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Micron-sized cross-linked polymer hollow microspheres and preparation method for same

A technology of cross-linked polymers and hollow microspheres, applied in the field of polymer materials, can solve the problems of application limitations of hollow microspheres, low output of hollow microspheres, small particle size of hollow microspheres, etc.

Active Publication Date: 2015-08-19
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are many methods for preparing polymer hollow microspheres. Among them, in the 1980s, Kowalski et al. reported the use of alkali swelling emulsion method to prepare polymer hollow microspheres in the patent US Patent 4427836, and this method has been industrialized, but the method There are disadvantages such as complicated steps and small particle size of prepared hollow microspheres
In the patent CN200710132704 (disclosure date: February 20, 2008), a preparation method of nano-scale cross-linked polystyrene hollow microspheres is disclosed. Divinylbenzene, hydrophobic organic matter and oil-soluble initiator are mixed and then added to the water phase containing emulsifier and co-emulsifier. After pre-emulsification, the temperature rises and polymerizes under stirring to obtain cross-linked styrene hollow microspheres. The process is simple , but the size of hollow microspheres is at the submicron level, which limits the wider application of hollow microspheres
Okubo et al. prepared micron-sized hollow microspheres by a dynamic swelling method. This method first prepared polystyrene seed microspheres, and then added them to an ethanol solution of toluene and divinylbenzene, and slowly added water to make the toluene and divinylbenzene swell into the seed microspheres, and finally initiate polymerization to obtain polymer hollow microspheres. Although the hollow microspheres prepared by this method reach the micron level, the yield of the hollow microspheres is too low, and the reaction takes too long

Method used

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  • Micron-sized cross-linked polymer hollow microspheres and preparation method for same
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  • Micron-sized cross-linked polymer hollow microspheres and preparation method for same

Examples

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Embodiment 1

[0021] Dissolve 1.0g dispersant polyvinyl alcohol and 0.1g auxiliary dispersant sodium lauryl sulfate in 210g deionized water, weigh 0.2g azobisisobutyronitrile, 18.0g styrene, 1.0g methyl methacrylate, Put 14.0g toluene and 1.0g hexadecane in a 100mL beaker, mix well, then add to the water phase, pre-emulsify at 3000rpm for 15min, then transfer the emulsion to a four-necked flask at a speed of 300rpm, and heat up to 70 ℃, after reacting for 2 hours, add 2.0 g of divinylbenzene, continue to keep warm at 70 ℃ for 12 hours, then discharge, and after centrifugal washing and drying, cross-linked polymer hollow microspheres are obtained.

[0022] TEM test: Dilute the obtained hollow microspheres with deionized water to about 2% by mass, ultrasonically disperse them for 30 minutes, add them dropwise to a special copper grid, and use TECNAI G 2 F30 transmission electron microscope observation and characterization.

[0023] Calculation of hollowness (A): measure the outer diameter (D...

Embodiment 2

[0025] In the preparation method of the micron-scale cross-linked polymer hollow microspheres in this embodiment, 18 g of methyl methacrylate as the main monomer was added to replace 18 g of styrene, and the others were the same as in Example 1.

Embodiment 3

[0027] In the preparation method of micron-scale cross-linked polymer hollow microspheres in this embodiment, 18 g of butyl methacrylate as the main monomer is added to replace 18 g of styrene, and the others are the same as in Example 1.

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Abstract

The invention discloses micron-sized cross-linked polymer hollow microspheres and a preparation method for the same, and belongs to the field of polymer microsphere materials. A micro-suspension polymerization method is used for preparing the micron-sized cross-linked polymer hollow microspheres. The preparation method comprises the following steps of dissolving a dispersant and a second dispersant into water, then adding a mixed solution of an initiator, various monomers, a pore-forming agent and a co-stabilizer into an aqueous phase, performing pre-emulsification with high-speed stirring, raising temperature for polymerization with low-speed stirring, adding a cross-linking agent after reaction for a certain time, continuing performing reaction for a certain time, and centrifugally washing and drying products to obtain the cross-linked polymer hollow microspheres after reaction is finished. The hollow microspheres prepared by the method have large particle sizes and the advantages of low density, high light scattering performance, large specific surface area, high thermal insulating property and the like, and are widely applied to the fields of lightweight fillers, high-performance opaque coatings, microcapsules, leather and the like.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a preparation method of micron-scale crosslinked polymer hollow microspheres. Background technique [0002] Polymer hollow microspheres are a kind of functional microsphere materials with special properties. Compared with solid microspheres, polymer hollow microspheres have the advantages of low density and high specific surface area due to their internal cavity structure, and polymer hollow microspheres The refractive index of the inner cavity of the microsphere is different from that of the shell layer. After the light enters, it will be refracted multiple times in it, so that it has excellent light scattering performance, heat insulation, sound absorption and light covering performance. Performance Blackout coatings, microcapsules, leather and other fields are widely used. At present, there are many methods for preparing polymer hollow microspheres. Among them, in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F220/14C08F220/18C08F220/06C08F212/36C08F222/14C08J9/28
Inventor 李效玉王雷雷邱藤何立凡郭隆海叶俊
Owner BEIJING UNIV OF CHEM TECH
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