Lipase-Catalyzed Copolymerization of Dialkyl Carbonate with 1,4-Butanediol and 蠅-Pentadecalactone: Synthesis of Poly(蠅-pentadecalactone-co-butylene-co-carbonate)

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• 作者：Zhaozhong Jiang
• 刊名：Biomacromolecules
• 出版年：2011
• 出版时间：May 9, 2011
• 年：2011
• 卷：12
• 期：5
• 页码：1912-1919
• 全文大小：876K
• 年卷期：v.12,no.5(May 9, 2011)
• ISSN：1526-4602

文摘

Candida antarctica lipase B (CALB) was successfully used to promote synthesis of aliphatic poly(carbonate-co-ester) copolymers from dialkyl carbonate, diol, and lactone monomers. The polymerization reactions were carried out in two stages: first-stage oligomerization under low vacuum, followed by second-stage polymerization under high vacuum. Therefore, copolymerization of 蠅-pentadecalactone (PDL), diethyl carbonate (DEC), and 1,4-butanediol (BD) yielded PDL-DEC-BD copolymers with a M_w of whole product (nonfractionated) up to 33鈥?00 and M_w/M_n between 1.2 and 2.3. Desirable reaction temperature for the copolymerization was found to be 80 掳C. The copolymer compositions, in the range from 10 to 80 mol % PDL unit content versus total (PDL + carbonate) units, were effectively controlled by adjusting the monomer feed ratio. Reprecipitation in chloroform/methanol mixture allowed isolation of the purified copolymers in up to 92% yield. ¹H and ¹³C NMR analyses, including statistical analysis on repeat unit sequence distribution, were used to determine the polymer microstructures. The synthesized PDL-DEC-BD copolymers possessed near random structures with all possible combinations of PDL, carbonate, and butylene units via either ester or carbonate linkages in the polymer chains and are more appropriately named as poly(PDL-co-butylene-co-carbonate).