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Surface-Initiated Initiators for Continuous Activator Regeneration (SI ICAR) ATRP of MMA from 2,2,6,6–tetramethylpiperidine–1–oxy (TEMPO) Oxidized Cellulose Nanofibers for the Preparations of PMMA Nanocomposites

Industrial Technology Research Institute, No. 195, Sec. 4, Chung Hsing Road, Chutung, Hsinchu 31057, Taiwan
Hubei Key Laboratory of Polymer Materials, Key Laboratory for the Green Preparation and Application of Functional Materials (Ministry of Education), Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, School of Materials Science and Engineering, Hubei University, Wuhan 430062, China
Department of Chemical Engineering, Feng Chia University, 100 Wenhwa Road, Seatwen District, Taichung 40724, Taiwan
Department of Chemical Engineering, National Chung Hsing University, 145 Xingda Road, South District, Taichung 40227, Taiwan
Department of Materials and Optoelectronic Science, Center of Crystal Research, National Sun Yat-Sen University, Kaohsiung 80424, Taiwan
Department of Medicinal and Applied Chemistry, Kaohsiung Medical University, Kaohsiung 80708, Taiwan
Key Laboratory of Marine Materials and Related Technologies, Zhejiang Key Laboratory of Marine Materials and Protective Technologies, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China
Research Center for Sustainable Energy and Nanotechnology, National Chung Hsing University, Taichung 40227, Taiwan
Authors to whom correspondence should be addressed.
Polymers 2019, 11(10), 1631;
Received: 11 September 2019 / Revised: 7 October 2019 / Accepted: 8 October 2019 / Published: 9 October 2019
(This article belongs to the Special Issue Cellulose and Renewable Materials)
An effective method of oxidation from paper pulps via 2,2,6,6–tetramethylpiperidine–1–oxy (TEMPO) compound to obtain TEMPO-oxidized cellulose nanofibers (TOCNs) was demonstrated. Following by acylation, TOCN having an atom transfer radical polymerization (ATRP) initiating site of bromoisobutyryl moiety (i.e., TOCN–Br) was successfully obtained. Through a facile and practical technique of surface-initiated initiators for continuous activator regeneration atom transfer radical polymerization (SI ICAR ATRP) of methyl methacrylate (MMA) from TOCN–Br, controllable grafting polymer chain lengths (Mn = ca. 10k–30k g/mol) with low polydispersity (PDI < 1.2) can be achieved to afford TOCN–g–Poly(methyl methacrylate) (PMMA) nanomaterials. These modifications were monitored by Fourier-transform infrared spectroscopy (FT–IR), scanning electron microscopy (SEM), electron spectroscopy for chemical analysis (ESCA), and water contact angle analysis. Eventually, TOCN–g–PMMA/PMMA composites were prepared using the solvent blending method. Compared to the pristine PMMA (Tg = 100 °C; tensile strength (σT) = 17.1 MPa), the composites possessed high transparency with enhanced thermal properties and high tensile strength (Tg = 110 °C and σT = 37.2 MPa in 1 wt% TOCN containing case) that were investigated by ultraviolet-visible spectroscopy (UV-Vis), thermogravimetric analysis (TGA), dynamic mechanical analysis (DMA), and tensile tests. We demonstrated that minor amounts of TOCN–g–PMMA nanofillers can provide high efficacy in improving the mechanical and thermal properties of PMMA matrix. View Full-Text
Keywords: TOCN; SI ICAR ATRP; PMMA nanocomposites TOCN; SI ICAR ATRP; PMMA nanocomposites
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MDPI and ACS Style

Tu, C.-W.; Tsai, F.-C.; Chang, C.-J.; Yang, C.-H.; Kuo, S.-W.; Zhang, J.; Chen, T.; Huang, C.-F. Surface-Initiated Initiators for Continuous Activator Regeneration (SI ICAR) ATRP of MMA from 2,2,6,6–tetramethylpiperidine–1–oxy (TEMPO) Oxidized Cellulose Nanofibers for the Preparations of PMMA Nanocomposites. Polymers 2019, 11, 1631.

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