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Layer-by-layer microcapsule assembling process based on mutual covalent action

A technology of microcapsules and covalent bonds, which is applied in the field of preparation of polymer hollow microcapsules to achieve fast reaction speed and easy functionalization

Inactive Publication Date: 2007-08-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Method used

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  • Layer-by-layer microcapsule assembling process based on mutual covalent action
  • Layer-by-layer microcapsule assembling process based on mutual covalent action
  • Layer-by-layer microcapsule assembling process based on mutual covalent action

Examples

Experimental program
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Effect test

Embodiment 1

[0027] 4 g of silica particles with a diameter of 1 μm were suspended in a toluene solution containing 5% γ-aminopropyltriethoxysilane by stirring overnight, then centrifuged, washed twice with toluene, and then washed twice with ethanol. Second, dry. Suspend 1 g of aminated silica particles in 4 mg / ml polyglycidyl methacrylate solution in tetrahydrofuran, pass nitrogen gas for 10 minutes, stir at 60°C for 3 hours, then centrifuge, and wash three times with tetrahydrofuran solvent Then these particles were suspended in the aqueous solution of 4 mg / ml polyallylamine by stirring, nitrogen gas flowed for 10 minutes, stirred at 80° C. for 3 hours, then centrifuged, and washed with water three times. Repeat the above process until the number of assembled layers reaches 7, then use 0.4mol / L hydrofluoric acid to remove the silica particles, and perform an atomic force microscope test on the mica sheet. Figure 1a is the AFM image of the microcapsules, and Figure 1b is the magnified A...

Embodiment 2

[0029] 4 g of silica microparticles with a diameter of 1 μm were suspended overnight in toluene containing 5% γ-aminopropyltrimethoxysilane by sonication, then centrifuged and washed twice with toluene and then twice with methanol ,drying. Suspend 1 g of aminated silica microparticles in 8 mg / ml polyglycidyl methacrylate in tetrahydrofuran solution by ultrasonication, blow nitrogen for 20 minutes, stir at 20°C for 10 hours, then centrifuge and wash with acetone Three times; then these particles were suspended in 2 mg / ml polyallylamine aqueous solution by ultrasonic, nitrogen gas was passed for 20 minutes, stirred at 80° C. for 1 hour, then centrifuged, and washed with water three times. Repeat the above process until the number of assembled layers reaches 7 layers. Figure 2a is the transmission electron microscope image when the silicon dioxide is not removed, and Figure 2b is the transmission electron microscope image after the silicon dioxide is removed with 0.1mol / L hydrofl...

Embodiment 3

[0031] Suspend 4 g of silica particles with a diameter of 1 micron in a toluene solution containing 10% γ-aminopropyltrimethoxysilane by stirring overnight, then centrifuge, wash with toluene 5 times, and dry. Suspend 1 g of aminated silica particles in 1 mg / ml polyglycidyl methacrylate in tetrahydrofuran solution by stirring, blow nitrogen for 30 minutes, stir at 60 °C for 4 hours, then centrifuge and wash with chloroform Three times; these particles were then suspended in an aqueous solution of 1 mg / ml polyallylamine, passed through nitrogen for 10 minutes, stirred at 20° C. for 10 hours, then centrifuged, and washed with water 5 times. Repeat the above-mentioned process until the number of layers assembled reaches 7 layers, then remove silicon dioxide with 0.4mol / L hydrofluoric acid, drop the microcapsule suspension on the mica sheet and carry out scanning electron microscope observation, prove that the gained microcapsules have a hollow structure ( image 3).

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Abstract

The layer-by-layer microcapsule assembling process based on mutual covalent action includes: the reaction of two kinds of polymer on the surface of aminated silica grains to obtain super thin polymer film in multilayer structure; and subsequent eliminating inorganic grains with hydrofluoric acid to obtain hollow microcapsule with wall of covalent cross-linked multilayer film structure. The microcapsule thus obtained has the features of adjustable wall thickness of nanometer or submicron level, high strength, high stability and acid, alkali and salt corrosion resistance, and easy functionalization. The microcapsule may be used in medicine, dye, cosmetics, sensor and other fields.

Description

technical field [0001] The invention relates to a preparation method of polymer hollow microcapsules. Specifically, the interaction of covalent bonds is used to form a polymer film with a multilayer structure through the layer-layer assembly reaction of two reactive polymers on the surface of silica colloidal particles; then the silica colloidal particles are removed. , to obtain microcapsules with a covalently cross-linked multilayer film structure. Background technique [0002] A microcapsule is a substance that separates the space inside the capsule from the space outside the capsule by a film-forming substance to form a specific geometric structure, and its interior can be filled or hollow. The shape of the microcapsules is mainly spherical, and can also be oval, square or rectangular, polygonal and various irregular shapes. The size of traditional microcapsules is usually on the order of microns to millimeters, and the wall thickness is from submicron to hundreds of m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/02
Inventor 高长有封志强王志鹏沈家骢
Owner ZHEJIANG UNIV
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