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Synthesis of sugar‐based macromolecules via sono‐ATRP in miniemulsion
Polymers for Advanced Technologies ( IF 3.4 ) Pub Date : 2020-04-12 , DOI: 10.1002/pat.4921
Izabela Zaborniak 1 , Karolina Surmacz 2 , Paweł Chmielarz 1
Affiliation  

Ultrasound‐mediated atom transfer radical polymerization (sono‐ATRP) in miniemulsion media is used for the first time for the preparation of complex macromolecular architectures by a facile two‐step synthetic route. Initially, esterification reaction of sucrose or lactulose with α‐bromoisobutyryl bromide (BriBBr) is conducted to receive multifunctional ATRP macroinitiators with 8 initiation sites, followed by polymerization of n‐butyl acrylate (BA) forming arms of the star‐like polymers. The brominated lactulose‐based molecule was examined as an ATRP initiator by determining the activation rate constant (ka) of the catalytic process in the presence of a copper(II) bromide/tris(2‐pyridylmethyl)amine (CuIIBr2/TPMA) catalyst in both organic solvent and for the first time in miniemulsion media, resulting in ka = (1.03 ± 0.01) × 104 M−1 s−1 and ka = (1.16 ± 0.56) × 103 M−1 s−1, respectively. Star‐like macromolecules with a sucrose or lactulose core and poly(n‐butyl acrylate) (PBA) arms were successfully received using different catalyst concentration. Linear kinetics and a well‐defined structure of synthesized polymers reflected by narrow molecular weight distribution (Mw/Mn = 1.46) indicated 105 ppm wt of catalyst loading as concentration to maintain controlled manner of polymerization process. 1H NMR analysis confirms the formation of new sugar‐inspired star‐shaped polymers.

中文翻译:

通过细乳液通过声纳-ATRP合成糖基大分子

在细乳液介质中,超声介导的原子转移自由基聚合(sono-ATRP)首次用于通过简便的两步合成路线制备复杂的大分子结构。最初,进行蔗糖或乳果糖与α-溴代异丁酰溴(BriBBr)的酯化反应,以接收具有8个引发位点的多功能ATRP大分子引发剂,然后聚合丙烯酸丁酯(BA)形成星形聚合物的臂。在溴化铜(II)/三(2-吡啶基甲基)胺(Cu II Br 2)存在下,通过确定催化过程的活化速率常数(k a),检查了溴化乳果糖基分子是否作为ATRP引发剂/ TPMA)催化剂在两种有机溶剂和在细乳液介质的第一时间,导致ķ一个=(1.03±0.01)×10 4中号-1小号-1ķ一个=(1.16±0.56)×10 3中号- 1 s -1。使用不同的催化剂浓度成功地获得了具有蔗糖或乳果糖核和聚丙烯酸丁酯(PBA)臂的星形大分子。窄分子量分布(M w / M n)反映了合成聚合物的线性动力学和结构明确的结构= 1.46)表示105ppm wt的催化剂负载量作为维持聚合过程受控方式的浓度。1 H NMR分析证实了新的糖型星形聚合物的形成。
更新日期:2020-04-12
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