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可降解两亲性共聚物
Poly-α,β-[N-(2-hydroxyethyl)-L-aspartamide]-g-poly(ε-caprolactone)的合成与表
征
程巳雪
武汉大学化学与分子科学学院，武汉，430072，中国
摘要
用亲水性聚氨基酸poly-α,β-[N-(2-hydroxyethyl)-L-aspartamide] （PHEA）上的羟基作为引发中心，引发环状单体ε-己内酯（ε-caprolactone，CL）的开环聚合，得到了两种不同分子量的两亲性接枝共聚物poly-α,β-[N-(2-hydroxyethyl)-L-aspartamide]-g-poly(ε-caprolactone) (PHEA-g-PCL)，并表征了它们的化学结构。
引言
两亲性可生物降解聚合物在水溶液中可能自组装形成纳米胶束。在生物医学等领域有着广泛的应用。1-3
本研究中用亲水性聚氨基酸poly-α,β-[N-(2-hydroxyethyl)-L-aspartamide] （PHEA）上的羟基作为引发中心，引发环状单体ε-己内酯（ε-caprolactone，CL）的开环聚合，得到了两亲性接枝共聚物PHEA-g-PCL，并表征了它们的化学结构。
实验部分
材料
ε-己内酯为Aldrich公司产品，使用前减压蒸馏纯化。
PHEA-g-PCL的合成
PHEA根据文献方法合成。4将一定比例的PHEA、CL加入硅烷化的聚合瓶中，抽真空封管后在200oC油浴中放置5分钟，然后在120oC油浴中反应48小时。反应结束后，产物用二氯甲烷溶解，用乙醚沉淀，过滤，真空干燥，得到共聚物PHEA-g-PCL。
PHEA-g-PCL的表征
共聚物用红外光谱（PerkinElmer-2）和1H核磁共振波谱（Mercury VX-300）表征结构，用尺寸排除色谱-多角度激光光散射联用（SEC-MALLS）（DAWN EOS, Wyatt Technology Co.）测定分子量。
结果与讨论
通过PHEA上的羟基引发环状单体CL的开环聚合、合成的接枝共聚物的化
学结构见图1。
图1. 接枝共聚物的化学结构
合成反应的投料比、聚合物的组成及分子量见表1。由于接枝反应时严格地控制无水条件，CL的开环聚合可以被PHEA上的羟基有效地引发，生成接枝共聚物。为了检测在加热条件下PHEA的稳定性，我们将PHEA样品在同聚合反应一样的温度下处理，得到PHEA-2，发现其分子量明显比处理前的样品（PHEA）低，这说明在聚合条件下，主链PHEA有一定程度的降解。即使这样，接枝共聚物的分子量仍然较高，说明接枝共聚反应的成功进行。
表1聚合物的组成、分子量及分子量分布
聚合物
投料比
-OH/CL
(mol/mol)
1H NMR SEC-MALLS
共聚物组成
HEA/CL
(mol/mol)
PHEA主链
上未反应的
-OH (%)
M w
(g/mol)
M w/M n
PHEA - - 100 2.56 x 104 1.49
PHEA-2 - - 100 3.21 x 103 1.17 Copolymer a1/4 1/4.88 55 1.73 x 104 1.17 Copolymer b1/10 1/15.67 45 2.16 x 104 1.10
1H NMR表征中，PHEA和PHEA-2的溶剂为D
2
O，Copolymer a 和Copolymer b 的溶剂为CDCl3。SEC-MALLS 测试时，PHEA和PHEA-2的溶剂为0.15 M NaCl/0.1M 磷酸缓冲溶液(pH 7.4) ，Copolymer a 和Copolymer b 的溶剂为CHCl3。
两亲性接枝共聚物的红外图谱见图2，从图中可见接枝共聚物在1725 cm-1出现PCL侧链上酯基C=O的伸缩振动；在1660 and 1543 cm-1出现PHEA主链上酰胺键的C=O的伸缩振动和N-H的弯曲振动，这些峰清楚地表明了接枝反应的成功进行。
图2 接枝共聚物和PHEA及PCL均聚物的FTIR图谱
两亲性接枝共聚物的核磁共振波谱中可以检测到以下来自主链PHEA和侧链PCL的核磁共振信号：PHEA: 2.61 ppm (CHC H2CONH), 3.14 ppm (NHC H2CH2OH), 3.44 ppm (CH2C H2OH), 4.50 ppm (NHC H(CO)CH2); PCL: 1.22 ppm (CH2CH2C H2CH2CH2), 1.46 ppm (CH2C H2CH2C H2CH2), 2.24 ppm (COC H2), 3.96 ppm (C H2O)。此外，还有两个新信号出现在3.32 ppm (C H2CH2OCO)和4.02 ppm (CH2C H2OCO)，这进一步验证了接枝聚合物的结构。
结论
主链为PHEA、侧链为PCL链段的新型两亲性接枝共聚物被成功合成。
致谢感谢国家自然科学基金委的资助（项目号：20474046）。
参考文献
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大学英语专业英语写作 试卷 HUA system office room 【HUA16H-TTMS2A-HUAS8Q8-HUAH1688】
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化学专业-英语单词
Chemistry Summer Holidays Homework for Future Freshmen of High school Class: __________________________ Chinese Name:______________________ English Name:______________________
Beijing#80 High School International Department
Introduction to Chemistry 化学入门 Definition: Chemistry is the study of the composition, structure, and properties of matter, the processes that matter undergoes, and the energy changes that accompany there processes. (化学的定义：化学是研究物质的组成，结构，性质，物质发生的变化，以及变化过程中涉及的能量变化。) Branches of Chemistry: Organic Chemistry；Inorganic Chemistry；Physical Chemistry; Analytical Chemistry; Biochemistry; Theoretical chemistry (化学的分支：有机化学；无机化学；物理化学；分析化学；生物化学；理论化学)
Day 1 【Task】Please put the Chinese name into the suitable chapter. Vocabulary about chapter name. 章节名称词汇 （----What may we study about chemistry in the first year? 高一可能涉及哪些化学知识？） 物质和变化；原子：构建物质的基本单元；酸和碱；氧化还原反应；气体； 化学键；原子中的电子排布；称量和计算；有机化学；反应能量；元素周期律；化学方程式和化学反应；化学平衡；化学反应动力学；化学计量学； 化学式和化学物质；物质的状态；生物化学；电化学；滴定与pH值； 水溶液中离子和稀溶液的依数性；溶液； Chapter 1 Matter and Change ( ) Chapter 2 Measurement and Calculation ( ) Chapter 3 Atom-Building Block of Matter ( ) Chapter 4 Arrangement of Electrons in Atoms( ) Chapter 5 The periodic Law ( ) Chapter 6 Chemical Bonding ( ) Chapter 7 Chemical Formulas and Chemical Compounds ( ) Chapter 8 Chemical Equations and Reactions ( ) Chapter 9 Stoichiometry ( ) Chapter 10 States of Matter ( ) Chapter 11 Gas ( ) Chapter 12 Solution ( ) Chapter 13 ions in Aqueous Solution and colligative Properties ( ) Chapter 14 Acid and Base ( ) Chapter 15 Acid-Base Titration and pH ( ) Chapter 16 Reaction Energy ( ) Chapter 17 Reaction Kinetics ( ) Chapter 18 Chemical Equilibrium ( ) Chapter 19 Oxidation-Reduction Reactions ( ) Chapter 20 Electrochemistry ( ) Chapter 22 Organic Chemistry ( ) Chapter 23 Biology Chemistry ( )