A kind of preparation method of functionalized polymer microsphere

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

Active Publication Date: 2020-10-27
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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

Method used

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  • A kind of preparation method of functionalized polymer microsphere
  • A kind of preparation method of functionalized polymer microsphere
  • A kind of preparation method of functionalized polymer microsphere

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 Washed several times, dried 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

A method for preparing functional polymer microspheres belongs to the technical field of functional polymer preparation. The present invention takes oil-soluble multifunctionality acrylate monomer, polyethyleneimine and photoinitiator as raw materials, and the weight ratio of multifunctionality acrylate monomer, photoinitiator, polyethyleneimine and water solvent is 100:( 1~5): (5~20): (500~2000). After the system is evenly mixed, it is first emulsified under the action of a high-speed disperser, and then subjected to ultraviolet light irradiation to obtain multifunctional acrylate polymer microspheres. Then Michael addition reaction occurs with polyethyleneimine to obtain functional polymer microspheres with active primary and secondary amino groups on the surface. The invention obtains surface aminated functional polymer microspheres, the reaction energy consumption is low, and the reaction rate and reaction yield can be adjusted through time. The particle size of polymer microspheres can be adjusted within the range of 2μm-100μm. Polyethyleneimine is used not only as a stabilizer during the formation of microsphere polymerization, but also as a modifier during the modification of microspheres.

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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Patent Type & Authority Patents(China)
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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