Telechelic dithiol copolymers as tunable building blocks for synthesizing multiblock materials
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A new strategy is reported to access α,Ïâdithiol polymer building blocks with tunable molecular weights and compositions for the preparation of random multiblock copolymers based on styrenic, acrylic, and siloxanes. This facile synthetic approach provides access to dithiols through a twoâstep process: (1) an initial copolymerization of vinyl monomers with ethyl lipoate followed by (2) disulfide bond reduction, producing dithiol terminated polymer products. Thiolâterminated polymers are easily prepared over a wide range of molecular weights (2â32âkDa) by simply controlling the feed ratio of vinyl monomer to ethyl lipoate. Mixtures of these linear dithiolâterminated building blocks were repolymerized via oxidative coupling to create random multiblock copolymers with high molecular weights (68â95âkDa) and controlled degradability. In summary, this approach for preparing and recombining telechelic dithiol polymers creates opportunities to manipulate the mechanical and physical properties of..., Characterization methods
1H nuclear magnetic resonance (NMR) spectroscopy
 1H-NMR spectra were collected on a Bruker Avance NEO 500 MHz at 25 °C using chloroform-d as a deuterated solvent.
Size-exclusion chromatography (SEC) instrumentation
Size-exclusion chromatography (SEC) was performed on a Waters instrument using a differential refractive index detector and two Tosoh columns (TSKgel SuperHZM-N, 3 μm polymer, 150 à 4.6 mm) with THF at 35 °C or chloroform containing 0.25% TEA at 35 °C for the mobile phase. Molar mass and molar mass dispersities (Ä) were determined against narrow PS standards (Agilent).
Differential scanning calorimetry (DSC)
DSC was performed on a TA Instruments Q2000 DSC with three repeated cycles between â150 and +150 °C at a constant rate of 10 °C/min. Only the second heating scan is shown.
Small-angle X-ray scattering (SAXS)
SAXS measurements were performed on a custom-built SAXS diffractometer housed at the University of California, Santa Barbara. The sample-to-..., , # Title of Dataset: Telechelic dithiol copolymers as tunable building blocks for synthesizing multiblock materials
This deposit includes the data necessary to reproduce all figures in the associated manuscript, except for figures that consist of pictures or illustrations.
Data is acquired from the following analytical characterization techniques:
Characterization methods
1H nuclear magnetic resonance (NMR) spectroscopy
1H-NMR spectra were collected on a Bruker Avance NEO 500 MHz at 25 °C using chloroform-d as a deuterated solvent.
Size-exclusion chromatography (SEC) instrumentation
Size-exclusion chromatography (SEC) was performed on a Waters instrument using a differential refractive index detector and two Tosoh columns (TSKgel SuperHZM-N, 3 μm polymer, 150 à 4.6 mm) with THF at 35 °C or chloroform containing 0.25% TEA at 35 °C for the mobile phase. Molar mass and molar mass dispersities (Ä) were determined against narrow PS standards (Agilent).
Differential scanning calorimet...
本研究报道了一种全新策略,用于制备α,ω-二硫醇聚合物结构单元,该单元可调控分子量与组成,用于制备基于苯乙烯类、丙烯酸类及硅氧烷类单体的无规多嵌段共聚物。该简便合成策略通过两步反应制备二硫醇化合物:(1) 乙烯基单体与硫辛酸乙酯的初始共聚反应,(2) 二硫键还原反应,最终得到端基为巯基的聚合物产物。只需调控乙烯基单体与硫辛酸乙酯的投料比,即可在2~32 kDa的宽分子量范围内便捷制备巯基封端聚合物。将这类线性二硫醇封端结构单元的混合物通过氧化偶联进行再聚合,可得到分子量达68~95 kDa且可控制降解的无规多嵌段共聚物。综上,这种遥爪二硫醇聚合物的制备与重组策略,为调控...的力学与物理性能提供了可能。
表征方法
1. 氢核磁共振(¹H nuclear magnetic resonance, ¹H NMR)光谱
¹H-NMR光谱测试在25 ℃下于Bruker Avance NEO 500 MHz核磁共振仪上完成,以氘代氯仿(chloroform-d)作为氘代溶剂。
尺寸排阻色谱(Size-exclusion chromatography, SEC)设备
尺寸排阻色谱测试采用Waters公司仪器,搭配示差折光检测器与两根Tosoh色谱柱(TSKgel SuperHZM-N,3 μm聚合物填料,150 × 4.6 mm),流动相为35 ℃下的四氢呋喃(THF),或35 ℃下含0.25%三乙胺(TEA)的氯仿溶液。以窄分布聚苯乙烯(PS)标准品(Agilent)为参比,测定聚合物的摩尔质量及其分布宽度(Đ)。
差示扫描量热法(Differential scanning calorimetry, DSC)
差示扫描量热测试在TA Instruments Q2000型差示扫描量热仪上完成,在-150 ℃至+150 ℃范围内以10 ℃/min的速率进行三次循环升温/降温,仅展示第二次升温扫描结果。
小角X射线散射(Small-angle X-ray scattering, SAXS)
小角X射线散射测试在加州大学圣巴巴拉分校定制的SAXS衍射仪上完成。样品到探测器的距离...
# 数据集标题:遥爪二硫醇共聚物作为可调谐结构单元用于多嵌段材料合成
本数据集包含复现相关论文中所有图表所需的实验数据(图片类插图图表除外)。
实验数据来源于以下分析表征技术:
表征方法
1. 氢核磁共振光谱
¹H-NMR光谱测试在25 ℃下于Bruker Avance NEO 500 MHz核磁共振仪上完成,以氘代氯仿作为氘代溶剂。
尺寸排阻色谱设备
尺寸排阻色谱测试采用Waters公司仪器,搭配示差折光检测器与两根Tosoh色谱柱(TSKgel SuperHZM-N,3 μm聚合物填料,150 × 4.6 mm),流动相为35 ℃下的四氢呋喃,或35 ℃下含0.25%三乙胺的氯仿溶液。以窄分布聚苯乙烯标准品(Agilent)为参比,测定聚合物的摩尔质量及其分布宽度。
差示扫描量热法...
创建时间:
2024-12-12



