ortho silicon to the three-necked flask. Ethyl acid, react at room temperature for 8h. Transfer the obtained suspension to a beaker, and wait until the solvent is naturally volatilized to obtain a silica colloidal template with an average particle size of 600 nm. Finally, the template is sintered in a muffle furnace at 500°C for 3 hours and slowly reduced to room temperature. A silica colloidal crystal template in which silica microspheres with an average particle size of 600 nm are bonded to each other;

[0065] (2) Surface modification of silica colloidal crystal template

[0066] Silane coupling agent [3-(2-bromoisobutyryl)aminopropyl]-triethoxysilane (BITS) modified sili...

Example Embodiment

[0076] Example 1 The surface area of ​​the material obtained with the model Micromeritics ASAP2020M+C automatic surface area analyzer can reach 600m. 2 ·G -1 .

[0077] Note: The preparation method of the silane coupling agent [3-(2-bromoisobutyryl)aminopropyl]-triethoxysilane in step (2) of the present invention is as follows: (the same as other embodiments)

[0078] Add 40.0mL toluene, 16.0mL (3-aminopropyl) triethoxysilane (APTS), 9.40mL triethylamine (TEA) into a three-necked flask, place in an ice bath and stir, add 8.40mL 2-bromoisobutyl The acyl bromide was dissolved in 40 mL of toluene, and the mixture was added dropwise to a three-necked flask. After 1 h of dripping, the mixture was stirred for 3 h in an ice bath, and then stirred at room temperature for 10 h to obtain a solid-liquid mixture. The mixture was filtered and the filtrate was removed by distillation under reduced pressure. Unreacted TEA and solvent toluene can be used to obtain the surface modifier BITS. The sy...

Example Embodiment

[0079] Embodiment two:

[0080] (1) The preparation of 600nm silica colloidal crystal template is the same as the step (1) of Example 1;

[0081] (2) Surface modification of silica colloidal crystal template

[0082] γ-methacryloxypropyltrimethoxysilane (MPS) modified silica colloidal crystal template, 0.3g dried and sintered silica colloidal crystal template, put into a 250mL three-necked flask, add 100ml ethanol , 2.5mL of distilled water, 0.25mL of ammonia, mechanical stirring at 25°C, adding 1.5mL of γ-methacryloxypropyltrimethoxysilane (MPS), condensing and refluxing at room temperature for 24h. After the reaction, the stirring was stopped, the liquid was discarded, washed and replaced with absolute ethanol three times, and finally vacuum dried at 25°C for 12 hours to obtain the MPS modified silica colloidal crystal template with an average particle size of 600 nm;

[0083] (3) Controllable grafted polymer segments of silica colloidal crystal template

[0084] Add 0.03 g of MPS m...

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Abstract

The invention discloses a preparation method for a polymer-based hierarchical porous structure interlocking microcapsule. The method comprises the steps of modifying a silicon dioxide colloid crystal template, controllably grafting a polymer by a surface triggering atom transferring free radical polymerization method and a double-bond free radical polymerization method, crosslinking a linear polymer chain section by an Friedel-Crafts crosslinking method for an external crosslinking agent, removing the silicon dioxide colloid crystal template to prepare the polymer-based hierarchical porous structure interlocking microcapsule. Due to the controllably grafted polymer layer, a certain slit is reserved between every two adjacent microcapsules, so that the mass is reduced, and more mass transfer ways are formed; by the adoption of the Friedel-Crafts crosslinking method for the external crosslinking agent, micropores and mesoporous are formed by crosslinking capsule walls made of polymer materials; the apertures of the formed holes and the crosslinking degree are adjusted according to the type of the crosslinking agent; a foundation is laid for the application; communicating windows formed among the micropores, the mesoporous and the interlocking microcapsules in the capsule walls and the slits between the microcapsules adopt classified hole interlocking structures in the mass.

Description

technical field [0001] The technical solution of the invention relates to the field of polymer materials, in particular to a preparation method of polymer-based hierarchical pore structure interlocking microcapsules. Background technique [0002] Microcapsule refers to a micro-container with a hollow structure and a shell made 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 active ingredients, and controlling the slow release of the core material. In the late 1970s, Narty et al. (Narty J J, Oppenheim R C, Speiser P.Nanoparticles a new colloidal drug delivery system.Pharmaceutica Acta Helvetiae, 1978,53:17-23.) proposed the concept of nanocapsules (Nanocapsules), the Microcapsules have expanded into new materials with nanoscale dimensions. Microcapsules have developed rapid...

Claims

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Application Information

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IPC IPC(8): B01J13/14
Inventor 张旭田磊王小梅刘盘阁吴翠红杨碧微
Owner HEBEI UNIV OF TECH
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