Synthesis of High Molecular Weight Nylon 46 in Supercritical Carbon Dioxide
Synthesis of High Molecular Weight Nylon 46 in Supercritical Carbon Dioxide
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超临界二氧化碳中合成高分子量尼龙 46
DOI：
10.1021/ma102696y
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发表时间：
2011-01
期刊：
影响因子：
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通讯作者：
张子勇
中科院分区：
文献类型：
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作者：
张子勇
以1，4-丁二胺和1，6-己二酸的盐为单体，在超临界二氧化碳（sc-CO2）中，采用一步法三步聚合法成功合成了高分子量尼龙46。聚合过程分为三个反应阶段：预缩合，后缩合，和真空。为了制备高分子量尼龙46，先将pH大于7.23的盐在190 °C、30 MPa下预缩合2 h。然后沿着除去副产物水而排出反应器中的CO2，并用干燥液体CO2再填充反应器。随后，将形成的预聚物在280 °C下在15 MPa下进行后缩合3小时。最后，将反应器在真空中在270 - 280 °C下加热30 - 45 min。由上述方法合成的尼龙46样品的最高粘均分子量为48 200 g/mol。用傅里叶变换红外光谱（FTIR）对尼龙46的化学结构和热性能进行了表征。
Nylon 46 with high molecular weight was successfully synthesized in supercritical carbon dioxide (sc-CO2) by one-step three-stage polymerization using the salt prepared from 1,4-diaminobutane and 1,6-adipic acid as a monomer. The polymerization process was divided into three reaction stages: precondensation, postcondensation, and vacuum. To prepare high molecular weight nylon 46, the precondensation of the salts with pH over 7.23 was first carried out at 190 °C under 30 MPa for 2 h. Then CO2 in the reactor was exhausted along with removing byproduct water, and the reactor was refilled with dry liquid CO2. Subsequently, the prepolymer formed was subjected to the postcondensation at 280 °C for 3 h under 15 MPa. Finally, the reactor was heated in vacuum at 270−280 °C for 30−45 min. The highest viscosity-average molecular weight of the nylon 46 sample synthesized from the above process is 48 200 g/mol. The chemical structure and thermal properties of the nylon 46 were characterized by Fourier transform infrar...