This paper reports the synthesis of cellulose nanocrystals grafted by polystyrene chains via surface-initiated ATRP. Naturally occurring cellulose was first hydrolyzed to obtain cellulose nanocrystals. Their surface was then chemically modified using 2-bromoisobutyryl bromide to introduce initiating sites for ATRP. A varying extent of surface modification was achieved by changing reaction conditions. Further initiation of styrene polymerization from these modified nanocrystals with a CuBr/PMDETA (N,N,N',N',N''-pentamethyldiethylenetriamine) catalytic system and in the presence of a sacrificial initiator produced polysaccharide nanocrystals grafted by polystyrene chains. A range of nanocrystals-g-polystyrene with different graft lengths (theoretical polymerization degree = 27-171) was synthesized through this method and characterized by elemental analysis, XPS, FT-IR, TEM, and contact angle measurements. We are thus able to produce cellulose nanoparticles with varying grafting densities (by altering extent of initiator surface modification) and varying polymer brush length (through polymerization control). The nanocrystals-g-polystyrene (NC-g-PS) particles were tested for their capacity to absorb 1,2,4-trichlorobenzene from water. The results obtained show that they can absorb the equivalent of 50% of their weight in pollutant compared to 30 wt % adsorption for nonmodified nanocrystals, while also displaying faster absorption kinetics.

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Chitin nanowhiskers are structured into mesoporous aerogels by using the same benign process used previously in our group to make cellulose nanowhisker aerogels. The nanowhiskers are sonicated in water to form a hydrogel before solvent-exchange with ethanol and drying under supercritical CO2 (scCO2). Aerogels are prepared with various densities and porosities, relating directly to the initial chitin nanowhisker content. scCO2 drying enables the mesoporous network structure to be retained as well as allowing the gel to retain its initial dimensions. The chitin aerogels have low densities (0.043–0.113 g cm−3), high porosities (up to 97 %), surface areas of up to 261 m2 g−1, and mechanical properties at the high end of other reported values (modulus between 7 and 9.3 MPa). The aerogels were further characterized by using X-ray diffraction, BET analysis, electron microscopy, FTIR, and thermogravimetric analysis. Characterization showed that the rod-like crystalline nature of the nanowhiskers was retained during the aerogel production process, making the aerogel truly an assembled structure of chitin nanocrystals. These aerogels also showed the lowest reported shrinkage during drying to date, with an average shrinkage of only 4 %.

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