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Method for preparing hollow microsphere with hydrogel microsphere as stencil

A technology of hydrogel microspheres and microspheres, which is applied in the preparation of microspheres and microcapsule preparations, etc., which can solve the problems of many steps and long time, and achieve the effect of safe preparation process and easy operation

Inactive Publication Date: 2008-02-13
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has many steps and takes a long time, and the process conditions such as pH value and temperature need to be strictly controlled in the final acid-base treatment.

Method used

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  • Method for preparing hollow microsphere with hydrogel microsphere as stencil
  • Method for preparing hollow microsphere with hydrogel microsphere as stencil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Put 5.0g of N-isopropylacrylamide (NIPAAm), 0.05g of N,N'-methylenebisacrylamide (BIS) and 50g of deionized water into a 100ml flask and stir to dissolve, add 0.005g of hexadecyltri Methyl ammonium chloride, 0.25g methacryloyloxyethyltrimethylammonium chloride (DMC), after nitrogen gas for 60 minutes, add 0.05g N,N'-azobisisobutylamidine hydrochloride (AIBA) Heat the oil bath to 75°C, turn on the condensing reflux device to react for 8 hours, naturally cool to room temperature and let stand for half an hour until it swells completely. After purification by dialysis and drying, 0.3 g of the product was taken in 50 ml of deionized water and redispersed by ultrasonic vibration to obtain a suspension of hydrogel microspheres. Put the hydrogel microsphere suspension into a 250ml Erlenmeyer flask as a seed, add 150ml ionized water, 0.05g sodium dodecyl sulfate (SDS) successively, stir and ventilate nitrogen for 60 minutes, then add 0.3g styrene ( St), 0.005g divinylbenzene (...

Embodiment 2

[0030] Put 4.0g of N-isopropylacrylamide (NIPAAm), 0.04g of BIS and 800g of deionized water into a 1000ml flask and stir to dissolve, add 0.4g of cetyltrimethylammonium chloride, 0.2g of styrene benzyl trimethyl Methyl ammonium chloride, after nitrogen gas for 60 minutes, then add 0.02g AIBA to raise the temperature of the oil bath to 60°C, turn on the condensing reflux device to react for 72 hours, naturally cool to room temperature and let it stand for half an hour until it is completely swollen, after dialysis and purification, After drying, 0.3 g of the product was taken and dispersed in 100 ml of deionized water to obtain a suspension of hydrogel microspheres. Put the hydrogel microsphere suspension into a 250ml Erlenmeyer flask as a seed, add 150ml ion water, 0.15g sodium bis(2-ethylhexyl) sulfosuccinate, 2.0g St, 0.05gDVB and 0.05 gKPS, stirred and passed nitrogen for 10 minutes, then added 0.024g SSA to react for 1 hour, and obtained polystyrene hollow microspheres aft...

Embodiment 3

[0032] Put 5.0g of N-isopropylacrylamide (NIPAAm), 0.01g of BIS and 500g of deionized water in a 1000ml flask and stir to dissolve, add 1g of styrene benzyltrimethylammonium chloride, and after nitrogen gas for 60 minutes, add 0.005g AIBA Heat the oil bath to 60°C, turn on the condensing reflux device to react for 72 hours, naturally cool to room temperature and let stand for half an hour until it swells completely. After purification by dialysis and drying, 0.3 g of the product was taken and dispersed in deionized water to obtain a suspension of hydrogel microspheres. Take 50ml of the hydrogel microsphere suspension and put it into a 250ml Erlenmeyer flask as a seed, add 150ml of ionized water, 0.057gSDS, 10.0g styrene (St), 0.5g divinylbenzene (DVB) and 0.12gKPS successively, stir Nitrogen was passed for 10 minutes, and then 0.06 g of sodium sulfite (SSA) was added to react for 1 hour. After drying, polystyrene hollow microspheres were obtained ( FIG. 3 ).

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Abstract

The present invention discloses a hollow microsphere preparation method, which uses a hydrogel microsphere as a template. The preparation method is that an emulsion or inverse emulsion polymeric method is adopted to synthesize the hydrogel microsphere with electric charge. A surfactant with inverse electric charge and hydrophobic monomer are added into the hydrogel microsphere suspension, and the hydrogel microsphere is coated by a polymer crust layer of the hydrophobic monomer by a seed emulsion polymerization method to form a core-shell microsphere with an inner layer of hydrogel and an outer layer of polymer; a hydrolyzation of a silicon dioxide or titanium dioxide precursor is used to form the core-shell microsphere with the outer layer of inorganic matter and the inner layer of hydrogel. The core-shell microsphere is dried to obtain the hollow microsphere. The method of the present invention does not need removing the template by organic impregnant dissolving, strong acid or strong alkali etching or high temperature calcining; the preparation process is safe and the operation is simple; and the hollow microsphere with different chemical components can be obtained by changing core or shell.

Description

technical field [0001] The invention relates to a method for preparing hollow microspheres using hydrogel microspheres as templates. Background technique [0002] Nanoscale and submicron-scale polymer hollow microspheres have received more and more attention in recent years, and they have broad application prospects in cosmetics, coatings, inks, biomedicine, and paper manufacturing industries. The successful development of hollow microspheres is one of the three major achievements that have changed the coatings industry in the past 40 years. Due to the hollow structure of the hollow particles, there is a large difference in the refractive index between the shell polymer and the inner core air, and multiple refractions occur when the light passes through the hollow microspheres, so the hollow microspheres have effective covering properties and can replace expensive As a white pigment, titanium dioxide can save costs and improve the stain resistance and wash resistance of coa...

Claims

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Application Information

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IPC IPC(8): B01J13/14
Inventor 彭懋陈颖王慧珺
Owner ZHEJIANG UNIV
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