聚丙烯取向结晶行为及其微孔膜制备的研究
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摘要
全同聚丙烯(iPP)是典型的具有多晶型的半结晶型聚合物之一，由于材料的化学特性和加工工艺的不同，等位聚丙烯主要有单斜的晶型,三斜的晶型和正交的γ-晶型三种结晶形态，其中和β晶型较为常见。在通常的加工情况下-聚丙烯热性能最稳定所以最容易得到，亚稳态的β晶型聚丙烯与晶型聚丙烯相比，具有很多优良的性能，比如较低的结晶密度，熔融温度和熔融热焓，另外它的抗冲击性能和韧性得到大大的改善。然而只有利用一些特殊的方法才能得到，如温度梯度法、剪切熔体法或者特殊成核剂法等，针对聚丙烯β晶结晶机理的研究很少。近年来，β-iPP的形变研究得到广泛研究，主要是因为不同相变间密度的差异在拉伸过程中使得低密度向高密度转变，发生β晶型向晶型转变形成微孔，从而可以用来制备气体交换膜、过滤膜或锂电池隔膜等。
我们利用高聚物熔体结晶过程中存在过冷态的性质，将纤维引入到过冷态的聚丙烯熔体中，制备了均质和异质纤维复合体系，从而用纤维诱导得到了取向的β-iPP结晶。通过对比均质纤维和异质纤维诱导的聚丙烯β晶体的再次熔融重结晶行为发现聚丙烯基体在均质和异质纤维/基体复合体系中的结晶机理不同，熔体中分子链取向是聚丙烯β结晶的前提。从而在理论上更全面的认识了聚丙烯β晶型的形成机理。
通过研究聚丙烯β晶结晶机理及聚丙烯纤维/基体复合体系β结晶对各种条件的依赖性，确立了聚丙烯薄片的最佳制备条件，从而为高质量的β聚丙烯薄片的制备建立了新方法。对获得的高质量聚丙烯薄片进行了拉伸成孔实验，研究结果表明，由于所制薄片中的β聚丙烯晶体高度取向，晶区与非晶区的不均一应变行为增强了其成孔性和成孔均匀性。通过微孔的数量、尺寸、分布等对拉伸温度、速率、倍速、纵横向拉伸比等诸多拉伸参数依赖性研究，确定了最佳拉伸工艺条件，从而制备了具有较高孔隙率、均匀孔径分布的聚丙烯微孔膜。微孔膜的平均孔径为50-100nm，孔隙率为40~50%，与美国Celgard的聚乙烯微孔薄膜结构类似（孔隙率为40~45%）。跟踪研究聚丙烯微孔膜的力学性能。结果表明，通过控制聚丙烯纤维的熔融程度，可实现纤维的表面熔融诱导聚丙烯结晶，由此产生聚丙烯晶体单向拉伸产生微孔，而未熔融的聚丙烯纤维中心部分不形成微孔，此部分聚丙烯纤维对微孔聚丙烯膜起到了增强的作用，使其抗张强度大大增加。
将微孔膜作为锂电池隔膜进行电池装机实验测试电性能，测试结果表明，电池的离子导电率、电化学稳定窗口、电池容量和循环性能等各项性能均满足要求，且优于美国Celgard公司的聚乙烯隔膜，明显优于国产PP隔膜。
由于纤维的部分熔融诱导β聚丙烯结晶，未完全熔融的聚丙烯纤维仍有一定的强度可以对聚丙烯基体起到增强作用。所以我们进一步对比研究聚丙烯纤维和尼龙纤维增强聚丙烯复合体系的机械性能，并从纤维和聚丙烯复合体系的界面方面讨论了影响其性能的因素。结果表明聚丙烯纤维和尼龙纤维的加入都能大大提高复合体系的拉伸强度和拉伸弹性模量。但是由于纤维引入温度对复合体系界面结晶的影响，同质纤维复合体体系的韧性对样品制备温度有很大依赖性，随温度的升高而增大，且远远大于异质纤维复合体系。
同时我们还对成核剂诱导的β-iPP的熔融重结晶行为作了初步的对比研究。研究发现，β-iPP熔融重结晶行为受热历史影响较大，熔融过程中记忆效应使样品在退火过程中自成核结晶，使结晶显影般瞬间完成，熔融温度继续升高使熔体完全处于无序状态，β成核剂才会起作用从而诱导β-iPP的形成。
Isotactic polypropylene (iPP) is one of the semicrystalline polymersexhibiting pronounced polymorphisms and morphologies depending onboth the chemical characters of the materials and their preparationconditions. At least three crystalline modifications, i.e., the monoclinic
-form, the trigonal-form and the orthorhombic γ-form, have beenreported. It was well documented that the-iPP crystals arethermodynamically most stable and commercial grade iPP crystallizesfrom bulk most generally in its-form under traditional industryprocessing conditions. The metastable-iPP exhibits some excellentperformance characteristics such as low crystal density, meltingtemperature, fusion enthalpy, the remarkably improved elongation atbreak and impact strength, which make it useful for many industrialapplications. It can, however, only be obtained through some kinds ofspecial procedures, such as crystallization in thermal gradient,crystallization of the sheared or elongated melts, or crystallization at thepresence of nucleation agents. The formation mechanism of the-iPP crystals is, however, not clear.
The deformation of-form polypropylene has been an interestingsubject of research because transformation from to or to smectic formwith unusual micropore formation can be obserIsotactic polypropylene(iPP) is one of the semicrystalline polymers exhibiting pronouncedpolymorphisms and morphologies depending on both the chemicalcharacters of the materials and their preparation conditions. At least threecrystalline modifications, i.e., the monoclinic-form, the trigonal-formand the orthorhombic γ-form, have been reported. It was welldocumented that the-iPP crystals are thermodynamically most stableand commercial grade iPP crystallizes from bulk most generally in its
-form under traditional industry processing conditions. The metastable
-iPP exhibits some excellent performance characteristics such as lowcrystal density, melting temperature, fusion enthalpy, the remarkablyimproved elongation at break and impact strength, which make it usefulfor many industrial applications. It can, however, only be obtainedthrough some kinds of special procedures, such as crystallization inthermal gradient, crystallization of the sheared or elongated melts, orcrystallization at the presence of nucleation agents. The formationmechanism of the-iPP crystals is, however, not clear. The deformationof-form polypropylene has been an interesting subject of researchved inthe process of deformation. So it can be used to prepare gas exchange membrane, filter membrane or seperator of lithium-ion batteries.
In our reasearch group, by introducing fibers into supercooledmolten iPP matrices, homogeneous and heterogeneous matix-fibercomposites have been prepared, and the-iPP cylindritic crystals wasproduced. It can be seen that the different origins of the β-iPP cylindritesin those composites by comparing the melt recrystallization behaviors ofthe-iPP crystals. The oriented molecular chain in melt plays a veryimportant role in the subsequent-iPP crystallization.
The best preparation condition of-iPP cylindritic crystals can beobtained depending on the formation mechanism and crystallizationcondition. Microporous membranes obtained from fibers induced-formpolypropylene films by stretching. The micropores are formedhomogeneously for the different strain of oriented-iPP crystalline andamorphous phases. The microporous membrane had pores around50-100nm, porosity of40~50%and the similar structure with the PEmicroporous of Celgard(USA). The formation of the β-iPP is related tothe melting, or at least partial melting of the iPP fibers.The machenicalproperties of microporous membrane can improved greatly for partialmelting of the iPP fibers.
The porous membrane was used as Lithium-ion battery separators totest electric properties. It was observed that ionic conductivity,electrochemical stability window and charge-discharge cycle all meet the requirment of battery, and are better than domestic microporousmembrane.
On the base of above experiments, we compared the mechanicalproperties of homogeneous iPP fiber–matrix composites andheterogeneous polyamide (PA)–iPP fiber–matrix composites. It wasfound that the mechanical properties of those composites such an thetensile modulus and tensile strength all increased significantly. Theelongation at break of iPP fibers/β-PP self-reinforced compositessignificantly increased with preparation temperature elevated which isdue to the surface crystallization contributes to the better interfaceadhesion and provides better bonding for iPP fibers/PP composites,while PA fibers/PP composites still exhibit a brittle fracture for the weakinterfacial adhesion between PA fibers and PP matrix.
The preliminary study on melt recrystallization behaviors of the
-iPP crystals induced by β-nucleating agent. A new type of
-modification has been developed by self-seeding process.The growthprocess of these crystals is just like “photographic development process.”Crystalline phase transformation and the memory effect caused by localorder was observed during the melting and annealing process. A hightemperature is sufficient to destroy the local order and the β-nucleatingagent efficiently induces formation of β-form.
我们利用高聚物熔体结晶过程中存在过冷态的性质，将纤维引入到过冷态的聚丙烯熔体中，制备了均质和异质纤维复合体系，从而用纤维诱导得到了取向的β-iPP结晶。通过对比均质纤维和异质纤维诱导的聚丙烯β晶体的再次熔融重结晶行为发现聚丙烯基体在均质和异质纤维/基体复合体系中的结晶机理不同，熔体中分子链取向是聚丙烯β结晶的前提。从而在理论上更全面的认识了聚丙烯β晶型的形成机理。
通过研究聚丙烯β晶结晶机理及聚丙烯纤维/基体复合体系β结晶对各种条件的依赖性，确立了聚丙烯薄片的最佳制备条件，从而为高质量的β聚丙烯薄片的制备建立了新方法。对获得的高质量聚丙烯薄片进行了拉伸成孔实验，研究结果表明，由于所制薄片中的β聚丙烯晶体高度取向，晶区与非晶区的不均一应变行为增强了其成孔性和成孔均匀性。通过微孔的数量、尺寸、分布等对拉伸温度、速率、倍速、纵横向拉伸比等诸多拉伸参数依赖性研究，确定了最佳拉伸工艺条件，从而制备了具有较高孔隙率、均匀孔径分布的聚丙烯微孔膜。微孔膜的平均孔径为50-100nm，孔隙率为40~50%，与美国Celgard的聚乙烯微孔薄膜结构类似（孔隙率为40~45%）。跟踪研究聚丙烯微孔膜的力学性能。结果表明，通过控制聚丙烯纤维的熔融程度，可实现纤维的表面熔融诱导聚丙烯结晶，由此产生聚丙烯晶体单向拉伸产生微孔，而未熔融的聚丙烯纤维中心部分不形成微孔，此部分聚丙烯纤维对微孔聚丙烯膜起到了增强的作用，使其抗张强度大大增加。
将微孔膜作为锂电池隔膜进行电池装机实验测试电性能，测试结果表明，电池的离子导电率、电化学稳定窗口、电池容量和循环性能等各项性能均满足要求，且优于美国Celgard公司的聚乙烯隔膜，明显优于国产PP隔膜。
由于纤维的部分熔融诱导β聚丙烯结晶，未完全熔融的聚丙烯纤维仍有一定的强度可以对聚丙烯基体起到增强作用。所以我们进一步对比研究聚丙烯纤维和尼龙纤维增强聚丙烯复合体系的机械性能，并从纤维和聚丙烯复合体系的界面方面讨论了影响其性能的因素。结果表明聚丙烯纤维和尼龙纤维的加入都能大大提高复合体系的拉伸强度和拉伸弹性模量。但是由于纤维引入温度对复合体系界面结晶的影响，同质纤维复合体体系的韧性对样品制备温度有很大依赖性，随温度的升高而增大，且远远大于异质纤维复合体系。
同时我们还对成核剂诱导的β-iPP的熔融重结晶行为作了初步的对比研究。研究发现，β-iPP熔融重结晶行为受热历史影响较大，熔融过程中记忆效应使样品在退火过程中自成核结晶，使结晶显影般瞬间完成，熔融温度继续升高使熔体完全处于无序状态，β成核剂才会起作用从而诱导β-iPP的形成。
Isotactic polypropylene (iPP) is one of the semicrystalline polymersexhibiting pronounced polymorphisms and morphologies depending onboth the chemical characters of the materials and their preparationconditions. At least three crystalline modifications, i.e., the monoclinic
-form, the trigonal-form and the orthorhombic γ-form, have beenreported. It was well documented that the-iPP crystals arethermodynamically most stable and commercial grade iPP crystallizesfrom bulk most generally in its-form under traditional industryprocessing conditions. The metastable-iPP exhibits some excellentperformance characteristics such as low crystal density, meltingtemperature, fusion enthalpy, the remarkably improved elongation atbreak and impact strength, which make it useful for many industrialapplications. It can, however, only be obtained through some kinds ofspecial procedures, such as crystallization in thermal gradient,crystallization of the sheared or elongated melts, or crystallization at thepresence of nucleation agents. The formation mechanism of the-iPP crystals is, however, not clear.
The deformation of-form polypropylene has been an interestingsubject of research because transformation from to or to smectic formwith unusual micropore formation can be obserIsotactic polypropylene(iPP) is one of the semicrystalline polymers exhibiting pronouncedpolymorphisms and morphologies depending on both the chemicalcharacters of the materials and their preparation conditions. At least threecrystalline modifications, i.e., the monoclinic-form, the trigonal-formand the orthorhombic γ-form, have been reported. It was welldocumented that the-iPP crystals are thermodynamically most stableand commercial grade iPP crystallizes from bulk most generally in its
-form under traditional industry processing conditions. The metastable
-iPP exhibits some excellent performance characteristics such as lowcrystal density, melting temperature, fusion enthalpy, the remarkablyimproved elongation at break and impact strength, which make it usefulfor many industrial applications. It can, however, only be obtainedthrough some kinds of special procedures, such as crystallization inthermal gradient, crystallization of the sheared or elongated melts, orcrystallization at the presence of nucleation agents. The formationmechanism of the-iPP crystals is, however, not clear. The deformationof-form polypropylene has been an interesting subject of researchved inthe process of deformation. So it can be used to prepare gas exchange membrane, filter membrane or seperator of lithium-ion batteries.
In our reasearch group, by introducing fibers into supercooledmolten iPP matrices, homogeneous and heterogeneous matix-fibercomposites have been prepared, and the-iPP cylindritic crystals wasproduced. It can be seen that the different origins of the β-iPP cylindritesin those composites by comparing the melt recrystallization behaviors ofthe-iPP crystals. The oriented molecular chain in melt plays a veryimportant role in the subsequent-iPP crystallization.
The best preparation condition of-iPP cylindritic crystals can beobtained depending on the formation mechanism and crystallizationcondition. Microporous membranes obtained from fibers induced-formpolypropylene films by stretching. The micropores are formedhomogeneously for the different strain of oriented-iPP crystalline andamorphous phases. The microporous membrane had pores around50-100nm, porosity of40~50%and the similar structure with the PEmicroporous of Celgard(USA). The formation of the β-iPP is related tothe melting, or at least partial melting of the iPP fibers.The machenicalproperties of microporous membrane can improved greatly for partialmelting of the iPP fibers.
The porous membrane was used as Lithium-ion battery separators totest electric properties. It was observed that ionic conductivity,electrochemical stability window and charge-discharge cycle all meet the requirment of battery, and are better than domestic microporousmembrane.
On the base of above experiments, we compared the mechanicalproperties of homogeneous iPP fiber–matrix composites andheterogeneous polyamide (PA)–iPP fiber–matrix composites. It wasfound that the mechanical properties of those composites such an thetensile modulus and tensile strength all increased significantly. Theelongation at break of iPP fibers/β-PP self-reinforced compositessignificantly increased with preparation temperature elevated which isdue to the surface crystallization contributes to the better interfaceadhesion and provides better bonding for iPP fibers/PP composites,while PA fibers/PP composites still exhibit a brittle fracture for the weakinterfacial adhesion between PA fibers and PP matrix.
The preliminary study on melt recrystallization behaviors of the
-iPP crystals induced by β-nucleating agent. A new type of
-modification has been developed by self-seeding process.The growthprocess of these crystals is just like “photographic development process.”Crystalline phase transformation and the memory effect caused by localorder was observed during the melting and annealing process. A hightemperature is sufficient to destroy the local order and the β-nucleatingagent efficiently induces formation of β-form.
引文
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