CN1646621A - 超高分子量聚乙烯制品和制造方法 - Google Patents

超高分子量聚乙烯制品和制造方法 Download PDF

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CN1646621A
CN1646621A CNA038082624A CN03808262A CN1646621A CN 1646621 A CN1646621 A CN 1646621A CN A038082624 A CNA038082624 A CN A038082624A CN 03808262 A CN03808262 A CN 03808262A CN 1646621 A CN1646621 A CN 1646621A
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CN100491454C (zh
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J·G·维利兹
K·J·惠尔
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Daramic LLC
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    • B29K2023/00—Use of polyalkenes or derivatives thereof as moulding material
    • B29K2023/04—Polymers of ethylene
    • B29K2023/06—PE, i.e. polyethylene
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
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    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
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Abstract

制造的制品包括与加工油和润滑剂混合的超高分子量聚乙烯(UHMWPE)，所述润滑剂选自脂肪酸酯、乙氧化脂肪酸酯、二元醇酯、PEG酯、甘油酯、乙氧化酯、山梨醇酯、乙氧化山梨醇酯、芳族乙氧化物、脂肪醇乙氧化物、硫醇乙氧化物、改性乙氧化物、酰胺表面活性剂、磷酸酯、膦酸酯、亚磷酸酯、烷基硫酸盐、脂肪酸醚、烷基醚硫酸盐、烷芳基醚硫酸盐、磺酸盐、萘磺酸盐、磺基琥珀酸盐、磺化酯、磺化酰胺、烷基醚羧酸盐、烷芳基醚羧酸盐、季胺、氨基季胺、乙氧化胺、咪唑啉衍生物、甜菜碱、磺基甜菜碱、氨基丙酸盐、儿茶酚衍生物、饱和脂肪酸、不饱和脂肪酸及其结合。还公开了制造那些制品的方法。

Description

超高分子量聚乙烯制品和制造方法
发明领域
本发明涉及超高分子量聚乙烯(UHMWPE)制品及其制造方法。
发明背景
UHMWPE难以加工，这是因为该树脂当熔化时不流动。Berins，M.L.，编辑，Plastics Engineering Handbook of the Society of the PlasticIndustry，Chapman & Hall，New York City，NY(1991)，p52。因此，通过烧结、压塑、活塞式挤塑或凝胶处理，来加工UHMWPE。烧结是其中通过固态扩散使树脂聚集的方法，热和压力通常重要。压塑是其中藉助热和压力，在模具的表面之间使树脂成型的方法。活塞式挤塑是其中通过使树脂受力经过模头，从而使树脂成型的方法，通过活塞提供外力。美国专利Nos.5234652和5399308公开了由树脂和润滑剂组成的混合物的干燥挤塑方法。凝胶处理是其中将树脂成形为凝胶供随后加工的方法。凝胶是树脂在溶剂，例如可萃取溶剂(或油或增塑剂)内的稀溶液或悬浮液。
UHMWPE是纺丝成纤维的凝胶。在凝胶纺丝中，硬化的主要机理是通过冷却，聚合物溶液胶凝，形成由沉淀聚合物和溶剂组成的凝胶长丝。在硬化之后，接着通过在液体浴中洗涤完成溶剂的除去。该方法也用于形成微孔膜。参见美国专利Nos.4588633和5248461。在美国专利No.4588633中，凝胶溶液由2-4％重量UHMWPE组成，参见实施例1-12。在美国专利No.5248461中，凝胶溶液由最多20％重量UHMWPE组成，参见实施例1-20。这些膜尤其用作电化学电池用隔板，参见美国专利Nos.4588633，第4栏第30-36行，和5248461，第4栏第57-60行。
凝胶加工的另一变通方案是采用填料的凝胶加工。例如，参见美国专利Nos.3351495、4833172和5948557。一般地，在挤塑机内混合UHMWPE、加工油(或增塑剂)和填料，随后制成微孔片材。在美国专利No.3351459中，溶液由最多20％体积UHMWPE组成，参见实施例6、8、18、19、20和21。所形成的微孔膜用作电池隔板，参见第1栏第24-33行。在美国专利Nos.4833172和5948557中，将硬脂酸钙/锌润滑剂，PETRACCZ-81加入到溶液中，分别参见表1和2。所形成的微孔膜用作标签、扩散膜和隔板，参见美国专利No.5948557，第1栏第27-41行。
需要改进UHMWPE的加工性。
发明概述
制造的制品包括与加工油和润滑剂混合的超高分子量聚乙烯(UHMWPE)，所述润滑剂选自脂肪酸酯、乙氧化脂肪酸酯、二元醇酯、PEG酯、甘油酯、乙氧化酯、山梨醇酯、乙氧化山梨醇酯、芳族乙氧化物、脂肪醇乙氧化物、硫醇乙氧化物、改性乙氧化物、酰胺表面活性剂、磷酸酯、膦酸酯、亚磷酸酯、烷基硫酸盐、脂肪酸醚、烷基醚硫酸盐、烷芳基醚硫酸盐、磺酸盐、萘磺酸盐、磺基琥珀酸盐、磺化酯、磺化酰胺、烷基醚羧酸盐、烷芳基醚羧酸盐、季胺、氨基季胺、乙氧化胺、咪唑啉衍生物、甜菜碱、磺基甜菜碱、氨基丙酸盐、儿茶酚衍生物、饱和脂肪酸、不饱和脂肪酸及其结合。还公开了制造这些制品的方法。
发明描述
制造的制品是任何形状的制品。例如，制造的制品可包括，但不限于，薄膜、纤维、片材、板、厚板、棒、杆、坯料和块料。优选通过挤塑方法制造这些制品。这些制品也可以是微孔，例如微孔片材和薄膜。
超高分子量聚乙烯(UHMWPE)是重均分子量大于5×105的聚乙烯聚合物。该聚合物或者是乙烯均聚物或者是含有最多10mol％一种或多种α-烯烃的乙烯共聚物。该聚合物可以是UHMWPE的共混物，其中UHMWPE占共混物的至少50％重量，和余量为其它聚合物，如聚烯烃和合成与天然橡胶。优选的重均分子量大于2×106。最优选的UHMWPE的重均分子量大于5×106。UHMWPE树脂可以以GUR(获自Summit，NJ的TiconaLLC)，STAMYLAN(获自荷兰Geleen的DSM)，UTEC(获自巴西Camacari的Polyailden)，和HI-ZEX Million，LUBMER以及MIPELON(各自获自于日本Tokyo Mitsui Chemical)形式商购。优选GUR 4130(分子量为约4-5百万)和GUR 4170(分子量为约8-9百万)。
加工油(或加工增塑剂)在较低温度(例如60℃)下对UHMWPE具有很少的溶剂化效果，但在升高的温度(例如200℃)下具有显著的溶剂化效果。这种油包括石蜡油、萘油和芳烃油，以及包括邻苯二甲酸酯增塑剂如邻苯二甲酸二丁酯、邻苯二甲酸二双(2-亚乙酯)、邻苯二甲酸二异癸酯、邻苯二甲酸二环己酯、邻苯二甲酸丁基苄酯和邻苯二甲酸双十三烷酯在内的其它物质。在美国专利Nos.3351495、4588633、4833172、5248461和5948557中提及了额外的油、增塑剂和/或溶剂，在此通过参考将其引入。
填料包括本领域公知的任何粒状填料，例如，参见美国专利Nos.3351495、4833172和5948557，在此通过参考将其中的每一篇引入。优选填料是氧化硅。这种填料以商标HiSil商购于PA，Pittsburgh的PPG Industries，Inc.、以SIPERANT商购于德国，Wesseling的DegussaAG，以ZEOSIL商购于Cranberry，NJ的Rhodia，Inc.，或以KETJENSIL商购于法国Compiegne的Akzo Chemie。
可以添加小量辅助组分。这种辅助组分包括炭黑、稳定剂和抗氧剂。这些化合物是常规的且本领域已知的。
润滑剂是当添加到UHMWPE混合物中时改进UHMWPE混合物加工性的化合物。改进的加工性是指熔化时间(聚合物体系熔融(或溶解)成可流动溶液所花费的时间)下降。也可从发动机能耗的下降和从当比较添加和不添加润滑剂的体系的混合物温度的下降中看出改进的加工性。来自于这一现象的结果包括，但不限于，降低的能耗，聚合物降低的热和机械降解，增加的聚合物强度，降低的机械磨耗和增加的聚合物产量。
这种润滑剂选自由下述组成的材料组：脂肪酸酯、乙氧化脂肪酸酯、二元醇酯、PEG酯、甘油酯、乙氧化酯、山梨醇酯、乙氧化山梨醇酯、芳族乙氧化物、脂肪醇乙氧化物、硫醇乙氧化物、改性乙氧化物、酰胺表面活性剂、磷酸酯、膦酸酯、亚磷酸酯、烷基硫酸盐、脂肪酸醚、烷基醚硫酸盐、烷芳基醚硫酸盐、磺酸盐、萘磺酸盐、磺基琥珀酸盐、磺化酯、磺化酰胺、烷基醚羧酸盐、烷芳基醚羧酸盐、季胺、氨基季胺、乙氧化胺、咪唑啉衍生物、甜菜碱、磺基甜菜碱、氨基丙酸盐、儿茶酚衍生物、饱和脂肪酸、不饱和脂肪酸及其结合。优选润滑剂选自由下述组成的材料组：脂肪酸酯、乙氧化脂肪酸酯、PEG酯、甘油酯、乙氧化酯、山梨醇酯、乙氧化山梨醇酯、芳族乙氧化物、脂肪醇乙氧化物、磷酸酯、膦酸酯、亚磷酸酯及其结合。最优选山梨醇酯、乙氧化山梨醇酯和芳族乙氧化物。
这种润滑剂是可商购的。下表列出了例举的明细表。这种润滑剂特别地排除硬脂酸的金属盐(例如硬脂酸锌和硬脂酸钙)和包含它们的润滑剂。
表
商标或简称 表面活性剂的原则分类 具体化学物质 公司
RhodasurfLA-12 脂肪醇乙氧化物 混合线性脂肪醇乙氧化物 RhodiaHPCII
RhodasurfLA-3 脂肪醇乙氧化物 混合线性脂肪醇乙氧化物 RhodiaHPCII
RhodapexCD-128 烷基(和烷芳基)醚硫酸盐 线性醇醚硫酸铵 RhodiaHPCII
RhodaponBOS 烷基硫酸盐 2-乙基己基硫酸钠 RhodiaHPCII
RhodaponUB 烷基硫酸盐 月桂基硫酸钠 RhodiaHPCII
AlkamideSTEDA/B 酰胺表面活性剂 亚乙基双硬脂酰胺 RhodiaHPCII
IgepalCO-210 芳族乙氧化物 壬基酚乙氧化物 RhodiaHPCII
IgepalCO-630 芳族乙氧化物 壬基酚乙氧化物 RhodiaHPCII
IgepalRC-630 芳族乙氧化物 十二烷基酚乙氧化物 RhodiaHPCII
MirataineCBS 甜菜碱，磺基甜菜碱，和氨基丙酸盐 椰油/油酰胺丙基甜菜碱 RhodiaHPCII
表(续)
MirataineCOB 甜菜碱，磺基甜菜碱，和氨基丙酸盐 椰油酰胺丙基羟基甜菜碱 RhodiaHPCII
MiranateLEC-80 醚羧酸盐 Laureth 13羧酸钠 RhodiaHPCII
RhodameenPN-430 乙氧化脂肪胺 乙氧化(5mol)牛油胺 RhodiaHPCII
RhodameenT-50 乙氧化脂肪胺 乙氧化(50mol)牛油胺 RhodiaHPCII
硬脂酸钙 饱和脂肪酸 硬脂酸钙
亚麻子油 不饱和脂肪酸 亚油酸和亚麻酸 HardwareStore
桐油 不饱和脂肪酸 桐酸 HardwareStore
AlkamulsGMS 甘油酯 硬脂酸甘油酯 RhodiaHPCII
Kemester1000 三油酸甘油酯 三油酸甘油酯 CromptonCorp.
AlkamulsEGDS 二元醇酯 二硬脂酸甘油酯 RhodiaHPCII
AlkamulsJK Guerbet酯 Guerbet二酯 RhodiaHPCII
Neustrene059 氢化牛油甘油 (30％棕榈酸，60％硬脂酸) CromptonCorp.
Neustrene064 氢化牛油甘油 (88％硬脂酸，10％棕榈酸) CromptonCorp.
MiranolC2M-SF 咪唑啉衍生物 椰油两性(cocoampho)二丙酸二钠 RhodiaHPCII
MiranolJEM 咪唑啉衍生物 混合C8两性羧酸钠 RhodiaHPCII
Antarox724/P 乙氧化物 RhodiaHPCII
RhodacalN 萘甲醛磺酸盐 萘甲醛磺酸钠 RhodiaHPCII
SupragilTMWP 萘磺酸盐 二异丙基萘磺酸钠 RhodiaHPCII
AlkamulsEL-620 PEG酯 PEG-30蓖麻油(蓖麻油酸+油酸+棕榈酸...) RhodiaHPCII
表(续)
Duraphos2EHAPO4 磷酸酯 磷酸，单和二(2-乙基己基)酯 RhodiaHPCII
DEHPA萃取剂 磷酸酯 磷酸，双(2-乙基己基)酯 RhodiaHPCII
RhodafacLO-11ALA 磷酸酯 磷酸，线性辛基/癸基醇酯的共混物 RhodiaHPCII
AmgardTOF 磷酸酯 磷酸，三(2-乙基己酯)酯 RhodiaHPCII
AlbriteB(2EH)2EHP 膦酸酯 膦酸，(2-乙基己基)双(2-乙基己基)酯 RhodiaHPCII
辛基膦酸 膦酸酯 辛基膦酸酯 RhodiaHPCII
RhodaquatDAET-90 季胺 复合二牛油硫酸盐季胺 RhodiaHPCII
AlkamulsSML 脱水山梨醇酯 单月桂酸脱水山梨醇酯 RhodiaHPCII
AlkamulsSMO 脱水山梨醇酯 单月桂酸脱水山梨醇酯 RhodiaHPCII
AlkamulsSTO 乙氧化脱水山梨醇酯 三油酸脱水山梨醇酯 RhodiaHPCII
OT-75，OT-100 磺基琥珀酸盐 二辛基磺基琥珀酸钠 Cytec
混合各组分，UHMWPE，填料(任选)，加工油和润滑剂。在含填料的配方中，聚合物对填料的重量比范围可以是1∶1到1∶5，其中优选1∶3。UHMWPE和填料对油之比的范围可以是1∶1到1∶2，其中优选1∶1.5。润滑剂可最多占配方重量的15％，其中优选0.2-8％。在不含填料的配方中，聚合物可最多占混合物重量的80％，优选在20-65％范围内。油对润滑剂之比的范围可以是3∶1到1∶3，其中优选2∶1到1∶2的范围。优选以连续的方式，例如在双螺杆挤出机中或在Brabender挤塑机或具有吹膜模头的螺杆挤出机内混合各组分。
在混合之后，使混合物成型。成型取决于所需的特定制品，这是本领域公知的。例如，若希望膜或片材，则可将合适的模头添加到挤塑机上。在成型之后，最经常地使制品经历从制品(凝胶)中除去加工油或溶剂的步骤(例如萃取(或洗涤或漂白)步骤，以除去加工油和润滑剂)。这一步骤是方便的。例如，参见美国专利Nos.3351495、4588633、4833172、5248461和5948557，在此通过参考将其中的每一篇引入。在含有填料的配方中，挤塑片材优选经历萃取步骤以除去加工油。在萃取之后，这些片材可具有约0.5％(标称0％)-30％重量残留的油，优选5-25％，和最优选10-20％。应当理解，不可能从任何混合物中除去全部加工油和润滑剂，结果至少痕量将残留在最终制品内。在不含填料的配方中，挤塑片材优选经历萃取步骤。在萃取之后，这些片材可仅具有残留含量的油和润滑剂。可在萃取之前、之中或之后使制品经历拉伸或拉幅。
优选这些制品成形为微孔片材或薄膜。这种微孔片材和薄膜可用作标签、扩散膜和在电化学器件(如电池、电容器和燃料电池)内的隔板。电池是一种电化学器件，它具有阳极、阴极、电解质和夹在该阳极与阴极之间并用电解质浸渍的隔板。含有填料的配方优选用于铅酸电池内。不含填料的配方优选用于锂电池内。
实施例
在表1-8列出的下述实施例中，一起共混超高分子量聚乙烯(GUR4130和GUR 4170，获自Summit，NJ的Ticona LLC)、填料(具体地氧化硅，HiSil，获自Pittsburgh，PA的PPG)、加工油(萘油，获自Princeton，LA的Calumet Co.)，和润滑剂(表内所指的润滑剂)，并从双螺杆挤出机中挤塑。挤塑产品，片材经历萃取步骤，以除去加工油。在挤塑过程中，测量扭矩(％KW)和熔体温度，为的是与对照组(不含添加剂的实施例)比较，并表明混合各组分所需的能量大小。在萃取之后，通过萃取技术测定制造的制品中残留的油量(最终的油％)，其中称取干燥的1.33英寸(3.38cm)×6英寸(15.24cm)的一块片材(W1)，然后在超声浴中，浸渍在200ml新鲜室温己烷中至少15分钟；然后干燥样品并再称重(W2)。％油为[(W1-W2)/W1]*100。取两个样品的平均。另外，以常规方式测量基重，和使用获自Circle Pines，MN的Palico仪器有限公司的常规测试仪，通过ASTM D 374测量厚度，通过ASTM D 638测量MD拉伸，通过国际电池协会(BCI)TM-3.207，测量孔隙度，和通过BCITM-3.218，测量ER。穿孔强度通常遵循ASTM D3763，除了以下所述的以外：所使用的仪器是基于电动试验标准(stand)TCM 201的Chatillon数字式外力测量仪DFIS 10。Chatillon/Ametek位于Largo，FL。孔尖略圆且直径为1.930mm，和平台空穴直径为6.5mm。移动速度设定为300mm/min，和在样品的代表性区域上至少平均10次测量。该方法通常与样品尺寸无关，和样品的代表性区域是指在合理大小的样品上的宽度与长度。以单位N或1bs记录击穿样品所需的峰值外力。
在表1-5中，在挤出机的进料口处混合各成分，和在表6-8中，在挤塑机的机筒中混合润滑剂。
表1
实施例 1 2 3 4 5 6 7 8
添加剂名称 A B C D E F G
聚合物类型 4170 4170 4170 4170 4170 4170 4170 4170
聚合物 Kg 4.14 4.14 4.14 4.14 4.14 4.14 4.14 4.14
填料 Kg 10.76 10.76 10.76 10.76 10.76 10.76 10.76 10.76
添加剂 Kg 0.00 1.09 1.09 1.09 1.09 1.09 1.09 1.09
油 Kg 27.50 26.41 26.41 26.41 26.41 26.41 26.41 26.41
扭矩 ％KW 26 24 25 27 24 25 26 24
熔体温度 ℃ 210 214 214 216 208 268 208 212
料片厚度 微米 189.2 217.2 220.0 209.8 208.0 206.2 205.5 203.2
基重 g/m2 106.9 140.0 140.9 127.1 134.1 129.4 134.0 127.0
穿孔 N 11.9 24.3 23.6 24.2 17.8 20.0 19.2 16.8
MD拉伸 N/mm2 17.5 28.9 29.1 29.3 27.3 21.9 26.4 21.6
孔隙度 ％ 63.1 60.2 60.1 61.9 65.6 63.2 59.0 61.1
ER w/o涂层 mohm-cm2 582.6 285.2 279.4 285.2 385.2 505.8 705.8 541.3
最终的油 ％ 18.2 13.9 14.1 15.2 14.9 16.7 14.5 19.7
表2
实施例 9 10 11 12 13 14 15 16
  添加剂名称   A   B   C   D   E   F   G
  聚合物类型   4130   4130   4130   4130   4130   4130   4130   4130
  聚合物   Kg   4.14   4.14   4.14   4.14   4.14   4.14   4.14   4.14
  填料   Kg   10.76   10.76   10.76   10.76   10.76   10.76   10.76   10.76
  添加剂   Kg   0.00   1.09   1.09   1.09   1.09   1.09   1.09   1.09
  油   Kg   27.50   26.41   26.41   26.41   26.41   26.41   26.41   26.41
  扭矩   ％KW   28   24   26   27   25   28   25   26
  熔体温度   ℃   207   211   214   214   203   216   214   221
  料片厚度   微米   179.1   232.2   227.3   211.3   172.0   209.6   202.4   229.4
  基重   g/m2   106.6   147.8   139.9   131.8   112.9   135.3   132.1   144.7
  穿孔   N   11.8   20.4   21.0   17.0   14.2   16.6   15.9   14.8
  MD拉伸   N/mm2   18.3   24.8   21.9   23.1   21.9   19.1   22.6   16.9
  孔隙度   ％   67.2   60.7   63.7   63.0   61.6   63.6   60.6   62.2
  ER w/o涂层   mohm-cm2   461.3   240.0   263.2   283.2   163.2   361.3   362.6   471.6
  最终的油   ％   23.8   13.4   15.6   13.7   22.8   14.7   14.3   13.7
表3
实施例 17  18  19  20  21  22
添加剂名称  A  B  C  F  H
聚合物类型 4170  4170  4170  4170  4170  4170
聚合物 Kg 3.10  3.10  3.10  3.10  3.10  3.10
填料 Kg 8.41  8.41  8.41  8.41  8.41  8.41
添加剂 Kg 0.00  0.82  0.82  0.82  0.82  0.82
油 Kg 20.35  19.52  19.52  19.52  19.52  19.52
扭矩 ％KW 27  24  24  24  26  22
熔体温度 ℃ 208  211  210  211  210  208
料片厚度 微米 173.0  161.5  177.8  180.1  177.8  191.3
基重 g/m2 111.7  119.6  107.3  123.5  126.3  140.3
穿孔 N 11.4  16.2  13.6  16.0  13.2  20.3
MD拉伸 N/mm2 20.3  34.5  18.4  24.2  20.6  26.5
孔隙度 ％ 59.2  58.1  59.7  60.7  59.7  59.1
ER w/o涂层 mohm-cm2 434.8  127.7  145.8  248.4  435.5  76.1
最终的油 ％ 14.0  13.7  13.9  13.7  12.9  12.8
表4
实施例 17  23  24  25  40
添加剂名称  A  H  A
聚合物类型 4170  4130  4170  4170  4170
聚合物 Kg 3.10  3.10  2.87  2.87  4.39
填料 Kg 8.41  8.41  9.20  9.20  11.86
添加剂 Kg 0.00  0.82  1.63  1.63  1.12
油 Kg 20.35  20.35  18.78  18.78  26.99
扭矩 ％KW 27  24  23  23  23
熔体温度 ℃ 208  209  211  208  216
料片厚度 微米 173.0  177.8  180.3  172.7  114.3
基重 g/m2 111.7  113.3  135.4  137.4  83.8
穿孔 N 11.4  10.1  13.5  17.5  11.4
MD拉伸 N/mm2 20.3  16.9  21.6  32.8  27.1
孔隙度 ％ 59.2  62.3  59.0  58.5  65.5
ER w/o涂层 mohm-cm2 434.8  464.5  78.1  64.5  36.1
最终的油 ％ 14.0  14.6  12.5  11.6  14.7
表5
实施例 26 31 27 28 29 30
添加剂名称 I J K K
聚合物类型 4130 4170 4170 4170 4170 4170
聚合物 Kg 3.10 4.39 3.10 3.10 4.34 3.25
填料 Kg 8.41 11.86 8.41 8.41 11.75 8.81
添加剂 Kg 0.00 0.00 0.82 0.82 0.53 0.82
油 Kg 20.35 28.66 19.52 19.52 27.86 20.48
扭矩 ％KW 28 23 23 24 25
熔体温度 ℃ 217 217 222 227
料片厚度 微米 188.5 183.4 192.8 179.6 198.9 191.5
基重 g/m2 100.1 102.4 117.9 127.2 114.6 116.7
穿孔 N 9.6 13.1 16.8 22.0 11.5 12.8
MD拉伸 N/mm2 15.6 20.4 28.4 33.2 12.8 12.5
孔隙度 ％ 63.0 66.3 62.5 61.1 66.2 65.9
ER w/o涂层 mohm-cm2 320.3 221.9 109.8 397.4 292.3 220.0
最终的油 ％ 13.7 10.9 11.2 11.5 11.9 12.5
表6
实施例 31  32  33  34  35  41
添加剂名称  J  J  J  J  J
聚合物类型 4170  4170  4170  4170  4170  4170
聚合物 Kg 4.39  4.39  4.39  4.39  4.39  3.35
填料 Kg 11.86  11.86  11.86  11.86  11.86  9.04
添加剂 Kg 0.00  0.55  1.12  2.32  3.59  1.63
油 Kg 28.66  27.83  26.99  25.25  23.42  23.59
扭矩 ％KW 28  28  26  24  25  24
熔体温度 ℃ 217  210  207  205  204  204
料片厚度 微米 183.4  175.3  182.9  162.6  170.2  182.9
基重 g/m2 102.4  119.2  122.2  126.0  141.2  118.5
穿孔 N 13.1  15.2  20.8  22.5  24.5  17.1
MD拉伸 N/mm2 20.4  24.3  38.2  48.8  48.5  22.1
孔隙度 ％ 66.3  65.3  61.4  58.1  57.0  61.1
ER w/o涂层 mohm-cm2 221.9  198.7  282.6  1052.9  751.6  543.9
最终的油 ％ 10.9  12.8  12.5  13.9  13.3  13.8
表7
实施例 31  36  37  38  39
添加剂名称  H  H  H  H
聚合物类型 4170  4170  4170  4170  4170
聚合物 Kg 4.39  4.39  4.39  4.39  4.39
填料 Kg 11.86  11.86  11.86  11.86  11.86
添加剂 Kg 0.00  0.55  1.12  2.32  3.59
油 Kg 28.66  27.83  26.99  25.25  23.42
扭矩 ％KW 28  25  24  26  27
熔体温度 ℃ 217  213  201  200  204
料片厚度 微米 183.4  170.2  182.9  183.6  167.6
基重 g/m2 102.4  108.2  152.2  145.4  156.4
穿孔 N 13.1  12.9  22.5  16.4  14.8
MD拉伸 N/mm2 20.4  21.3  46.7  38.3  33.4
孔隙度 ％ 66.3  64.4  61.2  61.1  57.0
ER w/o涂层 mohm-cm2 221.9  46.5  223.9  593.5  150.3
最终的油 ％ 10.9  14.1  12.9  13.8  12.5
表8
实施例 49 42 43 44 45 46 47 48
    添加剂名称     L     M     N     O     P     Q     R
    聚合物类型     4170     4170     4170     4170     4170     4170     4170     4170
    聚合物     Kg     3.25     3.25     3.25     3.25     3.25     3.25     3.25     3.25
    填料     Kg     8.79     8.79     8.79     8.79     8.79     8.79     8.79     8.79
    添加剂     Kg     0.00     0.82     0.82     0.82     0.82     0.82     0.82     0.82
    油     Kg     21.27     20.34     20.34     20.34     20.34     20.34     20.34     20.34
    扭矩     ％KW     24     24     24     24     23     24     23     24
    熔体温度     ℃     227     234     233     236     235     234     234     237
    料片厚度     微米     157.5     177.8     167.6     175.3     185.4     162.6     180.3     175.3
    基重     g/m2     110.6     126.3     120.0     125.0     129.4     119.4     119.4     125.6
    穿孔     N     10.6     18.5     15.9     18.5     16.4     17.5     13.8     17.4
    MD拉伸     N/mm2     16.3     34.8     31.9     45.7     31.6     35.8     33.1     35.8
    孔隙度     ％     64.5     61.6     62.5     63.0     63.4     61.7     63.0     63.7
    ER w/o涂层     mohm-cm2     470.3     872.9     1707.1     201.3     376.1     225.2     294.8     19.4
    最终的油     ％     13.6     12.5     12.7     14.3     14.0     14.8     15.5     14.3
在下表9列出的下述实施例中，一起共混超高分子量聚乙烯(GUR4130，获自Summit，NJ的Ticona.LLC)、加工油(萘油，获自Princeton，LA的Calumet Co.)，和润滑剂(表内所指的润滑剂)，并从双螺杆挤出机中挤塑。当它挤出挤塑机模头时，观察挤塑产品并根据外观等级1-10分类。评定为10是指看起来均匀混合的光滑产品，和评定为1是指非常多颗粒且粗糙的外观。
表9
实施例 46 47 48 49 50 51 52 53 54 55
  聚合物wt％   33.0   38.5   52.9   38.5   52.2   50.0   45.0   61.0   25.0   65.0
  油wt％   33.0   46.1   17.7   38.5   23.9   35.0   20.0   14.0   50.0   12.7
  添加剂wt％   33.0   15.4   29.4   23.0   23.9   15.0   35.0   25.0   25.0   22.3
  添加剂名称   J   J   J   J   J   J   J   J   J   J
  肉眼评定   5   6   8   8   9   4   1   10   10   4
A＝磷酸酯；脂肪醇共混物磷酸酯；Rhodafac LO-11A LA，获自Cranberry，NJ的Rhodia HPCII
B＝磷酸酯；双(2-乙基己基)磷酸酯，获自Cranberry，NJ的RhodiaHPCII
C＝磷酸酯；双(2-乙基己基)磷酸酯+单(2-乙基己基)磷酸酯，获自Cranberry，NJ的Rhodia HPCII
D＝磷酸酯；2-乙基己基双(2-乙基己基)磷酸酯，获自Cranberry，NJ的Rhodia HPCII
E＝磷酸酯；三(2-乙基己基)磷酸酯，获自Cranberry，NJ的RhodiaHPCII
F＝不饱和脂肪酸；亚油酸和亚麻酸；亚麻子油
G＝不饱和脂肪酸；桐酸；桐油
H＝膦酸酯；辛基膦酸酯，获自Cranberry，NJ的Rhodia HPCII
I＝PEG酯；PEG-30蓖麻油(蓖麻油酸+油酸+棕榈酸...)；Alkamuls EL-620，获自Cranberry，NJ的Rhodia HPCII
J＝脱水山梨醇酯；单油酸脱水山梨醇酯；Alkamuls SMO，获自Cranberry，NJ的Rhodia HPCII
K＝磺基琥珀酸酯；二辛基磺基琥珀酸钠；OT-100，获自Charlotte，NC的Cytec Industries
L＝脱水山梨醇酯；单月桂酸脱水山梨醇酯；Alkamuls SML，获自Cranberry，NJ的Rhodia HPCII
M＝乙氧化脱水山梨醇酯；三油酸脱水山梨醇酯；Alkamuls STO，获自Cranberry，NJ的Rhodia HPCII
N＝芳族乙氧化物；十二烷基酚乙氧化物；1gepal RC-630，获自Cranberry，NJ的Rhodia HPCII
O＝芳族乙氧化物；壬基酚乙氧化物；1gepal CO-210，获自Cranberry，NJ的Rhodia HPCII
P＝芳族乙氧化物；壬基酚乙氧化物；1gepal CO-630，获自Cranberry，NJ的Rhodia HPCII
Q＝脂肪醇乙氧化物；混合线性脂肪醇乙氧化物；Rhodasturf LA-3，获自Cranberry，NJ的Rhodia HPCII
R＝脂肪醇乙氧化物；混合线性脂肪醇乙氧化物；Rhodasurf LA-12，获自Cranberry，NJ的Rhodia HPCII
在下表10列出的下述实施例中，一起共混超高分子量聚乙烯(GUR4170，获自Ticona LLC，Summit，NJ)、填料(氧化硅，HiSil，获自Pittsburgh，PA的PPG)、加工油(萘油，获自Pamaton，LA的CalumetCo.)，和润滑剂(表内所指的润滑剂)，并从Brabender挤塑机(SouthHackensack，NJ的BW Brabender Co.)中挤塑。在对照组中，将5.42gUHMWPE与14.65g填料和30.56g油混合。在另一实施例中，将5.42gUHMWPE与14.65g填料，29.06g油和1.50g润滑剂混合。使用该方法，通过观察熔化时间和最终扭矩来预计润滑剂的效率。熔化时间是当聚合物溶解在油内(聚合物的相反转)时的量度。熔化时间典型地是扭矩作为时间函数所作图上的第二峰值。熔化时间典型地在表示聚合物被油润湿时的第一峰值后出现。在混合10分钟之后测量最终扭矩。
表10
添加剂 熔化时间(秒) 最终扭矩(mg) 平均穿孔(N)
对照组-59％油  149  576.3  11
对照组-62％  105  552  10.5
Octyl PO4  43  501  18
Antarox 724/P  106  666
Alkamide STEDA/B  108  918.5
Rhodasurf LA-12  69  598  18
T(2EH)PO4  64  640  17
Alkamuls SMO  42  668.5  22
Igepal CO-630  41  587.5  18
Alkamuls STO  108  590.3  16
Alkamuls SML  125  643  18.5
Rhodasurf LA-3  42  614  14
Alkamuls EL-620  149  690.5  17
Igepal CO-210  52  638  16.5
Igepal RC-630  41  635.5  17.5
亚麻子油  103  679.5  13
B(2EH)2EHP1  92  610  15
2EHAPO4  95  465  16
DEHPA  100  410  15
Rhodafac LO-11A  109  516  16
Rhodapon BOS  126  578.5
桐油  98  638.5  12
OT-75  145  818  12
Rhodapex CD-128  133  598
Miranol C2M-SF  63  631
Mirataine COB  138  760.5
Mirataine CBS  83  750
Miranate LEC-80  118  753
Miranol JEM  149  716.7
Rhodapon UB  125  763.7
Supragil WP  138  708.5
硬脂酸钙  64  570
Rhodacal N  143  739
Neustrene 059  112  662.5
Neustrene 064  122  705.5
Kemester 1000  103  690
RhodaquatDAET-90
Rhodameen PN-430  38  616.5
Rhodameen T-50
Alkamuls GMS  78  616.5
Alkamuls EGDS  99  699.5
A1kamuls JK  126  744.5
Igepal CA-620  51  636.5
Igepal CO-530  64  602.5
Igepal CA-630  68  625.7
硅油1000cP  85  561.5
硅油100cP  90  578.5
硅油500cP  95  557.5
硅油200cP  99  566.5
在没有脱离本发明的精神和主要特征的情况下，可以以其它形式体现本发明，和因此，应当参考表示本发明范围的所附权利要求，而不是前述说明。

Claims (27)

1.一种制造的制品，它包括：
与加工油和润滑剂混合的超高分子量聚乙烯(UHMWPE)，所述润滑剂选自脂肪酸酯、乙氧化脂肪酸酯、二元醇酯、PEG酯、甘油酯、乙氧化酯、山梨醇酯、乙氧化山梨醇酯、芳族乙氧化物、醇乙氧化物、硫醇乙氧化物、改性乙氧化物、酰胺表面活性剂、磷酸酯、膦酸酯、亚磷酸酯、烷基硫酸盐、脂肪酸醚、烷基醚硫酸盐、烷芳基醚硫酸盐、磺酸盐、萘磺酸盐、磺基琥珀酸盐、磺化酯、磺化酰胺、烷基醚羧酸盐、烷芳基醚羧酸盐、季胺、氨基季胺、乙氧化胺、咪唑啉衍生物、甜菜碱、磺基甜菜碱、氨基丙酸盐、儿茶酚衍生物、饱和脂肪酸、不饱和脂肪酸及其结合。
2.权利要求1的制品，其中所述润滑剂选自脂肪酸酯、乙氧化脂肪酸酯、PEG酯、乙氧化酯、山梨醇酯、乙氧化山梨醇酯、芳族乙氧化物、醇乙氧化物、磷酸酯、膦酸酯、亚磷酸酯及其结合。
3.权利要求1的制品，其中所述UHMWPE的分子量大于2×106。
4.权利要求1的制品，其中所述UHMWPE的分子量大于5×106。
5.权利要求1的制品，其中制品是孔隙度大于30％的微孔膜。
6.一种电池隔板，它包括含权利要求1的制品的微孔膜。
7.权利要求6的隔板，其中所述电池是锂电池。
8.一种制造的制品，它包括：
与填料、加工油和润滑剂混合的超高分子量聚乙烯(UHMWPE)，所述润滑剂选自脂肪酸酯、乙氧化脂肪酸酯、二元醇酯、PEG酯、甘油酯、乙氧化酯、山梨醇酯、乙氧化山梨醇酯、芳族乙氧化物、醇乙氧化物、硫醇乙氧化物、改性乙氧化物、酰胺表面活性剂、磷酸酯、膦酸酯、亚磷酸酯、烷基硫酸盐、脂肪酸醚、烷基醚硫酸盐、烷芳基醚硫酸盐、磺酸盐、萘磺酸盐、磺基琥珀酸盐、磺化酯、磺化酰胺、烷基醚羧酸盐、烷芳基醚羧酸盐、季胺、氨基季胺、乙氧化胺、咪唑啉衍生物、甜菜碱、磺基甜菜碱、氨基丙酸盐、儿茶酚衍生物、饱和脂肪酸、不饱和脂肪酸及其结合。
9.权利要求8的制品，其中所述润滑剂选自脂肪酸酯、乙氧化脂肪酸酯、PEG酯、乙氧化酯、山梨醇酯、乙氧化山梨醇酯、芳族乙氧化物、脂肪醇乙氧化物、磷酸酯、膦酸酯、亚磷酸酯及其结合。
10.权利要求8的制品，其中所述超高分子量聚乙烯与所述填料的重量比范围为1∶1到1∶5。
11.权利要求8的制品，其中所述润滑剂占最多15％重量。
12.权利要求8的制品，其中所述超高分子量聚乙烯的分子量大于2×106。
13.一种电池隔板，它包括含权利要求8的制品的微孔膜。
14.权利要求13的隔板，其中所述电池是铅酸电池。
15.一种制造超高分子量聚乙烯(UHMWPE)制品的方法，它包括步骤：
混合超高分子量聚乙烯、加工油和润滑剂，所述润滑剂选自脂肪酸酯、乙氧化脂肪酸酯、二元醇酯、PEG酯、甘油酯、乙氧化酯、山梨醇酯、乙氧化山梨醇酯、芳族乙氧化物、醇乙氧化物、硫醇乙氧化物、改性乙氧化物、酰胺表面活性剂、磷酸酯、膦酸酯、亚磷酸酯、烷基硫酸盐、脂肪酸醚、烷基醚硫酸盐、烷芳基醚硫酸盐、磺酸盐、萘磺酸盐、磺基琥珀酸盐、磺化酯、磺化酰胺、烷基醚羧酸盐、烷芳基醚羧酸盐、季胺、氨基季胺、乙氧化胺、咪唑啉衍生物、甜菜碱、磺基甜菜碱、氨基丙酸盐、儿茶酚衍生物、饱和脂肪酸、不饱和脂肪酸及其结合；和
挤塑所述混合物。
16.权利要求15的方法，进一步包括从所述挤塑混合物中萃取加工油的步骤。
17.权利要求15的方法，其中挤塑进一步包括螺杆挤塑、Brabender挤塑和吹膜挤塑。
18.权利要求15的方法，其中油与润滑剂的重量比范围为3∶1到1∶3。
19.权利要求15的方法，其中UHMWPE占混合物重量的最多80％。
20.权利要求15的方法，其中润滑剂选自脂肪酸酯、乙氧化脂肪酸酯、PEG酯、乙氧化酯、山梨醇酯、乙氧化山梨醇酯、芳族乙氧化物、醇乙氧化物、磷酸酯、膦酸酯、亚磷酸酯及其结合。
21.一种制造超高分子量聚乙烯(UHMWPE)制品的方法，它包括步骤：
混合超高分子量聚乙烯、填料、加工油和润滑剂，所述润滑剂选自脂肪酸酯、乙氧化脂肪酸酯、二元醇酯、PEG酯、甘油酯、乙氧化酯、山梨醇酯、乙氧化山梨醇酯、芳族乙氧化物、醇乙氧化物、硫醇乙氧化物、改性乙氧化物、酰胺表面活性剂、磷酸酯、膦酸酯、亚磷酸酯、烷基硫酸盐、脂肪酸醚、烷基醚硫酸盐、烷芳基醚硫酸盐、磺酸盐、萘磺酸盐、磺基琥珀酸盐、磺化酯、磺化酰胺、烷基醚羧酸盐、烷芳基醚羧酸盐、季胺、氨基季胺、乙氧化胺、咪唑啉衍生物、甜菜碱、磺基甜菜碱、氨基丙酸盐、儿茶酚衍生物、饱和脂肪酸、不饱和脂肪酸及其结合；和
挤塑所述混合物。
22.权利要求21的方法，进一步包括从所述挤塑混合物中萃取加工油的步骤。
23.权利要求21的方法，其中挤塑进一步包括螺杆挤塑、Brabender挤塑和吹膜挤塑。
24.权利要求21的方法，其中UHMWPE与填料的重量比范围为1∶1到1∶5。
25.权利要求21的方法，其中UHMWPE和填料对油的重量比范围为1∶1到1∶2。
26.权利要求21的方法，其中润滑剂选自脂肪酸酯、乙氧化脂肪酸酯、PEG酯、乙氧化酯、山梨醇酯、乙氧化山梨醇酯、芳族乙氧化物、醇乙氧化物、磷酸酯、膦酸酯、亚磷酸酯及其结合。
27.权利要求21的方法，其中润滑剂占混合物重量的最多15％。
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CN106380669A (zh) * 2016-10-18 2017-02-08 赵焕 一种导电pe及其制备方法

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