S.A. Direction Centrale des Recherches, Laboratoire Central, 31 0 rue de Ransbeek, B-1 120 Bruxelles, Belgium SYNOPSIS This work deals with the molecular characterization of maleic anhydride melt-functionalized polypropylene ( PP-g-MA). The functionalization mechanism, the nature, the concentration, and the location of grafted anhydride species onto the polypropylene chain are discussed. The polypropylene functionalization was performed using a pre-heated Brabender Plastograph ( 190°C, 4 min of mixing time). Several concentrations of maleic anhydride and organic peroxide were used for this study. In those experimental conditions, the organic peroxide undergoes an homolytic rupture and carries out a polypropylene tertiary hydrogen abstraction. The resulting macroradical undergoes a 0-scission leading to a radical chain end which reacts with maleic anhydride. When a termination reaction occurs at this first step a succinic type anhydride chain end is obtained. However, oligomerization of maleic anhydride is found to occur more frequently leading to poly( maleic anhydride) chain end. Concentration of both anhydride types and minimal length of the grafted poly (maleic anhydride) were determined. A fraction of maleic anhydride does not react with polypropylene or homopolymerize leading to nongrafted poly (maleic anhydride). 0 1995 John Wiley & Sons, Inc.

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Poly(lactic acid) (PLA)/halloysite nanotubes (HNT) nanocomposites were prepared by melt extrusion using a masterbatch dilution process. Effect of addition of both unmodified halloysites (HNT) and quaternary ammonium salt treated halloysites (m-HNT) was investigated at different nanofiller contents. A homogeneous distribution/dispersion of halloysites in the PLA matrix is obtained for both unmodified and modified nanotubes within the studied composition range. The nucleating effect of halloysites, resulting in a limited increase of degree of crystallinity, is more pronounced in the case of m-HNT. Besides, the rigidity, tensile, flexural, and impact resistances of PLA significantly increase on addition of halloysites, the property improvement being higher for m-HNT than for HNT. Interestingly, there is no significant embrittlement (almost constant elongation at break). Based on micromechanical models, this superior reinforcement efficiency of m-HNT was ascribed to the better interfacial compatibility induced by the modification of the nanotube surface.

SYNOPSISA set of anhydride-grafted polypropylenes was collected from various companies. They were studied in light of our recent results on polypropylene melt grafted with maleic anhydride.' This work confirmed that an important decrease of the anhydride content is recorded on heating or washing, due to the elimination of free, ungrafted products, respectively, by sublimation of maleic anhydride and by polymaleic anhydride solubilization. The deconvolution of the infrared spectra of washed anhydride-grafted polypropylenes (PP-g-MA) revealed two types of grafted anhydride: succinic anhydride form and polymaleic anhydride form. All in all, four forms of anhydride functions were detected two grafted and two free, each being either on monomeric or polymeric forms. Nevertheless, one PPg-MA (Hercoprime) can be distinguished by its very high grafting level. This polymer is therefore discussed in more detail. Finally, all the present results are discussed with regard to the principal applications of the PP-g-MA as a blend compatiblizer or as an adhesion promoter.

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