Synthesis of divinylbenzene-maleic anhydride microspheres using precipitation polymerization

Frank, Randy S.; Downey, Jeffrey S.; Stöver, Harald D. H.

doi:10.1002/(sici)1099-0518(19980930)36:13<2223::aid-pola8>3.0.co;2-u

Cited by 65 publications

(55 citation statements)

References 2 publications

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“…7,13,14 Precipitation polymerization as briefly mentioned earlier has found that fully crosslinked microspheres can be prepared in a simple single stage process. 15 Various monomers including methacrylate, 16 maleic anhydride, 17 and chloromethyl styrene 18 have been copolymerized to form miscrospheres with divinylbenzene (DVB) as the crosslinkable monomer using the precipitation polymerization.…”

Section: Introductionmentioning

confidence: 99%

Size and uniformity variation of poly(MMA-co-DVB) particles upon precipitation polymerization

et al. 2004

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Stable poly(methyl methacrylate-co-divinylbenzene) (poly(MMA-co-DVB)) microspheres were prepared by precipitation polymerization using acetonitrile as the main medium under various polymerization conditions, including modifications of the agitation speed, monomer and initiator concentrations, DVB content in the monomer mixture, and the use of various cosolvents. Gentle agitation was required to obtain smooth spherical particles. The individually stable microspheres were obtained at monomer concentrations of up to 15 vol% in an acetonitrile medium. The number-average diameter increased linearly with respect to increases in the monomer and initiator concentrations. We found, however, that the uniformity of the microspheres was independent of the variation of the polymerization ingredients because nuclei formation was solely influenced by the crosslinking reaction of the monomers. We obtained higher yields for the polymerization at higher concentrations of monomer and initiator. The concentration of DVB in the monomer mixture composition played an important role in determining not only the size of the microspheres but also the yield of the polymerization. In addition, although we employed various cosolvents as the polymerization medium, we found that acetonitrile/2-methoxyethanol was the only system that provided spherical particles without coagulation. This finding indicates that the precipitation polymerization is strongly dependent on the solvent used as the medium.

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Section: Introductionmentioning

confidence: 99%

Size and uniformity variation of poly(MMA-co-DVB) particles upon precipitation polymerization

et al. 2004

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“…[15][16][17] Most recently, the precipitation polymerization of crosslinkable monomer has been found that fully crosslinked microspheres can be prepared even without any stabilizers in the polymerization system. 18 Several monomers including methacrylate, 19 maleic anhydride, 20 and chloromethyl styrene 21 have been copolymerized to form microspheres with DVB as the crosslinkable monomer using the precipitation polymerization. The precipitation polymerization is quite similar to dispersion polymerization beside the absence of steric stabilizer.…”

Section: Introductionmentioning

confidence: 99%

Thermally robust highly crosslinked poly(methyl methacrylate-co-divinyl benzene) microspheres by precipitation polymerization

et al. 2004

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We prepared thermally robust fully crosslinked poly(methyl methacrylate-co-divinyl benzene) [poly(MMAco-DVB)] microspheres successfully by precipitation polymerization in the absence of a stabilizing agent. The DVB concentration plays a pivotal role not only in the formation of the individually stable microspheres but also in the polymerization characteristics, including the particle size, the uniformity of size, the polymerization yield, and the thermal properties. The number-average diameter of the microspheres increased linearly, from 0.72 to 2.15 μm, and the particle size distribution became narrower, by elevating the uniformity from 1.35 to 1.12, as the DVB concentration increased from 20 to 75 mol%. In addition, the yield of the polymerization increased, from 73.4 to 98.6%, as the DVB concentration increased. Since the prepared particles possess fully crosslinked microstructures, no glass transition temperatures were observed, but all the samples prepared with DVB concentrations ranging from 20 to 75 mol% possess enhanced thermal properties. Based on the DSC and TGA data, the thermal stability of the microspheres prepared by the precipitation polymerization is significantly improved as a result of crosslinking with DVB.

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“…Therefore, homoand copolymerization systems have been thoroughly investigated, including poly(divinylbenzene), 15 poly (methacrylic acid-co-polyethylene oxide methyl ether methacrylate), 16 poly(methacrylate-co-divinylbenzene), 17 poly(chloromethylstyrene-co-divinylbenzene), 18 poly(divinylbenzene-co-maleic anhydride) 19 , poly(methyl methacrylate-co-divinylbenzene)…”

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Synthesis of poly(acrylamide‐co‐divinylbenzene) microspheres by precipitation polymerization

Jin

Yang

Shim

et al. 2005

J. Polym. Sci. A Polym. Chem.

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The synthesis and application of polymeric microspheres are of great importance from both academic and industrial points of view. As polymeric microspheres have been used in wider fields of conventional 1 and more sophisticated 2-6 areas, the development of a new process to prepare such materials has received much attention. Polymer microspheres of a particular size and uniformity are generally obtained with one of the heterogeneous polymerizations, including suspension, emulsion, dispersion, seeded, and precipitation polymerizations. Moreover, each polymerization is branched to several subsidiary methods, such as macroemulsion, miniemulsion, microemulsion, and soap-free emulsion polymerizations.Fully crosslinked monodisperse polymer microspheres have unique applications because of their superior strength, thermal and solvent resistance, and antislip properties.7 However, the synthesis of such microspheres is limited to a few techniques, such as seeded polymerization, [8][9][10][11] Shirasu porous glass (SPG) membrane emulsification followed by postpolymerization, 12,13 and precipitation polymerization.14 Precipitation polymerization, in particular, has advantages over the other techniques because crosslinked microspheres can be readily prepared in a single process without any auxiliary apparatus to make the size distribution of the particles narrow. Therefore, homoand copolymerization systems have been thoroughly investigated, including poly(divinylbenzene), 15 poly (methacrylic acid-co-polyethylene oxide methyl ether methacrylate), 16 poly(methacrylate-co-divinylbenzene), 17 poly(chloromethylstyrene-co-divinylbenzene), 18 poly(divinylbenzene-co-maleic anhydride) 19 , poly(methyl methacrylate-co-divinylbenzene)[poly(MMA-co-DVB)], [20][21][22] and poly(styrene-co-divinylbenzene) [poly(St-co-DVB)]. 23In addition, mechanistic studies to elucidate the formation of stable microspheres in the absence of any stabilizer have been reported 24,25 in which the absorption of oligomeric species onto the nuclei and the high degree of crosslinking are the primary reasons for the formation and stable growth of the microspheres.Several examples of the copolymerization of the partially water-soluble monomer acrylamide (AAm) and oil-soluble monomers such as methacrylic acid 26 and styrene 27,28 have been recently reported with precipitation polymerization, 26 inverse microemulsion polymerization, 27 and water/oil/water emulsion by SPG membrane emulsification and subsequent suspension polymerization. 28In our previous studies, poly(St-co-DVB) and poly (MMA-co-DVB) microspheres containing various concentrations of divinylbenzene (DVB), from 5 to 75 mol %, were synthesized by precipitation polymerization, and their unexpected thermal properties, superior to those of crosslinked polymers prepared by emulsion and

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Synthesis of divinylbenzene-maleic anhydride microspheres using precipitation polymerization

Cited by 65 publications

References 2 publications

Size and uniformity variation of poly(MMA-co-DVB) particles upon precipitation polymerization

Size and uniformity variation of poly(MMA-co-DVB) particles upon precipitation polymerization

Thermally robust highly crosslinked poly(methyl methacrylate-co-divinyl benzene) microspheres by precipitation polymerization

Synthesis of poly(acrylamide‐co‐divinylbenzene) microspheres by precipitation polymerization

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