CN1568336A - 四氟乙烯－全氟丁基乙烯共聚物 - Google Patents

四氟乙烯－全氟丁基乙烯共聚物 Download PDF

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CN1568336A
CN1568336A CNA028201604A CN02820160A CN1568336A CN 1568336 A CN1568336 A CN 1568336A CN A028201604 A CNA028201604 A CN A028201604A CN 02820160 A CN02820160 A CN 02820160A CN 1568336 A CN1568336 A CN 1568336A
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R·L·百利
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Abstract

提供一种通过水性分散聚合技术制备四氟乙烯和全氟丁基乙烯共聚物的聚合方法以及由此制得的树脂。这种共聚物包含相对少量的共聚单体聚合单元，约为0.02－0.6重量％。认为所述共聚物由芯－壳结构组成，其中，所述聚合的共聚单体单元主要在芯中。所述共聚物的基本粒度为0.175－0.203微米，其标准比重小于2.143。这种共聚物具有粒度很小且分子量高的独特组合，是迄今为止所述分散体或细粉状四氟乙烯聚合物所末能获得的组合。本发明的特征在于，在没有氯化锌或其它离子强度促进剂的条件下进行高锰酸盐引发反应以及整个反应。在完成所述反应前，较好在所述完成反应中点处或之前停止加入引发剂。

Description

四氟乙烯-全氟丁基乙烯共聚物
发明背景
本发明涉及通过水性分散聚合反应制备的四氟乙烯和全氟丁基乙烯的共聚物。
许多已有专利揭示了分散聚合四氟乙烯的技术及其变化方法。四氟乙烯分散聚合反应制得已知为“细粉”的树脂。在这种方法中，要往水载体中加入足够的分散剂，使得在合适聚合引发剂存在下加入四氟乙烯并搅拌时，以及在10-40kg/cm2的自生的四氟乙烯压力下进行聚合反应，直到形成胶体状分散的聚合物颗粒，然后停止所述反应。见例如美国专利4,016,345(Holmes，1977)。
也可以通过悬浮聚合方法来制备四氟乙烯粉末，其中，在高速搅拌的水性悬浮液中聚合四氟乙烯单体，所述悬浮液中很少或不使用任何分散剂。悬浮聚合反应制得的粉末类型称为“粒状”树脂或者“粒状粉末”，见例如美国专利3,655,611(Mueller，1972)。
对于所述两种类型的聚合反应方法，已经说明了四氟乙烯和各种氟化烷基乙烯共聚单体的共聚反应。见例如美国专利4,792,594(Gangal等，1988)。本发明涉及水性分散聚合技术，其中，所述聚合反应的产物是本发明分散在水性胶体分散体中的共聚物。通常，所述方法如下：将四氟乙烯单体、用于抑制凝块形成的石蜡以及乳化剂压入包含水和某种聚合引发剂高压釜中。搅拌所述反应混合物，并在合适温度和压力下进行聚合反应。聚合反应形成聚合物的水性分散体。所述分散的聚合物颗粒可以通过本领域已知的技术凝聚，制得细粉聚合物。当往所述聚合反应中加入氟化烷基乙烯共聚单体时，已知所述共聚单体比四氟乙烯单体反应快得多，并且共聚单体的加入速度对所述共聚物中获得的共聚单体分布很重要。当预先单独加入这种共聚单体时，发现所述共聚单体以聚合的形式主要在所述芯中或聚合物颗粒内部。所述共聚单体也可以通过在聚合的某些或者所有过程中注入，并且注入的顺序决定了所述壳的结构，即如果自始至终加入共聚单体，则其在各共聚物颗粒的整个外壳上。
各种已有专利已经揭示了各种四氟乙烯均聚反应以及四氟乙烯和其它单体共聚反应的技术。其中包括美国专利4,576,869(Malhotra，1986)和美国专利6,177,533B1(Jones，2001)。其中包括某些已经或多或少成为用于确定某些涉及四氟乙烯均聚物和共聚物的定义和表征属性的公认方法。其中，那些性质为：
(a)标准比重(SSG)，按照ASTM D-1457-90，通过标准模制试样的排水量进行测量；
(b)粗分散体粒度(RDPS)，通过光谱法或者其它合适的技术进行确定。见例如美国专利4,016,345和4,363,900。通过使用Brookhaven 90+仪器的激光散射来进行测量。
通常在所引用的已有专利中，几乎普通地，均聚物样品的SSG与其分子量呈相反的关系，即高分子量(MW)对应低SSG，通常，SSG越低，则分子量越高。往所述聚合反应中加入共聚单体也可以降低SSG，对于用共聚单体改性的树脂来说，SSG可以用于在指定的固定单体含量条件下推断其分子量变化。
对于聚氟乙烯细粉来说，通常其RDPS约为0.175-0.325微米。这些细粉树脂已知可以用在糊剂挤出工艺以及拉伸(发泡)工艺中，其中，在除去挤出辅助润滑剂之后，所述糊剂挤出形成的挤出物可以迅速拉伸形成各种横截面形状的多孔的结实的产品，如棒、长丝、片材、管等。这种拉伸工艺在美国专利3,953,566(Gore，1976)有述，它一般由于本发明给定中。
迄今为止，对于分散体类型的四氟乙烯均聚物和共聚物来说，通常认为很难获得组合了所需粒度小(RDPS)和分子量(MW)高的树脂。以不同的等价方式表述这一结论，通常认为很难或者不可能获得粗分散体粒度(RDPS)小且标准比重(SSG)低的分散体树脂。
本发明提供一种分散体类型的四氟乙烯和全氟丁基乙烯共聚单体的共聚物，它具有迄今为止未能获得的基本树脂粒度(RDPS)小且SSG低(分子量高)的组合。
发明概述
提供了一种制备四氟乙烯共聚物的聚合方法以及由此制得的共聚物。所述共聚物为分散体/细粉类型的，包含聚合的四氟乙烯单体单元以及共聚的全氟丁基乙烯共聚单体单元，其中，认为所述基本粒子具有芯和壳结构，并且以共聚物总重量计，所述聚合的共聚单体单元占0.02-0.6重量％。所述共聚物的粗分散体基本粒度(RDPS)为0.175-0.203微米，其标准比重(SSG)小于2.143。较佳的是，所述共聚物的共聚单体单元含量为0.05-0.5重量％，所述RDPS为0.178-0.200微米，SSG小于2.140。
所述共聚物可以分散在水性分散体中，和/或可以呈细粉状。
本发明方法的特征在于，通过高锰酸钾引发剂催化所述共聚反应，并在没有任何多价离子强度促进剂如氯化锌的条件下进行整个反应。在完成所述反应前，较好在所述完成反应中点处或之前停止加入引发剂。此外，虽然直至部分聚合反应过程所述共聚单体可以作为聚合反应工艺的部分递增量、间歇地加入，但是较好预先将所述共聚单体加入所述共聚反应器中。
发明详述和优选实施方式
提供通过水性分散聚合技术制备的四氟乙烯和全氟丁基乙烯的共聚物。这种聚合物包含相对少量的氟化共聚单体聚合单元，约为0.02-0.6重量％。所述共聚物认为由芯-壳结构组成，其中，所述聚合的共聚单体单元主要在芯中。所述共聚物的基本粒度为0.175-0.203微米，其标准比重小于2.143。这种树脂尤其适用于发泡(拉伸)工艺，制得高强度的多孔聚四氟乙烯制件。
本发明的聚合物提供迄今为止未能获得的基本粒度很小，且分子量高的组合性能。这些聚合物通过分散聚合方法制备，在以下详细说明及实施例中有说明。从那些实施例，尤其是利用四氟乙烯单体分散聚合反应基本原理可见，本文所述某些工艺步骤是关键。
更具体的说明：
引发聚合反应
通过聚合方法制备本发明的共聚物，其中在没有任何多价离子强度促进剂的条件下，通过高锰酸盐引发剂，较好是高锰酸钾(KMnO4)催化所述共聚反应，并且在反应进程完成30-80％的时候完全停止加入所述引发剂，使反应减速并进行到完成反应。较好约在反应的中点处即在距反应完成40-65％时，最好在反应完成44％的时候停止加入引发剂。
所述全氟丁基乙烯共聚单体较好预先加入所述反应器中，或者直至部分反应仅以增量加入。
分散剂
使用基本上非调聚体的分散剂。全氟辛酸铵(APFO或“C-8”)是可接受的分散剂。已知并优选按程序加入(预先加入并泵入)。减少预先加入物可以使基本粒度增大。
聚合反应控制
已知离子强度会影响基本粒度控制和分散体稳定性。务必使分散体足够稳定，能完成所述聚合反应而不会出现分散体凝结，并且要使分散体足够稳定，能经得起从聚合反应器转移到凝聚器。可以往聚合反应器中预先加入无机盐，使基本粒度增大。通常，多价离子能更有效地增大离子强度。已经使用氯化锌，同时通过减少APFO来控制(增大)所述基本粒度。但是，在本发明的聚合反应中，不用往所述反应中加入多价离子强度促进剂如氯化锌。
已知必须特别关注成分的纯度，以获得本文所述聚合反应中所需的性能。必须使离子杂质(也可以增大离子强度)以及可溶性有机杂质(可以导致链转移或终止)最少。在所有聚合反应中使用超纯水显然是很重要的。
额外测试步骤
具体树脂制得的挤出和发泡(拉伸)条(beading)的断裂强度直接和树脂一般对发泡适应性有关，并且已经使用各种方法来测量断裂强度。使用以下步骤来制备和测试由本发明共聚物制得的发泡条。
对指定的树脂，将113.4g细粉树脂和32.5mlIsoparK混合。在22℃的恒温水浴中老化所述共合物约2小时。通过施加约270psi的预制件压力约20秒，制得直径为1英寸的圆柱预制件。检查所述预制件，确保其中没有任何裂缝。通过从0.100英寸直径的模头(具有30°的进口角)挤出所述预制润滑树脂，制得挤出的条。所述挤出机的机筒直径为1英寸，移动活塞速度为20英寸/分钟。所述挤出机的机筒和模头处于室温下，保持在23℃±1.5℃。通过在230℃下干燥约25分钟，除去所述条中的Isopar K。舍弃所述挤出条开始和末端8英尺，以消除所述末端效应。通过在290℃下拉伸成最终长度50英寸(发泡比为25∶1)的条件下，以100％/秒的起始(其恒速为2英寸/秒)使速度拉伸2.0英寸的挤出条部分发泡。除去距离中心约1英尺的发泡条。使用2英寸的起始样品长度和12英寸/分钟的十字头速度，并使用Instron拉伸试验机测量所述样品在室温(23℃±1.5℃)下的最大断裂负载。重复测量两样品，并记录所述平均值。这一步骤类似于美国专利6,177,533B1中所述的。此处，发泡步骤在290℃下进行，而不是在300℃下进行。
实施例
实施例1
往装有三叶片式搅拌器的50升卧式聚合反应器中加入1.5kg石蜡油、28kg去离子水、18g全氟辛酸铵(APFO)和5.0g溶于约50g去离子水中的丁二酸。将所述反应器和所含物质加热至所述石蜡的熔点以上。用TFE重复排空和加压所述反应器(约1大气压或更少)，直到氧含量降至20ppm或更少。在排空和吹扫循环过程中以约60rpm搅拌所含物质，确保使水脱氧。往真空下排空的反应器中加入8ml作为共聚单体预加入物的PFBE，并将反应器加热至83℃。然后，将TFE加入到反应器中，直到压力达到2.8Mpa、3.0kg，并以80ml/分钟的速度注入溶于去离子水中的高锰酸钾溶液(0.063g/l)，直到已经加入约2.0kgTFE为止。这一过程在约7分钟内完成。以40ml的增量将约320ml 20％APFO溶液加入，在往所述反应器中加入约1kgTFE之后，加入第一增量，并且，之后每加入1kgTFE，就加入下一个增量，这样在加入约9kgTFE之后加入最后一个增量。在2kgTFE量时将高锰酸钾的加入速度降至40ml/分钟，并以这一速度继续加入，直到已经加入约3kg的TFE。然后再次将高锰酸钾的加入速度降至20ml/分钟，直到已经加入5kg的TFE。然后，将所述高锰酸钾的加入速度降至10ml/分钟，并以这一速度继续加入，直到已经往所述反应器中加入约7kg的TFE，这时停止加入所述高锰酸钾。
然后继续所述聚合反应，并在往所述反应器中加入约16kgTFE之后停止所述反应。所得分散体的重量为46.7kg。所述分散体的密度为1.246g/ml(35.0重量％固体)。
在已经反应44％的TFE之后，不再加入高锰酸钾。使所述分散体凝聚并在170℃下干燥。
所述聚合物颗粒的粗分散体粒度(RDPS)为0.203微米，标准比重为2.138。如所示的，聚合产物中共聚单体的含量为0.07重量％。所述条的断裂强度为7.9磅。
实施例2
除了加入60mlPFBE作为反应的预加入物外，重复实施例1的步骤。逐渐加入高锰酸钾，使高锰酸钾溶液以30ml/分钟的速度注入，直到已经加入2480ml，然后将速度调整至40ml/分钟，直到再加入了1740ml，然后，将速度降至20ml/分钟，直到已经再加入1640ml，之后停止加入高锰酸钾，这时，已经反应了6kg的TFE。
继续所述聚合反应，并在已经往所述反应器中加入16kgPTFE之后停止所述反应。所得分散体的重量为49.7kg，所述分散体包含35.7重量％的固体。
所述反应产物中共聚单体的含量为0.5重量％。
所述聚合颗粒的RDPS为0.190微米，SSG为2.135。所述条的断裂强度为9.0磅。
实施例3
除了往所述反应器中预先加入43mlPFBE之后在聚合反应过程中以增量加入额外的PFBE，以2个7ml的增量加入总共14ml的PFBE外，重复实施例1所述的步骤。在已经往所述反应器中加入2kgTFE之后，加入第一个7ml的PFBE增量，在已经加入4kgTFE之后，加入第二个7ml增量。
在开始时以约54ml/分钟的速度加入高锰酸钾，直到已经加入2000ml，然后，将速度降至约50ml/分钟，直到已经再加入了900ml，之后，将速度再次降至约33ml/分钟，直到已经再加入了1780ml，之后停止加入高锰酸钾。这时，已经反应了6kg的TFE。
继续所述聚合反应，并在已经往所述反应器中加入16kgPTFE之后停止所述反应。所得分散体的重量为50.7kg，所述分散体包含33.9重量％的固体。
所述反应产物中共聚单体的含量为0.5重量％。在所述TFE反应完成38％时停止聚合反应的引发。
所述聚合颗粒的RDPS为0.176微米，SSG为2.142。所述测试条的断裂强度为11.0磅。
对比例A(省去预先加入PFBE)
除了不预先加入43ml PFBE，而是以7个7ml增量加入49ml PFBE外，基本上以实施例3所述的步骤进行聚合反应。在已经加入1kgTFE之后加入第一个7ml增量。此后每加入1kgTFE之后就加入下一个增量，在已经加入7kgTFE之后，加入最后一个增量。
在开始时以约54ml/分钟的速度加入高锰酸钾溶液，直到已经加入910ml，将所述速度降至约20ml/分钟，直到已经再加入400ml，然后，将速度增大至约40ml/分钟，直到已经再加入1600ml，之后停止加入高锰酸钾。这时，已经反应了7kg的TFE，并且已经加入了总共2910ml的高锰酸钾溶液。
继续所述聚合反应，并在已经往所述反应器中加入16kgTFE之后停止所述反应。所得分散体的重量为46.3kg，所述分散体的密度为1.244g/ml(34.8重量％固体)。使所述分散体凝聚并在180℃下干燥。
所述聚合颗粒的RDPS为0.258微米，SSG为2.145。所述条的断裂强度为7.7磅。
对比例B(预先加入过量的PFBE)
除了如实施例1所述预先往所述反应器中加入90.0ml而不是8ml PFBE外，基本如上所述重复实施例1的反应。以约53ml/分钟的速度加入高锰酸钾溶液，直到已经加入了约5890ml，这时停止所述试验，发现没有进行任何反应。
对比例C(不加PFBE)
除了不加PFBE外，基本如上所述重复实施例1的反应。在开始时以约60ml/分钟的速度加入高锰酸钾溶液，直到已经加入2.0kg TFE，然后，将该速度降至约40ml/分钟，直到已经加入5kg的TFE，并再次将速度降至20ml/分钟，之后停止加入高锰酸钾，这时已经反应了9kg TFE，并且已经加入总共1250ml的高锰酸钾溶液。
继续所述聚合反应，并在已经往所述反应器中加入总共16kgTFE之后停止所述反应。所得分散体的重量为45.7kg，所述分散体包含36.7重量％的固体。使所述分散体凝聚并在170℃下干燥。
所述聚合颗粒的RDPS为0.284微米，SSG为2.158。所述发泡条试样的断裂强度为6.9磅。
虽然已经结合某些实施方式和详细描述已经说明了本发明，但是本领域的技术人员应明白，在不背离本发明要点的条件下可以对这些细节进行修改或变动，并且这些修改或变动认为在以下权利要求书所述的范围内。

Claims (22)

1.分散体/细粉型四氟乙烯共聚物的共聚方法，所述共聚物主要包含99.4-99.98重量％四氟乙烯单体单元和0.02-0.6重量％共聚的全氟丁基乙烯共聚单体单元，所述方法包括：
(a)在加压反应器中共聚所述单体和共聚单体，
(b)通过加入高锰酸钾(KMnO4)来引发所述共聚反应，
(c)在没有任何离子强度促进剂的条件下进行整个反应，
(d)在反应还未完成80％的时候停止加入引发剂(KMnO4)。
2.权利要求1所述的方法，所述方法包括在共聚反应中预先加入共聚单体。
3.权利要求1所述的方法，所述方法包括从反应开始到反应仅完成一部分的过程中以增量间歇地加入共聚单体。
4.权利要求1所述的方法，所述方法包括在所述反应还未完成60％的时候停止加入KMnO4引发剂。
5.权利要求1所述的方法，所述方法包括在所述反应还未完成50％的时候停止加入KMnO4引发剂。
6.权利要求1所述分散体/细粉型四氟乙烯共聚物的共聚方法，其特征在于，
所述聚合的共聚单体单元占共聚物总重量的0.02-0.6重量％，
所述共聚物的粗分散体基本粒度(RDPS)为0.175-0.203微米，标准比重(SSG)小于2.143。
7.权利要求6所述的方法，其特征在于，所述共聚物的RDPS为0.175-0.203微米，SSG小于2.140。
8.权利要求6所述的方法，所述方法包括在共聚反应中预先加入共聚单体。
9.权利要求6所述的方法，所述方法包括从反应开始到反应仅完成一部分的过程中以增量间歇地加入共聚单体。
10.权利要求6所述的方法，所述方法包括在所述反应还未完成60％的时候停止加入KMnO4引发剂。
11.权利要求6所述的方法，所述方法包括在所述反应还未完成50％的时候停止加入KMnO4引发剂。
12.一种分散体/细粉型四氟乙烯共聚物，它包含聚合的四氟乙烯单体单元和共聚的全氟丁基乙烯共聚单体单元，其特征在于，
(a)所述共聚的共聚单体单元占所述共聚物总重量的0.02-0.6重量％，
(b)所述共聚物的粗分散体基本粒度(RDPS)为0.175-0.203微米，标准比重(SSG)小于2.143。
13.权利要求12所述的共聚物，其特征在于，所述共聚单体单元含量为0.05-0.5重量％。
14.权利要求12所述的共聚物，其特征在于，所述RDPS为0.178-0.200微米，SSG小于2.140。
15.权利要求12所述的共聚物，其特征在于，所述共聚物分散在水性分散体中。
16.权利要求12所述的共聚物，其特征在于，所述共聚物呈细粉状。
17.一种分散体/细粉型四氟乙烯共聚物，它包含聚合的四氟乙烯单体单元和共聚的全氟丁基乙烯共聚单体单元，其特征在于，
(a)所述共聚的共聚单体单元占所述共聚物总重量的0.05-0.5重量％，
(b)所述共聚物的RDPS为0.178-0.200微米，标准比重(SSG)小于2.140。
18.权利要求17所述的共聚物，其特征在于，所述共聚物分散在水性分散体中。
19.权利要求17所述的共聚物，其特征在于，所述共聚物呈细粉状。
20.权利要求12所述的共聚物，其特征在于，所述共聚物成形为断裂强度至少为7.9磅的发泡条。
21.权利要求17所述的共聚物，其特征在于，所述共聚物成形为断裂强度至少为9.0磅的发泡条。
22.权利要求20所述的共聚物，其特征在于，所述共聚物的断裂强度至少为11.0磅。
CNB028201604A 2001-10-15 2002-10-02 四氟乙烯－全氟丁基乙烯共聚物 Expired - Lifetime CN1274729C (zh)

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