Large particle diameter mono-disperse polymer microspheres containing epoxy group and preparation method thereof
A technology of polymer microspheres and epoxy groups, applied in the field of polymer microspheres and their preparation, can solve the problems that separation accuracy and purification efficiency cannot be guaranteed, separation and low reactivity, etc. Broad application prospects, great agglutination effect
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Embodiment 1
[0046] Prepare PS seed microspheres as follows:
[0047] Take by weighing 60 g of aqueous ethanol solution with a volume concentration of 95%, 1.2 g of PVP (polyvinylpyrrolidone), 0.3 g of AIBN (azobisisobutyronitrile), and 30 g of styrene, mix them uniformly and place them in a machine equipped with mechanical stirring and reflux condensation. tube and a nitrogen-protected three-neck flask were polymerized in a water bath at 70°C for 8 hours, and cooled and left to stand after the reaction was completed. Centrifuge the emulsion obtained by the reaction at a speed of 4000r / min, pour off the supernatant, add absolute ethanol to ultrasonically disperse, and then centrifuge; repeat this process for 3 times to remove unreacted monomers and dispersion stabilizers . Dry under vacuum at 60°C for 8 hours to obtain PS seed microspheres as a white powder product. The particle size of the styrene seed microspheres is 2.1 μm, and the distribution index is 3.2%.
[0048] Pre-swell:
[00...
Embodiment 2
[0056] Preparation of PMMA seed microspheres:
[0057] With 1.5g dispersant PVP (polyvinylpyrrolidone), 10g monomer MMA (methyl methacrylate), 0.1g initiator AIBN (azobisisobutyronitrile), be dissolved in the mixed solvent that ethanol and water form (ethanol : water=11:9), drop into the there-necked flask that stirrer is housed, reflux condenser and nitrogen protection device, react 6h at 70 ℃, cool after reaction finishes, leave standstill, then carry out centrifugal sedimentation with 3000r / min rotating speed , pour off the supernatant, add absolute ethanol to wash, and then centrifuge; repeat this way for 3 times to remove unreacted monomers, oligomers and dispersion stabilizers, and finally dry at 60°C for 24h under vacuum to obtain White powder product PMMA seed microspheres, ready for use.
[0058] Get above-mentioned PMMA microsphere 0.7g and DBP (glycidyl methacrylate) 0.1g and join in 25g containing SDS (sodium dodecyl sulfate) 0.3% (wt) aqueous solution respectivel...
Embodiment 3
[0061] Get PS seed microsphere 0.7g prepared in Example 1 and DBP (glycidyl methacrylate) 0.07g and join in 30g containing SDS (sodium dodecyl sulfate) 0.2% (wt) aqueous solution respectively, ultrasonic emulsification 55min respectively , the emulsions were mixed together, stirred in a three-neck flask equipped with mechanical stirring, reflux condenser, and nitrogen protection, and swelled at 35° C. for 12 hours to obtain primary expanded polystyrene microspheres (4.8 μm). Take GMA (glycidyl methacrylate) 0.7g, BPO (dibenzoyl peroxide) 0.035g, mix and dissolve, add to 140g SDS (sodium dodecyl sulfate) 0.2% (wt) aqueous solution and ultrasonically emulsify for 20min , then slowly added dropwise into the system, continued swelling for 6 hours, then added 0.7g of polyvinylpyrrolidone, raised the temperature to 60°C, polymerized for 8 hours, and synthesized a monodisperse polystyrene resin with a particle size of 7 μm and containing epoxy groups. The rate is 93%.
[0062] The p...
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