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Preparation method of functionalized polymer microspheres

A technology of polymer microspheres and functionalization, applied in the field of functional polymers, can solve the problems of cumbersome process, complicated process, solvent pollution, etc., and achieve the effect of energy saving in the preparation process and high product purity

Active Publication Date: 2018-07-31
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional polymer microsphere modification method is complex, cumbersome, and brings additional solvent pollution

Method used

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  • Preparation method of functionalized polymer microspheres
  • Preparation method of functionalized polymer microspheres
  • Preparation method of functionalized polymer microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Dissolve 0.08 g of the initiator 2,4,6-(trimethylbenzoyl)diphenylphosphine oxide in 8 g of trimethylolpropane triacrylate, and place it in a glass reaction vessel filled with 120 mL of deionized water Among them, use a disperser to emulsify the mixed solution for 20 minutes (set the speed at 2500rpm, and maintain it until the end of the light), add 20mL of an aqueous solution of branched polyethyleneimine (concentration is 0.05kg / L); cm 2 Under the irradiation reaction for 40 minutes, the obtained product was washed, centrifuged and dried to obtain polymer microspheres with a particle size of 2-8 μm and a yield of 82%. The particle size and morphology are shown in figure 1 SEM photographs. Take 2 g of the obtained polymer microspheres and place them in a glass reaction vessel containing 20 mL of branched polyethyleneimine aqueous solution (concentration: 0.1 kg / L), pass nitrogen into the system for 10 min, seal it, and heat it at 80 ° C for 10 h. The obtained polymer ...

Embodiment 2

[0022] Dissolve 0.1 g of the initiator 2,4,6-trimethylbenzoyl ethyl phosphonate in 6 g of trimethylolpropane trimethacrylate, and place it in a glass reaction vessel filled with 100 mL of deionized water. The disperser was emulsified for 15min (the speed was set at 2500rpm and maintained until the end of the light), and 10mL of the aqueous solution of branched polyethyleneimine was added (the concentration was 0.05kg / L); 2 Under the irradiation reaction for 60 minutes, the obtained product is washed, centrifuged and dried to obtain polymer microspheres with a particle size of 8-15 μm and a yield of 78%. Place 1 g of the obtained polymer microspheres in a glass reaction vessel containing 20 mL of branched polyethyleneimine aqueous solution, pass nitrogen gas into the system for 8 minutes, seal it, heat at 60°C for 8 hours, and take 1 g of the obtained polymer microspheres to centrifuge Washing several times, drying to obtain the target product.

Embodiment 3

[0024] Dissolve 0.5 g of the initiator bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide in 10 g of 1,6-hexanediol diacrylate, and place in a glass reaction vessel filled with 50 mL of deionized water Among them, the disperser was emulsified for 15 minutes (the speed was set at 2300rpm and maintained until the end of the light), and 25mL of an aqueous solution of branched polyethyleneimine was added (the concentration was 0.05kg / L); 2 Under irradiation for 90 minutes, the obtained product is washed, centrifuged and dried to obtain polymer microspheres with a particle size of 40-80 μm and a yield of 76%. Take 0.8g of the obtained polymer microspheres and place them in a glass reaction vessel with 20mL of branched polyethyleneimine aqueous solution (concentration: 0.1kg / L), pass nitrogen into the system for 5 minutes, seal it, and heat it at 100°C for 1 hour. The obtained polymer microspheres were centrifuged and washed several times, and dried to obtain the target product.

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Abstract

The invention relates to a preparation method of functionalized polymer microspheres, belonging to the technical field of preparation of functional polymers. According to the preparation method, an oil-soluble polyfunctionality acrylate monomer, polyethyleneimine and a photoinitiator are used as raw materials, wherein the weight ratio of the polyfunctionality acrylate monomer to the photoinitiatorto the polyethyleneimine to a water solvent is equal to 100 to (1-5) to (5-20) to (500-2000). After the system is uniformly mixed, emulsification is firstly carried out under the action of a high-speed disperser, and ultraviolet light irradiation is performed after the emulsification is finished, so that polymer microspheres of polyfunctionality acrylate are obtained; after that, the polymer microspheres and polyethyleneimine are subjected to a Michael addition reaction, so that the functional polymer microspheres having surfaces modified by active primary amino groups and secondary amino groups. The functional macromolecular microspheres, which are prepared by the method and have aminated surfaces, are low in reaction energy consumption, and the reaction rate and the reaction yield can be adjusted by means of time. The particle sizes of the polymer microspheres can be adjusted within a range of 2-100mu m. The polyethyleneimine not only serves as a stabilizer in a formation process ofthe microspheres, but also can be used as a modifier in a microsphere modification process.

Description

technical field [0001] The invention belongs to a method for preparing surface aminated functional polymer microspheres and belongs to the technical field of functional polymers. Background technique [0002] Polymer microspheres refer to polymer particles with diameters ranging from tens of nanometers to hundreds of microns. The small particle size and volume make the whole particle responsive and fast to external stimuli as a microreactor. The characteristics of large specific surface area and controllable particle size make polymer microspheres have special and important applications in biomedicine, electronic information, coatings, water treatment and other fields. [0003] Polymer microspheres can be synthesized by means of emulsion polymerization, precipitation polymerization and bulk polymerization. The disadvantage of emulsion polymerization is that the emulsifier in the product is not easy to remove, and it is easy to affect the final properties of the product. T...

Claims

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Application Information

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IPC IPC(8): C08G81/00C08F283/00C08F222/14C08F222/20C08F220/32C08F2/48C08F2/18C02F1/28C02F101/20
CPCC02F1/285C08F2/18C08F2/48C08F283/00C08G81/00C02F2101/20C08F222/104C08F220/32C08F222/102C08F222/103
Inventor 聂俊李卿朱晓群
Owner BEIJING UNIV OF CHEM TECH
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