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RAFT-mediated Pickering emulsion polymerization with cellulose nanocrystals grafted with random copolymer as stabilizer.

ABSTRACT: The synthesis of a RAFT-mediated Pickering emulsion was firstly achieved by using cellulose nanocrystals (CNCs) grafted with a random copolymer as the stabilizer. Firstly, poly(acrylonitrile-r-butyl acrylate) (poly(AN-r-nBA)) was synthesized by Cu(0)-mediated CRP, which was further modified via a click chemistry strategy to obtain poly(ethylene tetrazole-r-butyl acrylate) (poly(VT-r-nBA)). Then, poly(VT-r-nBA) was grafted onto the CNCs through a Mitsunobu reaction to obtain poly(VT-r-nBA)-g-CNCs. Stabilized by poly(VT-r-nBA)-g-CNCs, an O/W RAFT-mediated Pickering emulsion was formed for the preparation of well-controlled poly(methyl methacrylate) (PMMA) particles with water-soluble potassium persulfate (KPS) as an initiator and oil-soluble 4-cyanopentanoic acid dithiobenzoate (CPADB) as a chain transfer agent. Rheological analysis suggested that the prepared Pickering emulsion possessed good stability under the influences of changes in strain, time, frequency and temperature. Furthermore, the recycling and further utilization of the poly(VT-r-nBA)-g-CNCs could be simply realized through centrifugal separation.

SUBMITTER: Bai L

PROVIDER: S-EPMC9084400 | biostudies-literature | 2018 Aug

REPOSITORIES: biostudies-literature

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RAFT-mediated Pickering emulsion polymerization with cellulose nanocrystals grafted with random copolymer as stabilizer.

Bai Liangjiu L Jiang Xinyan X Liu Beifang B Wang Wenxiang W Chen Hou H Xue Zhongxin Z Niu Yuzhong Y Yang Huawei H Wei Donglei D

RSC advances 20180813 50

The synthesis of a RAFT-mediated Pickering emulsion was firstly achieved by using cellulose nanocrystals (CNCs) grafted with a random copolymer as the stabilizer. Firstly, poly(acrylonitrile-r-butyl acrylate) (poly(AN-r-nBA)) was synthesized by Cu(0)-mediated CRP, which was further modified via a click chemistry strategy to obtain poly(ethylene tetrazole-r-butyl acrylate) (poly(VT-r-nBA)). Then, poly(VT-r-nBA) was grafted onto the CNCs through a Mitsunob ...[more]

PMID: 35548399

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Project description:Incorporating unmodified silica nanoparticles onto polymer latexes to fabricate aqueous polymer dispersions without relying on electrostatic attraction during the Pickering emulsion polymerization process still faces challenges. For negatively charged silica nanoparticles to successfully adsorb onto polymer latexes, particularly in an anionic initiator emulsion polymerization system, they have remained elusive without the use of auxiliary monomers and cationic initiators. This study investigates various experimental parameters, such as emulsion polymerization temperature, monomer solubility, salt concentration, and cation type, to elucidate the factors influencing the adsorption of unmodified silica nanoparticles in Pickering emulsion polymerization. While poly(methyl methacrylate) (PMMA)/SiO2 hybrid latexes can be obtained under pH conditions of 5-6 and at temperatures of 65 °C or below, the loading rate of silica nanoparticles decreases as the reaction temperature increases, resulting in bare PMMA latexes without silica nanoparticle adsorption at temperatures exceeding 70 °C. Introducing styrene (St) into the monomer mixture with methyl methacrylate in a ratio of up to 10 wt % leads to a gradual decrease in silica nanoparticle loading rate, from 27.3 to 8.2 wt %, attributed to the low solubility of St in water. Furthermore, the presence of sodium ions (Na+) is found to be crucial for silica nanoparticle adsorption onto PMMA latexes, as the sodium ions have a stabilizing effect on both the silica nanoparticles and the silica nanoparticle-armored latexes. These findings highlight the complex nature of Pickering emulsion polymerization in the presence of unmodified silica nanoparticles, demonstrating that the loading rate of silica nanoparticles onto polymer latexes is influenced by various factors. These insights pave the way for developing aqueous polymer dispersions with high silica nanoparticle loading rates onto polymer latexes, which is a desirable trait in the coating industry.

Project description:A poly(2-(dimethylamino)ethyl methacrylate) (PDMA) chain transfer agent (CTA) is used for the reversible addition-fragmentation chain transfer (RAFT) alcoholic dispersion polymerization of benzyl methacrylate (BzMA) in ethanol at 70 °C. THF GPC analysis indicated a well-controlled polymerization with molecular weight increasing linearly with conversion. GPC traces also showed high blocking efficiency with no homopolymer contamination apparent and Mw/Mn values below 1.35 in all cases. 1H NMR studies confirmed greater than 98% BzMA conversion for a target PBzMA degree of polymerization (DP) of up to 600. The PBzMA block becomes insoluble as it grows, leading to the in situ formation of sterically stabilized diblock copolymer nanoparticles via polymerization-induced self-assembly (PISA). Fixing the mean DP of the PDMA stabilizer block at 94 units and systematically varying the DP of the PBzMA block enabled a series of spherical nanoparticles of tunable diameter to be obtained. These nanoparticles were characterized by TEM, DLS, MALLS, and SAXS, with mean diameters ranging from 35 to 100 nm. The latter technique was particularly informative: data fits to a spherical micelle model enabled calculation of the core diameter, surface area occupied per copolymer chain, and the mean aggregation number (Nagg). The scaling exponent derived from a double-logarithmic plot of core diameter vs PBzMA DP suggests that the conformation of the PBzMA chains is intermediate between the collapsed and fully extended state. This is in good agreement with 1H NMR studies, which suggest that only 5-13% of the BzMA residues of the core-forming chains are solvated. The Nagg values calculated from SAXS and MALLS are in good agreement and scale approximately linearly with PBzMA DP. This suggests that spherical micelles grow in size not only as a result of the increase in copolymer molecular weight during the PISA synthesis but also by exchange of individual copolymer chains between micelles and/or by sphere-sphere fusion events.

Dataset Information

RAFT-mediated Pickering emulsion polymerization with cellulose nanocrystals grafted with random copolymer as stabilizer.

Publications

RAFT-mediated Pickering emulsion polymerization with cellulose nanocrystals grafted with random copolymer as stabilizer.

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