WO2001000715A1 - Procede de preparation d'un materiau composite a base de polytetrafluoroethylene renforce par des polymeres cristaux liquides - Google Patents

Procede de preparation d'un materiau composite a base de polytetrafluoroethylene renforce par des polymeres cristaux liquides Download PDF

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WO2001000715A1
WO2001000715A1 PCT/CN2000/000175 CN0000175W WO0100715A1 WO 2001000715 A1 WO2001000715 A1 WO 2001000715A1 CN 0000175 W CN0000175 W CN 0000175W WO 0100715 A1 WO0100715 A1 WO 0100715A1
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minutes
liquid crystal
ptfe
crystal polymer
polytetrafluoroethylene
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PCT/CN2000/000175
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English (en)
French (fr)
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Wei Tang
Baoliang Zhu
Jiajun Liu
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Tsinghua University
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Priority to AU55189/00A priority Critical patent/AU5518900A/en
Publication of WO2001000715A1 publication Critical patent/WO2001000715A1/zh

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    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • C08L67/03—Polyesters derived from dicarboxylic acids and dihydroxy compounds the dicarboxylic acids and dihydroxy compounds having the carboxyl- and the hydroxy groups directly linked to aromatic rings

Definitions

  • the invention relates to a method for preparing a liquid crystal polymer reinforced polytetrafluoroethylene composite material, and belongs to the technical field of high molecular materials.
  • Polytetrafluoroethylene (hereinafter referred to as PTFE) is an excellent solid self-lubricating material, but its outstanding disadvantage is that the wear rate is large, and generally it needs to be filled and modified before it can be used as a sealing material. It is common practice to add inorganic fillers such as glass fiber, carbon fiber, tin bronze powder, and molybdenum disulfide. However, these filled modified products still have disadvantages such as poor compatibility of inorganic fillers with polytetrafluoroethylene, low affinity, obvious interfaces in the matrix, difficult to disperse uniformly, and great damage to the parts to be worn.
  • Liquid crystal polymers are unique members of the polymer family with outstanding comprehensive properties. From the application point of view, it can be divided into two categories, namely, lyotropic liquid crystal (LLCP) that forms a liquid crystal phase in the molten state and thermotropic liquid crystal (TLCP) that forms a liquid crystal phase in the molten state.
  • LLCP lyotropic liquid crystal
  • TLCP thermotropic liquid crystal
  • the purpose of the present invention is to study a method for preparing a polytetrafluoroethylene composite material reinforced with liquid crystal polymers.
  • a method for preparing a polytetrafluoroethylene composite material reinforced with liquid crystal polymers On the basis of maintaining the self-lubricating characteristics of polytetrafluoroethylene, its abrasion resistance is greatly improved, making it possible Become the material of choice for high-strength wear-resistant seals.
  • the thermotropic liquid crystal (TLCP) used in the present invention can undergo flow orientation alignment when heated, and forms a microfiber structure reinforcing phase in situ in the internal part of the substrate, thereby achieving the purpose of improving abrasion resistance.
  • the preparation method of the liquid crystal polymer reinforced polytetrafluoroethylene composite material designed by the present invention includes the following steps:
  • the present invention is a filled fluoropolymer-based composite material.
  • the formula is based on 60% ⁇ 90% fluoropolymer as the main component, and 10% ⁇ 30% liquid crystal polymer (LCP) and Glass fiber or calcium carbonate particles with a weight of 0-10%; It should be noted that the weight percentage of the glass fiber or calcium carbonate particles added here is 10% Within, that is, the adverse effect on the workpiece is within a small range, but the effect of improving the wear resistance is not affected, and the cost can be reduced.
  • the liquid crystal polymer described above is an aromatic polyester polymer compound, and its characteristics are one of the following structural units contained in the molecular chain.
  • These liquid crystals are high-heat LCPs with high melting points, which can meet the requirements of blending with PTFE and high-temperature sintering, and have certain compatibility.
  • the liquid crystal polymer is crushed to a particle size of less than 500 ⁇ m using low-temperature grinding. It is an irregular granular powder before use.
  • the low-temperature grinding and pulverization are obtained by cooling with liquid nitrogen, and the purpose is to prevent the physical properties of the liquid crystal from changing, and to impair its advantages of high strength and high temperature resistance.
  • the temperature is then increased by sintering at a rate of about 2 ° C per minute, and the temperature is maintained at 310 ° C ⁇ 320 ° C for 0.5 to 5-1 hours.
  • the temperature is then increased to a temperature of 365 ⁇ 380 ° C at a rate of about 1 ° C per minute. 50 ⁇ 100 minutes, then cooled to 310 ° C ⁇ 320 ° C, constant temperature for 20 ⁇ 30 minutes, and then cooled to room temperature with the furnace to obtain the composite material product of the present invention.
  • Xydar series liquid crystal polymer product B was purchased from Amoco company
  • Vectra series liquid crystal polymer product A was purchased from Tinoca company
  • Zenite series liquid crystal polymer product was purchased from Dupont company (: Fluoropolymer used PTFE suspension resin produced by Jinan Chemical Plant.
  • Example 6 Crush 30% Xydar G900 (ie, 100% B) powder below 150 ⁇ with 70% PTFE and dry at 150 ° C for 9 hours; pressing pressure is 60MPa, hold pressure for 3 minutes, sintering at 310 Constant temperature between ° C ⁇ 320 ° C for 40 minutes, and then rise to 365 ° C for 60 minutes; The cooling phase is constant at 310 ° C ⁇ 320 ° C for 25 minutes, and then the sample is cooled with the furnace to obtain GB3160-83 friction and wear Test, conditions are the same as 1). The results for the coefficient of friction of 0.207, the wear rate of 1. 73 X 10- 6 mmVKg / m ; increased about 287 times higher than the wear resistance of pure PTFE.
  • SGF in the table above stands for short glass fiber
  • LGF stands for long glass fiber
  • Table 2 compares the inverse of the ratio of the wear rate of various experimental materials with the wear rate of pure PTFE under the same experimental conditions as a multiple of the increase in wear resistance, in order to have a clear understanding.
  • the best-working example 2 has an abrasion resistance increase of more than 490 times; and the worst example 4 has an increase of about 170 times.
  • the best effect of ordinary fillers also improves the wear resistance by as much as 32 times.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Description

一种由液晶类聚合物增强的聚四氟乙烯复合材料的制备方法 发明领域
本发明涉及一种 液晶类聚合物增强的聚四氟乙烯复合材料的制备方法，属高分 子材料技术领域。
背景技术
聚四氟乙烯（以下简称 PTFE )是优良的固体自润滑材料，但其突出的缺点是磨损率大， 一般需进行填充改性才可用作密封材料。普遍的作法是在其中填加玻璃纤维、碳纤维、 锡青铜粉、 二硫化钼等无机填料。但这些填充改性制品仍存在无机填料与聚四氟乙烯 相容性差， 亲和力较小， 在基体中出现明显界面， 且不易分散均匀， 对被磨件损伤大 等不足之处。
相对于纯 PTFE而言， 发明人在同样的实验条件下发现， 普通填料改性的方法对 耐磨性提高效果为： 填加 15%的玻璃纤维和 5%的石墨的 PTFE, 其耐磨性提高 23倍， 填加 60%青铜粉的 PTFE, 其耐磨性提高 8倍多， 而改性效果最好的含玻纤、 青铜粉和 石墨混合物的 PTFE复合材料其耐磨性也才提高了 36倍。
液晶聚合物 （LCP) 是聚合物家庭中的独特成员， 具有卓著的综合性能。 从应用 角度來看， 可分为两大类， 即溶化状态下成液晶相的溶致液晶 （LLCP )和在熔融状态 下成液晶相的热致液晶 （TLCP)。 人们已经发现它们在加工过程中由于受到挤出、 注 塑、 拉伸等力的作用， 其分子链中刚性棒状结构会发生高度取向从而极大地起到原位 复合增强作用。 然而很少有研究者尝试用液晶增强模压工艺成型的树脂， 考察在没有 受拉伸、 挤出等力的作用下液晶聚合物的原位增强效果。
发明的公开
本发明的目的是研究一种 ώ液晶类聚合物增强的聚四氟乙烯复合材料的制备方 法， 在保持聚四氟乙烯的自润滑特征基础上， 极大地改善其耐磨性， 使其有可能 成 为高强耐磨密封件的选用材料。 本发明所采用的热致型液晶 （TLCP )在受热的情况下 能发生流动取向排列， 在基体内部部分原位形成微纤结构增强相， 从而达到改善耐磨 性的目的。
本发明设计的 ώ液晶类聚合物增强的聚四氟乙烯复合材料的制备方法，包括以下 各歩骤：
1、 本发明为一种填充型氟聚合物基复合材料， 配方是以重量占 60%~90%的氟聚 合物为主要成份， 加入重量占 10%~30%液晶类聚合物（LCP)和重量占 0~10%的玻璃纤 维或碳酸钙颗粒； 需要说明的是， 此处所加的玻纤或碳酸钙颗粒的重量百分比在 10% 以内， 即对被磨件的不良影响在很小的范围内， 却不影响耐磨性改善的效果， 又能降 低成本。
上述的液晶类聚合物为芳香族聚酯类高分子化合物,其物征是分子链中含的以下 结构单元中的一种。 这些液晶属高热型 LCP,熔点较高， 能满足与 PTFE共混并高温烧 结的要求， 且具有一定的相容性。
A :
Figure imgf000003_0001
并将上述的液晶类聚合物， 应用低温研磨粉碎至小于 500μπι的粒度使用。使用前为不 规则粒状粉末。 低温研磨粉碎用液氮冷却获得， 目的是防止液晶的物性发生变化， 损 害其高强度、 耐高温的优点。
2、将上述机械混合均勾的物料放置于干燥箱内，在 135~150°C下干燥 2~10小时， 取出后进行压制。 缓慢加压至 50~70MPa， 视样品大小保压一段时间预制成型， 一般 为 3— 5分钟；
3、 再以每分钟约 2°C的速度升温烧结， 在 310°C~320°C间恒温 0. 5-1小时； 再 以每分钟 1°C左右的速度升温到 365~380°C恒温 50~100分钟，然后冷却至 310°C~320°C 恒温 20~30分钟， 随炉冷却至室温， 即得本发明的复合材料制品。
具体实施例
下面介绍本发明的实施例：
为进行实验， 分别从 Amoco公司购得 Xydar系列液晶聚合物产品 B, 从 Tinoca公 司购得 Vectra系列液晶聚合物产品 A和从 Dupont公司购得 Zenite系列液晶聚合物 产品 (：。 氟聚合物采用了济南化工厂生产的 PTFE悬浮树脂。
实施例 1 :
将 20%Vectra C550 (50%A+50%矿物颗粒） 粉碎到 100~300μπι的粉料与 80%PTFE 的物料， 在 150°C 下干燥 4 个小时； 压制压力为 70MPa， 保压 3 分钟， 烧结时在 310。C~320。C间恒温 30分钟， 再升至 365°C恒温 70分钟； 冷却阶段在 310°C~320°C 恒温 25分钟， 再随炉冷却即得试样， 进行 GB3160- 83摩擦磨损试验， 载荷为 10Kg， 速度为 200转 /分， 实验进行 2小时。 取 3至 4次实验的平均值。 实验结果为摩擦系 数 0. 192， 磨损率为 1. 92x lO-W/ g/m; 而同样摩擦磨损实验条件下的纯 PTFE的磨 损率为 497X 10—6mmVKg/m。 即本实例的耐磨性提高了 259倍之多。
实施例 2 :
将 20%Vectra C550 ( 50%A+50%矿物颗粒） 粉碎到 ΙΟΟμπι的粉料与 80%PTFE的物 料，在 150°C下干燥 5个小时；压制压力为 65MPa，保压 5分钟，烧结时在 310°C~320°C 间恒温 30分钟， 再升至 365°C恒温 60分钟； 冷却阶段在 310°C~320°C恒温 20分钟， 再随炉冷却即得试样， 进行 GB3160- 83摩擦磨损试验， 条件同 1 )。实验结果为摩擦系 数 0. 204， 磨损率为 1. 01x10— 6mmVKg/m; 比之纯 PTFE的耐磨性提高 490倍左右。
实施例 3:
将 A粉碎到 200μίη以下直径的粉料与 PTFE混合成含 A30%的物料， 在 150°C下干 燥 6个小时；压制压力为 65MPa，保压 5分钟，烧结时在 310°C~320°C间恒温 30分钟， 再升至 365°C恒温 50分钟； 冷却阶段在 310°C~320°C恒温 20分钟， 再随炉冷却即得 试样， 进行 GB3160-83摩擦磨损试验， 条件同 1 )。 实验结果为摩擦系数 0. 196, 磨损 率为 1. 38x l(T¾mVKg/m; 比之纯 PTFE的耐磨性提高 360倍左右。
实施例 4
将 30%的 Xydar G930 (含 70%B和 30%玻璃纤维）粉碎到 100~300μπι的粉料与 70% 的 PTFE混合的物料， 在 150°C下干燥 10个小时； 压制压力为 60MPa， 保压 5分钟， 烧结时在 310°C~320°C 间恒温 45 分钟， 再升至 370°C恒温 80 分钟； 冷却阶段在 310°C~320°C恒温 25分钟， 再随炉冷却即得试样， 进行 GB3160-83摩擦磨损试验， 条 件同 1 )。 实验结果为摩擦系数 0. 224， 磨损率为 2. 92x lO-¾mVKg/m; 比之纯 PTFE的 耐磨性提高约 170倍。
实施例 5:
将 20%Xydar G930 含 70%B和 30%玻璃纤维）粉碎到 ΙΟΟμπι以下的粉料与 80%PTFE 混合的物料， 在 150°C下干燥 8个小时； 压制压力为 60MPa， 保压 4分钟， 烧结时在 310°C~320°C间恒温 50分钟， 再升至 375°C恒温 80分钟； 冷却阶段在 310°C~320°C 恒温 30分钟， 再随炉冷却即得试样， 进行 GB3160-83摩擦磨损试验， 条件同 1 )。 实 验结果为摩擦系数 0. 219， 磨损率为 2. 30x10- 6mm3/Kg/m; 比之纯 PTFE耐磨性提高约 216倍。
实施例 6: 将 30%Xydar G900 (即 100%B )粉碎到 150μιη以下的粉料与 70%PTFE混合的物料， 在 150°C下干燥 9个小时； 压制压力为 60MPa， 保压 3分钟， 烧结时在 310°C~320°C 间恒温 40分钟， 再升至 365°C恒温 60分钟； 冷却阶段在 310°C~320°C恒温 25分钟， 再随炉冷却即得试样， 进行 GB3160-83摩擦磨损试验， 条件同 1 )。 实验结果为摩擦系 数 0. 207， 磨损率为 1. 73X 10—6mmVKg/m; 比之纯 PTFE耐磨性提高约 287倍。
实施例 7:
将 30%Zeni te6130(含 70%C和 30%玻璃纤维）粉碎到 100~300μπι的粉料与 70%PTFE 混合成的物料， 在 135°C下干燥 3个小时； 压制压力为 55MPa， 保压 3分钟， 烧结时 在 310°C~320°C间恒温 60分钟，再升至 380°C恒温 100分钟；冷却阶段在 310°C~320°C 恒温 30分钟， 再随炉冷却即得试样， 进行 GB3160- 83摩擦磨损试验， 条件同 1 )。 实 验结果为摩擦系数 0. 222， 磨损率为 1. 85x 10— 6mmVKg/m; 其耐磨性比纯 PTFE提高了 268倍。
实施例 8:
将 20%Zeni te6130 (含 70%C和 30%玻璃纤维） 粉碎到 300~500μπι的粉料与 PTFE 混合成的物料， 在 135°C下干燥 2个小时； 压制压力为 50MPa， 保压 4分钟， 烧结时 在 310°C~320°C间恒温 60分钟，再升至 380°C恒温 90分钟；冷却阶段在 310°C~320°C 恒温 30分钟， 再随炉冷却即得试样， 进行 GB3160- 83摩擦磨损试验， 条件同 1 )。 实 验结果为摩擦系数 0. 228， 磨损率为 1. 52x l(T6mraVKg/m; 其耐磨性比纯 PTFE提高了 327倍。
为便于对比， 在同样的实验条件下， 进行了纯 PTFE 及填加一般无机填料的 GB3160-83实验， 载荷为 5公斤， 速度为 200转 /分。 所得结果如下表所示：
表 1 普通填料改性 PTFE复合材料摩擦磨损实验结果
Figure imgf000005_0001
说明： 上表中 SGF代表短玻璃纤维；
LGF代表长玻璃纤维
表 2是将各种实验材料的的磨损率与纯 PTFE在同样实验条件下的磨损率的比值 的倒数做为耐磨性提高倍数来进行比较， 以便有一目了然的认识。
表 2 普通填料改性 PTFE与液晶填充 PTFE的耐磨性提高倍数对比
Figure imgf000006_0001
它填充型复合材料又有了明显下降。 效果最好的实例 2与同样实验条件的纯 PTFE相 比， 耐磨性提高了 490多倍； 而实例中最差的实例 4也提高了 170倍左右。 而普通填 料效果最好的也才提高耐磨性 32倍之多。

Claims

权 利 要 求
1、 一种由液晶类聚合物增强的聚四氟乙烯复合材料的制备方法， 其特征在于， 该方法包括以下各步骤：
( 1 )以重量占 60%~90%的氟聚合物为原料， 加入重量占 10%~30%液晶类聚合物和 重量占 0~10%的玻璃纤维或碳酸钙颗粒， 其中的液晶类聚合物为芳香族聚酯类高分子 化合物， 其物征是分子链中含有以下结构单元中的任何一种，
A:
Figure imgf000007_0001
并将该液晶类聚合物用低温研磨粉碎至小于 500μπι的粒度使用；
( 2)将上述机械混合均匀的物料放置于干燥箱内， 在 I35~150°C下干燥 2~10小 时， 取出后缓慢加压至 50~70MPa， 保持 3— 5分钟， 使其预制成型；
( 3) 再以每分钟约 2°C的速度升温烧结， 在 310°C~320°C间恒温 0. 5~1小时； 再以每分钟 1°C 左右的速度升温到 365~380°C 恒温 50~100 分钟， 然后冷却至 310°C~320°C恒温 20~30分钟， 随炉冷却至室温， 即得本发明的复合材料制品。
PCT/CN2000/000175 1999-06-25 2000-06-26 Procede de preparation d'un materiau composite a base de polytetrafluoroethylene renforce par des polymeres cristaux liquides WO2001000715A1 (fr)

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CN 99109356 CN1095484C (zh) 1999-06-25 1999-06-25 一种由液晶类聚合物增强的聚四氟乙烯复合材料的制备方法
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CN112341737A (zh) * 2020-11-10 2021-02-09 刘纯科 一种阻燃隔音保温材料及其制备方法
CN114082111A (zh) * 2021-11-11 2022-02-25 重庆倍维科技有限公司 一种放疗用插植模板的加工处理方法
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CN110437641A (zh) * 2019-07-02 2019-11-12 扬州清研高分子新材料有限公司 一种ptfe/lcp高分子合金及其制备方法
CN112341737A (zh) * 2020-11-10 2021-02-09 刘纯科 一种阻燃隔音保温材料及其制备方法
CN114082111A (zh) * 2021-11-11 2022-02-25 重庆倍维科技有限公司 一种放疗用插植模板的加工处理方法
CN114082111B (zh) * 2021-11-11 2023-11-10 重庆倍维科技有限公司 一种放疗用插植模板的加工处理方法
CN114989547A (zh) * 2022-06-24 2022-09-02 佛山科学技术学院 一种具有磨损原位修复功能的聚合物复合材料及其制备方法和应用
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CN115850831B (zh) * 2022-09-06 2023-12-08 湖南弘辉科技有限公司 一种耐磨材料及水润滑轴承

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