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Method for determining optimal degree of vulcanization and optimal content of constituent ingredient of composition for vulcanization in real time by impedance measurement and analysis

机译:通过阻抗测量和分析实时确定最佳硫化程度和最佳硫化组合物成分含量的方法

摘要

The present invention relates to a method for evaluating the crosslink degree of a vulcanized sample in real time during a vulcanization process or diagnosing the electrical properties of the sample after the completion of the vulcanization process, and then determining an optimal vulcanization time and an optimal content of each constituent gradient of a composition for vulcanization that optimize the properties of the composition according to the vulcanization conditions, for the sake of improving the properties of the vulcanized sample prepared from a polymer by vulcanization at a high temperature.;The method for determining an optimal vulcanization time and an optimal content of each constituent gradient of a composition for vulcanization that optimize the properties of the composition according to the vulcanization conditions includes: (a) measuring an impedance spectrum in a specific frequency range in the individual vulcanization condition; (b) approximating the measured impedance spectrum to an equivalent circuit model consisting of resistance and capacitance components; (c) determining a polymer resistance Rp (i.e., a value obtained by subtracting a real part of the impedance measurement at a maximum frequency from a real part of the impedance measurement at a minimum frequency, or the magnitude of a real part of the semicircle in a Nyquist diagram) from the determined parameters; (d) determining, as an optimal end point of vulcanization, a time point at which the increasing rate of the polymer resistance Rp rapidly slows down; and (e) determining the optimal content of each constituent ingredient of the composition for vulcanization when the polymer resistance Rp of the sample completely vulcanized is at its minimum.
机译:本发明涉及一种在硫化过程中实时评估硫化样品的交联度或在硫化过程完成后诊断样品的电性能,然后确定最佳硫化时间和最佳含量的方法。为了改善在高温下通过硫化由聚合物制备的硫化样品的性能,根据硫化条件优化组合物性能的硫化组合物的每个组成梯度的组成;根据硫化条件优化组合物性能的最佳硫化时间和用于硫化的组合物的每个组成梯度的最佳含量包括:(a)在各个硫化条件下在特定频率范围内测量阻抗谱; (b)将测得的阻抗谱近似为一个由电阻和电容成分组成的等效电路模型; (c)确定聚合物电阻Rp(即,通过从最小频率的阻抗测量的实部减去最大频率的阻抗测量的实部或半圆的实部的大小而得到的值在奈奎斯特图中)根据确定的参数; (d)确定作为最佳的硫化终点的聚合物电阻Rp的增加速度迅速减慢的时间点; (e)当完全硫化的样品的聚合物电阻Rp为最小时,确定用于硫化的组合物的每种组成成分的最佳含量。

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