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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 bonding, these greatly limit the application of the double-template method in the preparation of polymer-based porous materials; (2) for the emulsion polymerization method, the suitable surfactant and ratio are The key to determining the size of the pores, and the pores synthesized by using liquid droplets as templates are prone to collapse and shrinkage, and the pore structure is unstable.
[0006] At present, there is no relevant report on the preparation method of polymer-based hierarchical pore structure interlocking microcapsules combining surface-induced atom transfer radical polymerization, double bond radical polymerization and Friedel-Crafts crosslinking method

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

Embodiment 1

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

[0064] Add 145g of absolute ethanol, 34.1g of ammonia water with a mass fraction of 25%, and 35.0g of deionized water to a 500mL three-necked bottle equipped with mechanical stirring at room temperature. After stirring evenly, quickly add 15.4g of orthosilicon Acid ethyl ester, reacted at room temperature for 8h. Transfer the obtained suspension into a beaker, wait for the solvent to volatilize completely naturally, and obtain a colloidal silica template with an average particle size of 600nm, and finally sinter the template in a muffle furnace at 500°C for 3 hours, and slowly lower it to room temperature to obtain A silica colloidal crystal template in which silica microspheres with an average particle size of 600nm are adhered to each other;

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

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

example 1

[0076] Example 1 The surface area of ​​the obtained material measured by the model Micromeritics ASAP2020M+C automatic specific surface area analyzer can reach 600m 2 g -1 .

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

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

Embodiment 2

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

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

[0082] γ-methacryloyloxypropyltrimethoxysilane (MPS) modified silica colloidal crystal template, put 0.3g of dried and sintered silica colloidal crystal template into a 250mL three-necked bottle, add 100ml of ethanol , distilled water 2.5mL, ammonia water 0.25mL, stirred mechanically at 25°C, added γ-methacryloxypropyltrimethoxysilane (MPS) 1.5mL, condensed and refluxed at room temperature for 24h. Stop stirring after the reaction, discard the liquid, wash and replace with absolute ethanol three times, and finally vacuum-dry at 25°C for 12 hours to obtain an MPS-modified silica colloidal crystal template with an average particle size of 600nm;

[0083] (3) Silica colloidal crystal template controllable grafting of polymer segments

[0084] Add 0.03 g of MPS-modified silica colloidal crystal temp...

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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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