CN1261385A - 不同颗粒尺寸的含氟聚合物水分散体 - Google Patents

不同颗粒尺寸的含氟聚合物水分散体 Download PDF

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CN1261385A
CN1261385A CN98806539A CN98806539A CN1261385A CN 1261385 A CN1261385 A CN 1261385A CN 98806539 A CN98806539 A CN 98806539A CN 98806539 A CN98806539 A CN 98806539A CN 1261385 A CN1261385 A CN 1261385A
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H·布莱德尔
G·洛尔
G·格罗斯曼
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Abstract

本发明涉及由乳液聚合制备的含氟聚合物水分散体,它包含至少一种平均颗粒尺寸(数均)至少为200nm的含氟聚合物A)和至少一种平均颗粒尺寸(数均)不超过100nm的含氟聚合物B)。A)和B)组分的一种是热塑性材料而另一种组分不能以它的熔体形式进行加工。在整个分散体中,颗粒尺寸的数值分布不是单峰的。该分散体适合于浸润,浸渗或涂覆表面,例如纤维或由纤维或多孔物质制得的板状结构,特别适合于涂覆玻璃纤维结构,以及配制成金属涂层体系。

Description

不同颗粒尺寸的含氟聚合物水分散体
US-A-5576381公开了一种由乳液聚合制得的含氟聚合物水分散体，这种含氟合物不能由熔体进行加工，烧结时形成薄膜，并且含有一种平均颗粒尺寸(数均)为180～400nm的含氟聚合物A)和一种平均颗粒尺寸要低0.3～0.7因子的含氟聚合物B)，因此整个分散体具有颗粒直径的非单峰数值分布。这种分散体是混合相应的分散体，并且如果需要，浓缩至所希望的固体含量而得到的。这种分散体适于浸润，浸渗或涂覆表面，适于浸润或浸渗纤维或由纤维或多孔材料制得的纤维或平板状制品，以及适于涤覆玻璃纤维织物，和配制成金属涂覆体系。
相反，本发明涉及一种由乳液聚合制得的颗粒尺寸不同的含氟聚合物分散体，它包含至少一种平均颗粒尺寸(数均)至少为200nm的含氟聚合物A)和至少一种平均颗粒尺寸(数均)不大于100nm的含氟聚合物B)，A)和B)组分中一种是热塑性而另一种组分不能由熔体进行加工，整个分散体具有颗粒直径的非单峰数值分布。
上述的平均颗粒尺寸是大致上球状颗粒直径的数值平均，这是从将可以在分散体的电镜照片中测量的颗粒直径量化得到的。对于非球状颗粒，两主轴的几何平均值取作为颗粒直径。
本发明优选的分散体具有以下的特征：
不能由熔体加工的组分优选是聚四氟乙烯(PTFE)或者一种有少量共聚单体的四氟乙烯(TFE)聚合物，共聚单体如六氟丙烯(HFP)或者一种烷基上有1～3个碳原子的全氟代烷基乙烯基醚(PAVE)例如全氟-正丙基乙烯基醚(PPVE)，共聚单体量很少以至于这种聚合物不能熔融加工。这些聚合物被称为“改性”PTFE。
大家都知道，“热塑性材料”是指可以熔融加工的聚合物。市场上购得的热塑性含氟聚合物是TFE的聚合物，它含有作为共聚单体的有1～3个碳原子的烷基的PAVE，一种不同于TFE并且具有2～4个碳原子氟化烯例如氟乙烯，1，1-二氟乙烯或HFP以及未氟化的低分子量烯烃如乙烯，丙烯，或者两种或三种这样的共聚单体。
优选的热塑性材料是主要单元为TFE而PPVE，HFP，乙烯或丙烯为次要摩尔比例的二元共聚物，和主要单元为TFE与乙烯和HFP单元的三元聚合物。
选取的共聚单体量要使共聚物是可熔融加工，但仍不具有弹性性能。
优选颗粒尺寸(数均)是组分A)至少230nm和组分B)不超过80nm，优选不超过50nm，特选不超过40nm。
US-A-3925292公开了水分散体，它们含有a)一种不能熔融加工的聚四氟乙烯，和b)一种非弹性的但能熔融加工的四氟乙烯共聚物以及非离子型表面活性剂，优选聚四氟乙烯具有至少300nm平均颗粒尺寸。没有给出关于共聚物颗粒尺寸的信息；仅在一实施例中给出160nm的颗粒尺寸。在这个实施例中，聚四氟乙烯的平均颗粒尺寸为230nm，因此有着共聚物相同数量级的尺寸。
为了制备相应于本发明组分B)细小分散的聚合物，必须采用特殊的措施，例如使用相对大量的表面活性剂，激烈搅拌或增加引发剂使用量。这种类型细小的聚合物分散体在EP-B-612770(US-A-5503213)和EP-B-612569中公开。它们也可以用熟知的种子聚合方法(例如在US-A-4391490中的方法)制备而得。
组分A)和B)在分散体中的重量比例可以在较宽的限制范围内变化，只要颗粒直径具有非单峰数值分布。倘使希望颗粒紧密填充，组分之间的重量比可以容易地从所知的颗粒半径进行计算或估算。倘使要涂覆一多孔载体，将使用更高比例的组分B)。
通常，组分A)和B)可以各自以1～99％重量比例存在，适宜10～90％重量，优选20～80％重量，特别是30～70％重量。在任何特殊的情况中，本领域技术人员将能够-如果需要借助简单的初步实验-为每一种基体“修剪出”一个适当的组分重量比例。
适合的组分A)有市场上购得的含氟聚合物分散体，其平均颗粒尺寸至少200nm(数均)。这种市场上可得的分散体颗粒尺寸分布在180～300nm之间。
本发明的分散体通过混合组分A)水分散体和组分B)水分散体混合而得到，它们可直接用于许多方面而不需加入表面活性剂。
为了其它方面的应用，也为了减少运输体积，将使用高浓缩的分散体而非混合各种分散体，或者相应地进行聚合反应以得到双峰的颗粒尺寸分布而得到。在这些情况中，分散体以熟知的方法进行浓缩。一种适当方法的实例是超滤(US-A-4369266)，通常要加入十二烷基磺酸钠类的阴离子型表面活性剂，或者烷基苯基乙氧化物类非离子型表面活性剂。具有较好生物降解性的相对较长链的烷基胺氧化物(US-A-5219910)是特别适宜的。在组分混合后进行浓缩过程是适宜的。
所加表面活性剂的量取决于浓缩方法的类型，也取决于接下来的应用领域。一般基于聚合物固体含量在4～15％重量之间。如果本发明的分散体例如欲用于涂覆金属，约5％重量相对较低的表面活性剂量是足够的。用于涂覆玻璃纤维织物，通常需要9％～11％重量的表面活性剂量。在这些情况中，所选的表面活性剂应是在烧结成膜中或之后容易除去，例如上面提到的胺氧化物的一种。
本发明分散体适于在平滑，多孔或纤维状材料上形成涂层，例如浸润或浸渗板状或非板状纤维材料或多孔材料，例如由石墨制备的材料。上面提到的平滑基体是金属，陶瓷，玻璃或塑料表面。为了涂覆金属，如必要，可以向本发明分散体加入通常为这种目的的粘合剂树脂，或者用所熟知的方法对金属表面进行预处理。
一个优选的应用领域是涂覆玻璃纤维织物。相比于用可比的各种组分分散体进行处理，本发明分散体可以以明显更少的过程步骤得到理想的层厚，而不产生裂缝或导致薄膜厚薄不均。因此使用本发明分散体意味着大大节省过程步骤，由此在时间和成本上有明显地节省。这一优点并不是以降低质量为代价而得到的；相反，根据本发明得到的薄膜显示出紧密的结构并且比用各种组分得到的涂层有更大的硬度。更具体地可以参考US A5576381。
本发明分散体产生的涂层孔隙率低和电击穿强度高。而且改善了与基体，特别是多孔表面和制品的粘结性能。
本发明在下面的实施例中更详细地进行描述。实施例1
100份重量平均颗粒尺寸(数均)为240nm浓度为58％重量的PTFE水分散体和33.14份重量浓度为21％重量的一种共聚物的水分散体进行混合得到包含88％重量PTFE和12％重量共聚物(基于含氟聚合物)的水分散体，共聚物具有96.4份重量TFE单元和3.6份重量PPVE单元并且具有平均颗粒尺寸(数均)为80nm。
用这种分散体制得厚度为25±3μm的浇铸薄膜。这薄膜的电击穿强度是264kV/mm。为了对比，仅用PTFE分散体得到的浇铸薄膜在厚度为30±3μm时显示出48.3kV/mm的电击穿强度。注：不同薄膜厚度是由于分散体的不同粘质。但是电击穿强度是指一毫米厚度。这种差异在测量方法中应被考虑。实施例2
在实施例1所提的具有88％重量PTFE和12％重量共聚物的固体含量的分散体通过喷射涂覆到一1mm厚度的蚀刻铝板，干燥得到层厚度为12μm。
为了对比，相应的层用仅含PTFE的分散体进行涂覆。
层的孔隙率通过上面滴浓盐酸进行测试。本发明的层，3分钟内只有几个气泡形成，而PTFE层有相当多的气体产生。

Claims (14)

1.一种由乳液聚合制得的颗粒尺寸不同的含氟聚合物水分散体，它含有至少一种平均颗粒尺寸(数均)至少200nm的含氟聚合物A)和至少一种平均颗粒尺寸(数均)不大于100nm的含氟聚合物B)，组分A)和B)中一种是热塑性材料而另一种组分不能由熔体加工，整个分散体具有颗粒直径非单峰的数值分布。
2.权利要求1的分散体，其中组分A)不能由熔体加工。
3.权利要求2的分散体，其中组分A)是聚四氟乙烯。
4.前面权利要求中一项或多项的分散体，它含有表面活性剂。
5.前面权利要求中一项或多项的分散体，其中组分A)和B)各自以1～99％重量比例存在。
6.前面权利要求中一项或多项的分散体，其中组分A)和B)各自以10～90％重量比例存在。
7.权利要求5的分散体，其中组分A)和B)各自以20～80％重量比例存在。
8.权利要求5或6的分散体，其中组分A)和B)各自以30～70％重量比例存在。
9.前面权利要求中一项或多项的分散体，其中组分A)具有至少230nm的平均颗粒尺寸(数均)。
10.前面权利要求中一项或多项的分散体，其中组分B)具有不大于80nm的平均颗粒尺寸(数均)，优选不大于50nm，特别是不大于40nm。
11.制备前面权利要求中一项或多项分散体的方法，其中至少一种含氟聚合物A)的水分散体和至少一种含氟聚合物B)的水分散体进行混合，并且如需要，浓缩至所希望的固体含量，优选至40～65％重量的固体含量。
12.权利要求1～9中任何一项分散体在浸润，浸渗或涂覆表面的用途。
13.权利要求1～9中任何一项分散体在配制金属涂覆体系的用途。
14.权利要求1～9中任何一项的分散体在浸润或浸渗纤维或由纤维或多孔材料制备的板状制品，以及涂覆玻璃纤维织物的用途。
CN98806539A 1997-06-24 1998-06-18 不同颗粒尺寸的含氟聚合物水分散体 Expired - Fee Related CN1106419C (zh)

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CN108676358A (zh) * 2018-05-28 2018-10-19 江苏兆鋆新材料股份有限公司 一种提高浸透性的制备聚苯硫醚热塑性预浸料的方法
CN112501713A (zh) * 2020-11-24 2021-03-16 江苏川羽高分子材料科技有限责任公司 一种含氟聚合物复合纤维的制备方法
CN116987358A (zh) * 2023-09-26 2023-11-03 山东华夏神舟新材料有限公司 一种含氟聚合物浓缩乳液及其制备方法与应用

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CN102432893A (zh) * 2003-08-25 2012-05-02 陶氏环球技术有限责任公司 水分散体、其生产方法及其用途
CN102604124A (zh) * 2003-08-25 2012-07-25 陶氏环球技术有限责任公司 水分散体、其生产方法及其用途
CN102604124B (zh) * 2003-08-25 2015-07-29 陶氏环球技术有限责任公司 水分散体、其生产方法及其用途
CN102432893B (zh) * 2003-08-25 2015-08-12 陶氏环球技术有限责任公司 水分散体、其生产方法及其用途
CN108676358A (zh) * 2018-05-28 2018-10-19 江苏兆鋆新材料股份有限公司 一种提高浸透性的制备聚苯硫醚热塑性预浸料的方法
CN112501713A (zh) * 2020-11-24 2021-03-16 江苏川羽高分子材料科技有限责任公司 一种含氟聚合物复合纤维的制备方法
CN116987358A (zh) * 2023-09-26 2023-11-03 山东华夏神舟新材料有限公司 一种含氟聚合物浓缩乳液及其制备方法与应用
CN116987358B (zh) * 2023-09-26 2023-12-22 山东华夏神舟新材料有限公司 一种含氟聚合物浓缩乳液及其制备方法与应用

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ZA985451B (en) 1999-01-06
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US6566452B1 (en) 2003-05-20
RU2217447C2 (ru) 2003-11-27
CA2295147A1 (en) 1998-12-30
US20030204011A1 (en) 2003-10-30
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TW509709B (en) 2002-11-11
MA24575A1 (fr) 1998-12-31
ATE214405T1 (de) 2002-03-15
UY25061A1 (es) 2001-01-31
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AU8338498A (en) 1999-01-04

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