Preparation of aqueous crosslinked dispersions of functionalized poly(d,l-lactic acid) with a thermomechanical method

Virpi Rämö (Corresponding Author), Adina Anghelescu-Hakala, Leena Nurmi, Tuomas Mehtiö, Elina Salomäki, Mika Härkönen, Ali Harlin

    Research output: Contribution to journalArticleScientificpeer-review

    11 Citations (Scopus)


    Aqueous crosslinked microparticle dispersions were prepared from a copolymer of d,l-lactic acid, 1,4-butanediol, and itaconic acid with a thermomechanical method. The copolymer was prepared in one step polycondensation reaction using Sn(Oct)2 as a catalyst. A polymer with Mn of 2800 g mol−1 and a molecular weight distribution of 1.41 was obtained (as determined by SEC), that contained double bonds introduced by the itaconic acid monomer units (6 mol-%, as determined by NMR). Crosslinking ability of the prepared copolymer was demonstrated in bulk by adding a thermal initiator and altering amounts of ethylene glycol dimethacrylate (EGDMA) crosslinking agent into molten polymer at 60–150 °C. A crosslinked gel was formed in less than 15 min at 80 °C when 10 wt.% of EGDMA was added and benzoyl peroxide (BPO) was used as the initiator. Aqueous dispersions were prepared of the non-crosslinked copolymer with a thermomechanical method that involved slow addition of aqueous polyvinyl alcohol (PVA) solution into molten copolymer at 60 °C under shear. Dispersions were prepared with 10 wt.% of EGDMA and 2 wt.% of BPO. Crosslinking of the dispersed microparticles was achieved by heating the dispersions at 80 °C for 30 or 60 min. The dispersions were characterized by SEM, DSC, TGA, FT-IR, solid state NMR, and gel content measurements. The effect of crosslinking was clearly seen in SEM images of films cast from the dispersions. The films cast from non-crosslinked dispersions had smooth morphology whereas in films cast from crosslinked dispersions separate spherical particles were observed. During the crosslinking reactions, glass transition temperatures increased (as determined by DSC), thermal stability of the samples increased (as determined by TGA), and the gel content of the samples increased.
    Original languageEnglish
    Pages (from-to)1495-1503
    JournalEuropean Polymer Journal
    Issue number8
    Publication statusPublished - 2012
    MoE publication typeA1 Journal article-refereed


    • Dispersion
    • crosslinking
    • polyester
    • biobased polymer
    • poly(lactic acid)


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