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
    1.
    发明授权
    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 失效
    通过阻抗测量和分析实时确定硫化最佳硫化度和组成成分组成成分最佳含量的方法

    公开(公告)号:US06924652B2

    公开(公告)日:2005-08-02

    申请号:US10322903

    申请日:2002-12-18

    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.

    摘要翻译: 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工艺完成后对样品的电性能进行诊断的方法,然后确定最佳硫化时间和最佳含量 的硫化用组合物的各组成梯度,以便通过硫化在高温下提高由聚合物制备的硫化试样的性能,从而优化硫化条件下组合物的性能。 用于确定根据硫化条件优化组合物的性能的用于硫化的组合物的最佳硫化时间和每种组成梯度的最佳含量的方法包括:(a)测量个体中特定频率范围内的阻抗谱 硫化条件; (b)将测量的阻抗谱近似为由电阻和电容分量组成的等效电路模型; (c)确定聚合物电阻Rp(即,以最小频率从阻抗测量的实部减去最大频率处的阻抗测量的实部或半圆的实部的大小获得的值 在奈奎斯特图中)从确定的参数; (d)确定硫化的最佳终点为聚合物电阻Rp的增加速度迅速减慢的时间点; 和(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。