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Preparation method of raspberry type pH value/temperature sensitive polymer microcapsules

A polymer and sensitive technology, applied in the preparation of microspheres, microcapsule preparations, etc., can solve the problems of uneven particle size of products, difficulty in obtaining nano or submicron microcapsules, etc., and achieve increased specific surface area and size Uniform size and stable performance

Active Publication Date: 2018-04-17
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing polymer microcapsules mostly adopt latex particle liquid surface self-assembly method, Velev [Velev OD, Furusawa K, Nagayama K.Langmuir, 1996, 12, 2374; Velev OD, Nagayama K.Langmuir, 1997, 13, 1856 -1859.] and others made this technology for preparing microcapsules public, after Croll and Stover [Croll L M, Stover H D.Langmuir, 2003, 19, 10077.] and others further improved, they used surface crosslinking The method of immobilizing microcapsules, but this method is difficult to obtain nanometer or submicron microcapsules
He Xiaodong [10] et al. improved the self-assembly technology of PS microspheres to prepare microspheres with a size down to a few microns. However, there are many kinds of polymerization in this method, resulting in very uneven particle sizes of the obtained products.

Method used

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  • Preparation method of raspberry type pH value/temperature sensitive polymer microcapsules
  • Preparation method of raspberry type pH value/temperature sensitive polymer microcapsules
  • Preparation method of raspberry type pH value/temperature sensitive polymer microcapsules

Examples

Experimental program
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Embodiment 1

[0030] 1. Preparation of polymethacrylic acid

[0031] Take 65mL of acetonitrile to a 100mL round bottom flask, add 15mL of MAA, add 0.060g of AIBN to start heating, and control to evaporate 40mL of acetonitrile in 1h to end the heating. After the product was cooled, the product was suction-filtered with a sand core funnel, and after being washed three times continuously with anhydrous acetonitrile, the particle size of the obtained PMAA microspheres was 1500 nm, and they were dispersed in 40 mL of anhydrous acetonitrile for subsequent use.

[0032] 2. Preparation of Silica Microspheres

[0033] Add 50mL of ethanol, 1mL of distilled water, and 1.1mL of concentrated ammonia water into a 100mL flask, stir at 25°C for 30min, add 1mL of TEOS, continue stirring for 5h, then add 0.05mL of APTES, and stir for 12 hours to end the reaction. Then centrifuge at 10000r / min for 10min, wash with ethanol until pH = 7, and obtain SiO with amino groups on the surface. 2 Microspheres, the par...

Embodiment 2

[0039] 1. Preparation of polymethacrylic acid

[0040] Take 70mL of acetonitrile into a 100ml round bottom flask, add 10mL of MAA, add 0.060g of AIBN to start heating, and control to evaporate 40mL of acetonitrile in 1h to end the heating. After the product is cooled, the product is suction-filtered with a sand core funnel, and after being washed three times continuously with anhydrous acetonitrile, the particle size of the obtained PMAA microspheres is 1000 nm, which is dispersed in 40 mL of anhydrous acetonitrile for subsequent use.

[0041] 2. Preparation of Silica Microspheres

[0042] Add 50mL of ethanol, 1mL of distilled water, and 1.1mL of concentrated ammonia water into a 100mL flask, stir at 25°C for 30min, add 1mL of TEOS, continue stirring for 5h, then add 0.05mL of APTES, and stir for 12 hours to end the reaction. Then centrifuge at 10000r / min for 10min, wash with ethanol until pH = 7, and obtain SiO2 microspheres with amino groups on the surface, the particle dia...

Embodiment 3

[0048] 1. Preparation of polymethacrylic acid

[0049] Take 75mL of acetonitrile into a 100ml round bottom flask, add 5mL of MAA, add 0.060g of AIBN to start heating, and control to evaporate 40mL of acetonitrile in 1h to end the heating. After the product is cooled, the product is suction-filtered with a sand core funnel, and after being washed three times continuously with anhydrous acetonitrile, the particle size of the obtained PMAA microspheres is 800nm, which is dispersed in 40mL of anhydrous acetonitrile for subsequent use.

[0050] 2. Preparation of Silica Microspheres

[0051] Add 50mL of ethanol, 1mL of distilled water, and 1.1mL of concentrated ammonia water into a 100mL flask, stir at 25°C for 30min, add 1mL of TEOS, continue stirring for 5h, then add 0.05mL of APTES, and stir for 12 hours to end the reaction. Then centrifuge at 10000r / min for 10min, wash with ethanol until pH = 7, and obtain SiO with amino groups on the surface. 2 Microspheres, the particle size...

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Abstract

The invention provides a preparation method of raspberry type pH value / temperature sensitive polymer microcapsules. In an experiment, small-size microspheres are taken as a crown, large-size polymer microspheres are taken as a core, raspberry type core-crown microspheres are prepared with a self-assembly technique, core-shell compound microspheres with pH value / temperature sensitive shell layers are prepared with the core-crown microspheres as a template, then, a strong alkaline solution is used for etching, and the polymer microcapsules are obtained. The cavity sizes, the wall thickness and the inner diameters of the bulge parts on the walls of the microcapsules are controllable. The polymer microcapsules have double properties of pH value sensitivity and temperature sensitivity, and theswelling ratio and the particle size of the microcapsules change remarkably with the pH value and temperature. Besides, the preparation method also has the advantages that the method is simple, the size is controllable, the dispersity is good, the product purity is high, the performance is stable and the like. Surface bulges can effectively amplify the sensitive effect, so that the microcapsules have higher application value and attract much attention in the aspects of catalyst carriers, disease diagnosis, targeted therapy and the like.

Description

technical field [0001] The invention relates to a preparation method of a raspberry-type pH value / temperature sensitive polymer microcapsule, wherein the thickness of the microcapsule wall and the size of the cavity are controllable, and belongs to the field of functional polymer materials. Background technique [0002] Today, with the increasing development of the microstructure of matter, it has attracted much attention to construct the fine structure of materials so that they have corresponding macroscopic properties. The research and discovery of new polymer materials, as well as the continuous improvement of material structure and performance requirements in various industries, have led to the emergence of functional polymer microcapsules. [0003] Polymer microcapsules generally have the characteristics of small and uniform particle size, large specific surface area, large hollow part volume and unbreakable structure, and are widely used in petrochemical, biomedicine, ...

Claims

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Application Information

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IPC IPC(8): C08F220/54C08F222/38C08J9/28C08F120/14B01J13/14
CPCB01J13/14C08F120/14C08F220/54C08F222/385C08J9/28
Inventor 刘巍李培森周士乐魏俊富许浩
Owner TIANJIN POLYTECHNIC UNIV