Feasibility Study on Continuous Flow Controlled/Living Anionic Polymerization Processes

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• 作者：Aiichiro Nagaki ; Yuichi Nakahara ; Mai Furusawa ; Tomoya Sawaki ; Tetsuya Yamamoto ; Hideaki Toukairin ; Shinsuke Tadokoro ; Toshiya Shimazaki ; Toshihide Ito ; Masakazu Otake ; Hidenori Arai ; Naoya Toda ; Keita Ohtsuka ; Yusuke Takahashi ; Yuya Moriwaki ; Yuta Tsuchihashi ; Katsuyuki Hirose ; Jun-ichi Yoshida
• 刊名：Organic Process Research & Development
• 出版年：2016
• 出版时间：July 15, 2016
• 年：2016
• 卷：20
• 期：7
• 页码：1377-1382
• 全文大小：401K
• 年卷期：0
• ISSN：1520-586X

文摘

A practical microchemical reaction system for keeping process flow at defined conditions, which is one of the key issues of industrial production, was developed. Controlled/living anionic polymerization was chosen as a test reaction because the molecular weight and molecular weight distribution of polymer products are quite sensitive to the relative flow rate of an initiator solution and that of a monomer solution. The polymerization of styrene in THF/hexane was carried out using a flow microreactor system consisting of two T-shaped micromixers and two microtube reactors using Smoothflow pumps at 0 °C. Poly(styrene) with higher molecular weight such as Mn > 10000 could be synthesized using s-BuLi (Mn = 14 000, M_w/M_n = 1.11). n-BuLi could also be used as an initiator. The continuous operation was performed for 3 h without any problems to obtain ca. 1 kg of the polymer, indicating the feasibility of continuous flow processes for controlled/living anionic polymerization on a relatively large scale.