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CN1145600A - 多孔聚四氟乙烯组合物 - Google Patents

多孔聚四氟乙烯组合物 Download PDF

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CN1145600A
CN1145600A CN94195073.5A CN94195073A CN1145600A CN 1145600 A CN1145600 A CN 1145600A CN 94195073 A CN94195073 A CN 94195073A CN 1145600 A CN1145600 A CN 1145600A
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ptfe
fibril
blend
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P·A·布兰卡
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WL Gore and Associates Inc
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08L27/18—Homopolymers or copolymers or tetrafluoroethene
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2027/00—Use of polyvinylhalogenides or derivatives thereof as moulding material
    • B29K2027/12—Use of polyvinylhalogenides or derivatives thereof as moulding material containing fluorine
    • B29K2027/18—PTFE, i.e. polytetrafluorethene, e.g. ePTFE, i.e. expanded polytetrafluorethene
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/0088—Blends of polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
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Abstract

在本发明中，对树脂组合物的共混物和共混技术进行优化，以在所得拉伸过的材料中获得结点尺寸和原纤长度与热稳定性的附加性能之间的所希望的平衡。拉伸过的共混物可被描述成由原纤互相连接的结点组成微结构的聚四氟乙烯多孔材料，该材料包含两种不同聚四氟乙烯的共混物，一种聚四氟乙烯是四氟乙烯的均聚物，另一种聚四氟乙烯是改性的四氟乙烯聚合物。

Description

多孔聚四氟乙烯组合物
本发明的领域
本发明涉及多孔聚四氟乙烯组合物，尤其是涉及这种多孔组合物的共混物。
本发明的背景
可以拉伸聚四氟乙烯(PTFE)形成带、管、珠或膜(其中的微结构是由原纤互相连接的一系列结点组成的)来制备各种产品(例如参见美国专利3,953,566)。然而，对于一些形成开放式结构的树脂，发泡产品的高温结构稳定性降低了，这就降低或消除了烧结或热锁定(thermally-lock)产品的能力。本发明的方法能形成均匀地分布在成形制品中且是热稳定的大的结点和长的原纤，因此能被烧结或热锁定。
已开展了一些对聚四氟乙烯树脂的共混物进行拉伸的研究。美国专利4,973,609(Browne)阐述了对商品购得的聚四氟乙烯微细粉末进行混和和拉伸，获得了原纤和结点结构以及比先前多孔含氟聚合物材料更高的抗张强度。所阐述的较好的混和方法是在润滑剂存在下并经鼓转过程简单地混和细小粉末状PTFE组分。美国专利(Harada和Mano)描述了一种多孔PTFE材料的经拉伸的共混物，其中共混物是高于2,000,000MW的高分子量PTFE和低于1,000,000MW的低分子量PTFE的混合物。Browne和Harada等人都在其实施例中使用均聚物PTFE组分或可熔融加工的含氟聚合物组分。他们都没有提及使用改性的PTFE均聚物。
美国专利4,482,516描述了一种制造据称含大结点和长原纤的多孔PTFE制品的方法。在该方法中，在除去润滑剂之后压实挤出物，而后拉伸获得具有高基体抗张强度、长原纤和大结点的多孔制品。在该专利中，用粗度因子(coarseness factor)来描述微结构。对于给定的经拉伸的PTFE制品，该因子是堆积密度与起泡点之比，它按下述公式计算：
Figure A9419507300031
本发明的方法可制得粗度因子比美国专利4,482,516的实施例中所述的值高得多的多孔PTFE制品。
本发明的概述
在本发明中，对树脂组合物的共混物和共混技术进行优化，以在所得拉伸过的材料中获得结点尺寸和原纤长度与热稳定性的附加性能之间的所希望的平衡。
拉伸过的共混物可被描述成具有由原纤互相连接的结点的微结构的聚四氟乙烯多孔材料；所述材料包含两种不同聚四氟乙烯的共混物，一种聚四氟乙烯是四氟乙烯的均聚物，另一种聚四氟乙烯是四氟乙烯的改性聚合物。
术语“改性”是指仅存在少量的共聚单体；亦即共聚单体的数量不会大得足以使PTFE聚合物变成可熔融加工的。换句话说，共聚物保持PTFE均聚物的非熔融加工特性。
附图的简要说明
图1a和1b是实施例1膜的形式的经拉伸过的材料的显微照相，图1a是膜的上层，图1b是边缘的横截面。
图2是产物高温结构稳定性与拉伸过材料的微结构的关系。
本发明的详细说明
有许多种类的聚四氟乙烯(PTFE)聚合物是可商品购得的。那些在本领域中视为细小粉末状的聚四氟乙烯特别可用于拉伸制造多孔拉伸的PTFE。
本发明通过使用两种PTFE聚合物来制备被拉伸成含大结点和长原纤的开放式微结构并具有良好高温结构稳定性的树脂；所用的一种聚合物是PTFE均聚物，另一种是改性的均聚物。所用的量可为10-90重量％的均聚物和90-10重量％的改性均聚物。较好的范围为10-50，或20-50重量％的均聚物，其余的为改性均聚物。
均聚物比改性聚合物更易以低发泡速度被拉伸。
聚合物以水分散体形式获得或制成水分散体形式，将分散体混和在一起并凝结和沉淀固体来使它们共混。然后将干固体进行润滑，糊料挤压，压延加热干燥，而后快速拉伸获得均匀而且在高于均聚物熔融的温度下结构稳定的含大结点和长原纤的非常开放的微结构。原纤的平均长度为25微米或更长，较好地为100微米或更长。
当不同的PTFE聚合物以分散体形式混和时，与干混细小粉末附聚物(直径为400-500μ的数量级)相反，是在原始颗粒(直径为0.23μ的数量级)尺度上发生紧密混和。混和较大的附聚物导致发泡的最终产物在总体上不均匀，而分散体混和的聚合物获得高度均匀的发泡产物。
在一个实例中，当高分子量PTFE均聚物与低分子量改性聚合物混和时，在发泡的微结构与高温结构稳定性之间产生强烈的协同作用。发泡时共混物中的改性聚合物组分对原纤的形成影响很小。这就大大减少了形成原纤的引发点的数目，获得了由大结点和长原纤组成的微结构。这样形成的原纤几乎完全是由高分子量的均聚物组分组成，低分子量改性聚合物主要存在于结点上。当将发泡的PTFE制品加热至其结构分解的温度时，原纤发生断裂而导致制品破坏。在本发明中，原纤是由高分子量的聚合物组成的，结果整个制品在较高的温度下具有结构稳定性。本发明独特的高温结构稳定性使树脂共混物的拉伸材料能在远高于PTFE熔点的高温下被加工。不同分子量PTFE均聚物的共混物不显示出这种协同作用，因而这种类型的共混物的利用率较低。
一种用于被拉伸共混物的主要PTFE树脂组分是PTFE均聚物，另一种主要组分是“改性”的均聚物。共聚单体单元由氟化烯型不饱和共聚单体提供。较好的共聚单体单元是由六氟丙烯或由全氟(烷基乙烯基醚)，通常是全氟(丙基乙烯基醚)提供的。如上所述，共聚单体单元的量是使共聚物保持均聚物的非熔融加工特性。本发明共混物中存在的少量改性剂可通过对树脂共混物红外光谱的特定吸收带强度进行比较而检测出来并确定其数量。美国专利4,391,940中介绍了一种FTIR方法，用于对以四氟乙烯为基的含氟聚合物中的三氟氯乙烯(CTFE)，全氟丙烯(HFP)和全氟(丙基乙烯基醚)(PPVE)进行定量测定。
以分散体形式混和PTFE树脂组分，可达到原始颗粒的紧密混和。然后使共混物凝结并干燥。在细小粉末中加入合适的润滑液体并共混之。制造一预型件(preform)，用糊料挤压得到所希望的预型件的形状。可压延挤压物，而后干燥除去润滑剂。在纵向或横向或此两个方向拉伸所得的型件，以获得所希望的孔隙度和微结构。最后，可加热拉伸过的PTFE至高于结晶熔点的温度，以将结构热锁定。所希望的形状可为带、长丝、膜、棒、管等。
拉伸过的PTFE的松弛时间为200秒或更长，粗度因子为0.6(g/cc)/psi或更大。分子量是这样确定的，首先测定PTFE树脂的标准比重(SSG)，随后按Doban等在1958年9月18日于大西洋城(新泽西州)召开的美国化学学会会议上提出的论文“PTFE的分子量”中的公式来计算。
该公式是： Mn = 0.597 [ log 0.157 2.306 - SSG ] - 1 × 10 6
Mn＝数均分子量
除了使样品不经湿度处理并且较快速地提高压力外，其余均按ASTM D-4894和D-4895来确定SSG。
实施例1
从杜邦公司(duPont)获得分散体形式的PTFE均聚物。该四氟乙烯是按Malhotra在美国专利4,576,869中所述的技术聚合的。标准比重为约2.158g/cc，该值相当于平均分子量为23,000,000。该均聚物分散体与分散体形式的CD090(由ICI生产的改性PTFE)混和，其混和比按聚合物固体计是30％高分子量PTFE均聚物和70％CD090。CD090的分子量为4,675,000(SSG为2.189g/cc)，它大部分是由四氟乙烯的重复单元组成，含有很少量的氟化共聚单体单元。制备总量30lbs、固体浓度为15％的聚合物。使用电动叶轮搅拌使混合物凝结。凝结后，从整体水中过滤分离出混和的细小粉末，在烘箱内干燥除去任何剩余的水分。然后将15.0磅这种粉末试样与3.12磅沸点在170-210℃范围的基本上为脂族烃的润滑剂混和。混和后，将润滑的粉末压成直径为4英寸的圆柱形片。通过矩形孔模将片挤压成约6.0英寸宽和0.027英寸厚的带。这种带在辊间压缩成最终厚度为0.00385英寸。在加热的辊上干燥带以除去润滑剂，而后以3.95∶1的比率进行拉伸。最后，使带通过保持在远高于PTFE结晶熔点的温度下的热辊，烧结或热锁定PTFE结构。所得的带非常均匀，且含很大的结点和长的原纤。结点是柱形的且连续地穿过带的整个厚度。
使用ASTM F316-80测量乙醇起泡点(EBP)。切割称重一正方形的带并测量长度、宽度和厚度来确定其整体密度。平均EBP为0.30psi，整体密度为0.473g/cc。按美国专利4,482,516计算得粗度因子为1.58(g/cc)/psi。
这种带可有各种应用，如作为电介质的卷带电缆。由于柱状结点的结构而使它耐压碎。在高温下具有结构稳定性。拉伸过的材料可用作医疗移植装置，电缆绝缘体，滤膜，或衬垫材料。
由图1a和1b可见，拉伸过的带包含大体排齐的一列列结点(SEM图中长的垂直排列的深色区域)，并具有许多与结点的大致方向约成直角把结点连接起来的绳状或阶梯状原纤(SEM图中水平分散的白色细线)。实施例2
所用的PTFE均聚物为实施例1中所用的均聚物。该均聚物分散体与分散体形式的CD090混和，其混和比按聚合物固体计为30％PTFE均聚物和70％CD090。通过机械搅拌使分散体共混物(约含15％的固体)凝结。所得的粉末在50℃的烘箱内干燥几天。取113.4g这种树脂共混物的试样与32.5ml实施例1中所用的润滑剂混和。由鼓转过程混和树脂/润滑剂混合物，然后制成适配于直径0.100英寸孔模的直径1.0英寸的圆柱形预型件。对预型件进行挤塑，所得挤塑物在230℃下干燥25分钟。选择2英寸的挤塑物在300℃下以25∶1进行膨胀，膨胀速率为每秒100％原始长度。膨胀的垫条(beading)含有非常长的原纤和跨越垫条整个横截面的大的结点。结点的分隔是大而且完整得足以切取原纤。将原纤片断合并起来，获得总重为2.8mg的样品。也收集了12.2mg具代表性结点的样品。由差示扫描量热法对这些样品进行分析。在第一步加热时以10℃/分钟从-10℃升至+400℃对样品进行扫描，在冷却时以10℃/分钟从+400℃降至-10℃进行扫描。
各种样品和标准的重结晶能(如Suwa在JAPS17，pp3253-3257(1973)中所讨论的)列于下表中：
    样品 重结晶能(Cal/g)
CD090     8.18
高MW均聚物     5.95
共混物结点组分     7.66
共混物原纤组分     6.17
重结晶能的测量误差为±0.3-0.5cal/g。
在实验误差范围内，重结晶能表明原纤几乎完全是由共混物的高分子量均聚物组分组成的。结点组分的重结晶能表明组分比为77％CD090/23％高MW均聚物。这就指出了结点中的高MW均聚物随着膨胀而减少，高MW均聚物从整体中被选择性地抽出而形成原纤。实施例3
以各种比例将PTFE均聚物分散体(与实施例1中所用的相同)与实施例1中所述的分散体形式的CD090混和。用去离子水稀释混和的分散体，使之含15％的聚合物固体。由机动叶轮搅拌使各种混合物凝结。使各凝结的粉末脱水并在150℃的烘箱内干燥24小时。每种混和粉末各取113.4g的试样与32.5ml实施例1中所用的润滑剂混和，并进行鼓转过程。室温下在装有直径0.100英寸孔模的直径1.00英寸的挤压机料桶中对各种加了润滑剂的粉末进行预成型。以20英寸/分钟的恒定推料杆速率(ram rate)挤压预型件成垫条。在230℃的温度下干燥垫条以除去润滑剂。切割一些短的垫条并在300℃下以16∶1的膨胀比和1000％/秒的膨胀速率进行分批膨胀。如下所述对垫条进行试验。对比实施例A
以各种比例将分散体形式的PTFE均聚物(实施例1中所用的)如实施例1那样与分散体形式的CD1混和。CD1为由ICI生产的低分子量PTFE均聚物，其标准比重为2.191g/cc，分子量为约4,400,000(按Doban方法)。按实施例3对这些共混物进行凝结、脱水和干燥。如实施例3那样将所得的粉末加工成拉伸和膨胀过的垫条。如下所述对垫条进行试验。实施例3和对比实施例A样品的对比试验
由扫描电子显微术检查各段膨胀垫条，将SEM分成六个部分，在每个部分中用钢尺从显微照片中直接测量一根原纤的长度，所选的原纤应能提供所在部分代表性的原纤长度。这些测量的平均值是对微结构粗度的大致量度。这些结果列于表2中。
也对实施例3和对比实施例A的各段膨胀垫条进行高温结构稳定性试验(松弛时间)。将各树脂共混物的膨胀垫条样品夹紧固定，置于390℃的烘箱内。将样品结构破坏(断裂)所需的时间(以秒计)记为“松弛时间”。这些结果列于表2中，并用图表示于图2中。
                              表2
     共   混    组   合    物          性        能
％高MW均聚物 ％CD090   ％CD1 原纤长度(um) 松弛时间(秒)
    100     0     50     493
    60     40     124     431
    40     60     114     354
    20     80     192     257
    0     100     322     107
    100     0     50     493
    60     40     106     526
    40     60     286     521
    20     80     1163     349
    0     100     在这些条件下不会膨胀
由上可见，在实施例3的样品中，改性聚合物与均聚物的共混比对原纤长度的影响较大，而对松弛时间的影响较小。这就表明，本发明的均聚物/改性聚合物PTFE共混物可用于制造含非常大结点和长原纤的经拉伸的PTFE制品，并且可在不损失结构完整性的情况下在远高于PTFE结晶熔点的温度下进行加工。
对于对比例A的样品，该均聚物/均聚物PTFE共混物在原纤长度和松弛时间之间显示出线性关系。当共混比发生变化时，可观察到原纤长度小的变化，而相应的松弛时间的变化非常大。这类树脂共混物作为制造大结点、长原纤结构的用处非常小，原因是它们不具有高温结构稳定性。由这类树脂制成的粗的微结构制品不可能在不显著损失结构完整性的情况下进行烧结以稳定其微结构。

Claims (10)

1.一种由原纤互相连接的结点组成微结构的经拉伸的多孔聚四氟乙烯材料，该材料包含两种不同聚合物的混合物，一种聚合物是聚四氟乙烯均聚物，另一种聚合物是改性的聚四氟乙烯聚合物。
2.如权利要求1所述的材料，其中聚四氟乙烯均聚物与改性聚四氟乙烯聚合物的重量比为90/10-10/90。
3.如权利要求1所述的材料，其中聚四氟乙烯均聚物与改性聚四氟乙烯聚合物的重量比为50/50-20/80。
4.如权利要求1，2或3所述的材料，它以带、长丝、膜、棒或管的形式存在。
5.如权利要求1所述的材料，其中均聚物主要存在于原纤中，改性聚四氟乙烯主要存在于结点中。
6.如权利要求1所述的材料，其中材料的松弛时间大于200秒。
7.如权利要求1所述的材料，其中平均原纤长度大于100μm。
8.如权利要求1所述的材料，其中粗度因子大于0.60(g/cc)/psi。
9.一种制造多孔聚四氟乙烯材料的方法，它依次包括下述步骤：
(a)制备聚四氟乙烯均聚物和改性聚四氟乙烯聚合物的水分散体；
(b)使固体从分散体中凝结；
(c)润滑并糊料挤压凝结的材料；和
(d)拉伸材料。
10.如权利要求9所述的方法，其中随后对拉伸过的材料进行热处理。
CN94195073.5A 1994-09-02 1994-10-14 多孔聚四氟乙烯组合物 Pending CN1145600A (zh)

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CA2183350C (en) 1999-04-27
DE69428056D1 (de) 2001-09-27
EP0777567B1 (en) 2001-08-22
JPH10505378A (ja) 1998-05-26
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