Size-controlled one-pot synthesis of viologen nanoparticles via a microwave heating technique
Size-controlled one-pot synthesis of viologen nanoparticles via a microwave heating technique
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DOI：
10.1038/s41428-021-00480-4
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发表时间：
2021-04
期刊：
影响因子：
2.8
通讯作者：
Ken Komoda;T. Kawauchi
中科院分区：
文献类型：
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作者：
Ken Komoda;T. Kawauchi
我们报告了一个大小控制的一锅合成氧化还原活性的有机纳米粒子组成的紫精单元通过精确的温度控制提供的使用微波加热。4，4 ′-联吡啶和1，3，5-三将对应于单体的（溴甲基）苯（TBMB）和对应于终止剂的溴乙烷在80 °C下进行微波加热20分钟作为对应于生长反应的第一阶段，然后在150 °C下加热5分钟作为对应于终止反应的第二阶段。步骤证实，在80 °C下，4，4 ′-联吡啶主要与TBMB反应，导致分子量增加，并且由于温度升高至150 °C，与溴乙烷发生终止反应。此外，可以通过改变第一阶段反应时间来控制纳米颗粒的尺寸;如通过动态光散射测量所证明的，对于10分钟的第一阶段反应时间，纳米颗粒直径被确定为142 ± 15 nm，其在20分钟时增加到269 ± 67 nm。
We report a size-controlled one-pot synthesis of redox-active organic nanoparticles consisting of viologen units via precise temperature control afforded by the use of microwave heating. A DMF solution of 4,4′-bipyridine and 1,3,5-tris(bromomethyl)benzene (TBMB) corresponding to monomers and ethyl bromide corresponding to a terminator was subjected to microwave heating at 80 °C for 20 min as the first stage corresponding to the growth reaction, which was then followed by heating at 150 °C for 5 min as the second stage corresponding to the termination reaction.1H NMR analysis of the reaction mixture at each step confirmed that at 80 °C, 4,4′-bipyridine primarily reacts with TBMB, leading to an increase in molecular weight and that a termination reaction with ethyl bromide occurs due to the increase in temperature to 150 °C. Moreover, the size of the nanoparticles can be controlled by varying the first stage reaction time; the nanoparticle diameter was determined to be 142 ± 15 nm for the first stage reaction time of 10 min, which increased to 269 ± 67 nm at 20 min, as evidenced by dynamic light scattering measurements.