摘要
CO2以其独特性质在聚合物加工中得到广泛应用。简单改变CO2温度和压力可调节CO2与聚合物间的相互作用,影响聚合物的物理化学性质,使聚合物晶型转变和结晶过程发生变化,进而达到对聚合物晶型结构的调控。等规聚丁烯-1是一种性能优异的多晶态半结晶聚合物,复杂的晶型转变严重限制了等规聚丁烯-1的广泛应用和发展,对等规聚丁烯-1晶型结构调控一直是研究热点。应用CO2调控等规聚丁烯-1晶型结构,提供了一种解决等规聚丁烯-1复杂晶型转变的新方法。本文首次对CO2环境中等规聚丁烯-1晶型转变和结晶行为进行了系统研究。
首先,研究了CO2诱导等规聚丁烯-1晶型Ⅱ向晶型Ⅰ转变过程。结果表明,晶型Ⅱ在5 MPa C02中升温熔融过程中即能全部转变为晶型Ⅰ,CO2可显著促进晶型Ⅱ向晶型Ⅰ转变。晶型转变前后等规聚丁烯-1结晶度未发生明显改变,表明晶型Ⅱ向晶型Ⅰ转变只发生在晶区。通过高压原位红外光谱研究了不同CO2温度和压力时等规聚丁烯-1晶型Ⅱ向晶型Ⅰ转变动力学,发现晶型转变速率随CO2温度的增加而降低,随CO2压力的增加而增加。控制晶型Ⅱ向晶型Ⅰ转变在低温高压CO2中进行,能够使晶型转变过程在几分钟内完成,是迄今报道的促进晶型Ⅱ向晶型Ⅰ转变最有效的方法。
然后,研究了CO2诱导等规聚丁烯-1晶型Ⅲ转变过程。结果表明,CO2可促进更多的晶型Ⅲ转变为晶型Ⅰ',也可促进晶型Ⅲ向晶型Ⅰ'转变在较低温度下进行。晶型Ⅲ向晶型Ⅰ'转变及晶型Ⅰ'的完善,能降低晶型Ⅲ和晶型Ⅰ'的熔融自由能垒,抑制熔融过程中晶型Ⅱ形成,使晶型Ⅲ和晶型Ⅰ'直接熔融。通过高压原位红外光谱定量研究了等规聚丁烯-1晶型Ⅲ向晶型Ⅰ'转变动力学,发现晶型Ⅲ向晶型Ⅰ'转变可能包括转变初期的瞬间成核和后期的二次随机成核两个过程,绝大多数晶型Ⅲ通过第一个过程转变为晶型Ⅰ'。CO2同时也改变晶型Ⅲ退火过程中晶型Ⅱ的形成过程,由常压N2中的“固态-固态”转变过程改变为CO2中“熔融-重结晶”过程。利用偏光显微镜研究了晶型Ⅲ转变过程对球晶形貌的影响,晶型Ⅲ向晶型Ⅰ'的“固态-固态”转变过程不影响等规聚丁烯-1球晶中片晶取向,而CO2中晶型Ⅲ向晶型Ⅱ的形成过程改变等规聚丁烯-1球晶中片晶取向。
第三,研究了CO2中等规聚丁烯-1晶型Ⅲ升温过程中的晶型Ⅱ重结晶行为,发现晶型Ⅲ熔融过程中向晶型Ⅱ的转变由两个过程组成：“固态-固态”转变过程和“熔融-重结晶”过程。CO2压力的增加明显抑制“固态-固态”转变过程,使通过“熔融-重结晶”过程形成晶型Ⅱ的相对含量逐渐升高。将非等温结晶动力学计算应用于晶型Ⅲ升温中晶型Ⅱ重结晶过程时,发现非等温结晶动力学参数Kc在3 MPa C02时明显减小,表明非等温结晶机理改变。高压原位红外光谱对等规聚丁烯-1晶型Ⅱ熔融过程的进一步研究证实晶型Ⅲ在3 MPa C02中熔融时重结晶机理确实已变化,晶型Ⅱ全部通过“熔融-重结晶”过程形成。晶型Ⅲ在4 MPa CO2中熔融时,晶型Ⅱ结晶峰和熔融峰消失是由CO2对晶型Ⅱ的强塑化作用引起。
第四,研究了CO2中熔融态等规聚丁烯-1非等温结晶行为。等规聚丁烯-1非等温结晶峰温度随CO2压力的增加线性下降。等规聚丁烯-1在0.5-8 MPa CO2中结晶为晶型Ⅱ,在10 MPa CO2以上结晶为晶型Ⅰ'。发现一种新的熔融态等规聚丁烯-1结晶为晶型Ⅰ'的非等温结晶过程。定量研究了CO2中熔融态等规聚丁烯-1非等温结晶动力学,发现Avrami指数随CO2压力的增加而减小,表明结晶过程逐渐改变。高压原位红外光谱对等规聚丁烯-1非等温结晶过程的研究证实等规聚丁烯-1在10-18 MPa CO2中由熔融态结晶为晶型Ⅰ'。偏光显微镜直接观察到了等规聚丁烯-1非等温结晶过程及机理随C02压力变化的过程。
最后,研究了CO2发泡等规聚丁烯-1过程中晶型结构的变化。通过高压差式扫描量热仪确定了晶型Ⅰ和晶型Ⅰ'的发泡窗口。等规聚丁烯-1晶型Ⅰ发泡过程,抑制熔融态向晶型Ⅰ'结晶,使其直接结晶为晶型Ⅰ。等规聚丁烯-1晶型Ⅰ'发泡过程也可使晶型Ⅰ'熔融态直接结晶为晶型Ⅰ。这些结果表明,利用等规聚丁烯-1发泡过程中基体形变使分子链取向能改变结晶过程,可直接从熔融态获得低密度多孔等规聚丁烯-1晶型Ⅰ材料。
CO2 has been extensively used in polymer processing owing to its attractive properties. Dissolution of CO2 in polymer will affect the polymer properties in both melt and solid states. Moreover, the activity of CO2 can be easily tuned by changing temperature and pressure, which provides us a technique to manipulate crystalline modification transition and crystallization of polymers. Isotactic poly-1-butene (iPB-1) is a polymorphous semi crystal polyolefin with many outstanding properties. However, the relatively complex phase transition restricts its commercialization. Manipulation of the crystal modification of iPB-1 by using CO2 provides a potential solution to overcome the drawback. In this work, the crystal modification transformation and crystallization of iPB-1 under CO2 is systematically studied for the first time. The details are shown as follows:
CO2-Inducted crystal phase transition from formⅡto I in iPB-1. CO2 substantially promoted the phase transition rate of formⅡtoⅠ, and formⅡtransformed completely to the formⅠduring the melting process under 5 MPa. The total crystallinity of iPB-1 samples before and after CO2 treatment did not seem to change dramatically, which indicated the phase transition was only occurred in the crystal region. Meanwhile, in-situ high-pressure Fourier transform infrared spectroscopy (FTIR) was used to investigate the phase transition of formⅡtoⅠat various CO2 temperatures and pressures. It was shown that the phase transition rate was increased with increased pressure and decreased with increased temperature. The phase transition of formⅡto formⅠcompleted in several minutes under low temperature and high pressure CO2, which was the most efficient ever reported method to accelerate the phase transition.
CO2-Induced polymorphous phase transition of iPB-1 with form III. The application of CO2 promoted more formⅢto transform into form I', and also made the phase transformation of formⅢto I'occur at a lower temperature. The phase transition of form III to ' and the perfection of form I'crystal lowered the free energy barrier for melting of form III and I', thereby making formsⅢand I'melt directly. The phase transition kinetics of CO2-induced phase transition of formⅢto I'was studied by in-situ high-pressure FTIR. It was shown that the phase transition of formⅢto I'might be comprised two stages:the initial instantaneous nucleation and random nucleation. Most of formⅢtransformed into form I'in the first stage. Meanwhile, the formation of formⅡwas changed from the solid-solid phase transition under ambient N2 to the melt-recrystallization under CO2. The crystalline morphology of the C2-treated iPB-1 with form III was also investigated using the polarized optical microscopy (POM). To obtain the strong orientation, the formation processes of form II displayed the following order:melt crystallization at ambient condition> melt recrystallization under CO2>phase transition upon annealing at ambient condition.
Effect of CO2 on the recrystallization of formⅡfrom iPB-1 with formⅢduring heating. The formation of formⅡduring heating of formⅢcomprised two processes:the solid-solid phase transition and the melt-recrystallization. The solid-solid phase transition of formⅡwas inhibited gradually with increasing CO2 pressure, making relatively more formⅡgenerate through the melt-recrystallization. The nonisothermal recrystallization kinetics of formⅡwas then analyzed by the modified Avrami method. Significant changes in the Avrami parameters at CO2 pressure of 3 MPa indicated a change in the recrystallization mechanism. In-situ high-pressure FTIR was also applied to detected the phase transition of formⅢunder compressed CO2. The results showed that the formⅡrecrystallization mechanism did change at 3 MPa, at which formⅡwas recrystallized from the completely melt state. The directly melt of formⅢinto the melt state at 4 MPa was ascribed to the plasticization effect of CO2.
Effect of CO2 on the nonisothermal crystallization behaviors of iPB-1 melt. The nonisothermal crystallization peak temperature of iPB-1 decreased linearly with increasing CO2 pressure. The crystallized crystal structure of iPB-1 changed from formⅡunder 0.5-8 MPa CO2 to formⅠ' under CO2 at above 10 MPa. A new approach to obtain formⅠ' was found during the nonisothermal crystallization of iPB-1 under high pressure CO2. Furthermore, the modified Avrami method was used to analyze nonisothermal crystallization kinetics of iPB-1 from the melt. The results showed that the gradually reduced n in the nonisothermal crystallization of iPB-1 with the increased CO2 pressure, indicating the possible change in the crystallization mechanism with increasing CO2 pressure. In situ high pressure FTIR measurement of the nonisothermal crystallization evidenced the formⅠ'was directly generated from iPB-1 melt under 10-18 MPa CO2. The gradually changed crystallization process and mechanism was also directly detected by using POM.
Effect of CO2 foaming process on the crystal modification of iPB-1. The high pressure differential scanning calorimeter (DSC) was used to determine the temperature window for foaming iPB-1 with formsⅠorⅠ'. The foaming process of iPB-1 using CO2 inhibited the crystallization of formⅠ' from the melt and made the iPB-1 melt directly transform into formⅠ. It indicated that the deformation of the iPB-1 matrix changed the crystallization behavior, and the porous stable formⅠwas directly generated after the foaming.
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