WO2022105132A1 - 一种耐水解的pps复合材料及其制备方法与应用 - Google Patents

一种耐水解的pps复合材料及其制备方法与应用 Download PDF

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WO2022105132A1
WO2022105132A1 PCT/CN2021/091367 CN2021091367W WO2022105132A1 WO 2022105132 A1 WO2022105132 A1 WO 2022105132A1 CN 2021091367 W CN2021091367 W CN 2021091367W WO 2022105132 A1 WO2022105132 A1 WO 2022105132A1
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hydrolysis
composite material
parts
pps
resistant
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French (fr)
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王文超
黄险波
叶南飚
吴小漫
杨旭峰
禹权
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金发科技股份有限公司
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
    • C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
    • C08G75/02—Polythioethers
    • C08G75/0204—Polyarylenethioethers
    • C08G75/0286—Chemical after-treatment
    • C08G75/029—Modification with organic compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
    • C08J5/042—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with carbon fibres
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/10—Reinforcing macromolecular compounds with loose or coherent fibrous material characterised by the additives used in the polymer mixture
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2381/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
    • C08J2381/02—Polythioethers; Polythioether-ethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/544—Silicon-containing compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/06—Elements
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/14—Glass

Definitions

  • the invention relates to the field of polymer material modification, in particular to a hydrolysis-resistant PPS composite material and a preparation method and application thereof.
  • Polyphenylene sulfide has excellent heat resistance, solvent resistance, high dimensional stability, excellent dielectric properties, excellent flame retardancy and mechanical properties, and is widely used in electrical and electronic, automotive, machinery, chemical and other fields. About 40% of modified PPS is used in the automotive industry, especially in the engine periphery, such as automotive water pumps and automotive thermostats. Due to the particularity of the working environment, the parts used in this part are exposed to high-temperature water or corrosive automotive fluids for a long time, which can easily lead to hydrolysis and cracking of the parts, resulting in abnormal engine operation.
  • the purpose of the present invention is to provide a hydrolysis-resistant PPS composite material to overcome the above-mentioned shortcomings of the prior art.
  • the technical solution adopted in the present invention is: a hydrolysis-resistant PPS composite material, comprising the following components in parts by weight: 40-90 parts of PPS resin, 10-70 parts of reinforcing fibers, aminopropyl silane coupling In the PPS resin, the chlorine content does not exceed 1200ppm.
  • the PPS resin Due to the long-term immersion in the aqueous solution at high temperature, the PPS resin is easily degraded and the performance is reduced. By adding isocyanates and PPS resin with low chlorine content, it can react with the end groups in PPS and the side groups in the molecular chain. End-capping reduces reactivity, thereby improving hydrolysis resistance and improving performance retention.
  • the chlorine content is 800 ppm.
  • the melt index of the PPS resin is 10-100 g/10min under the test condition of 300°C and 1.2kg.
  • the reinforcing fibers are glass fibers or carbon fibers.
  • the diameter of the fibers is 4-20 microns.
  • the hydrolysis-resistant PPS composite material includes the following components in parts by weight: 50-70 parts of PPS resin, 30-50 parts of reinforcing fibers, 0.2-1.2 parts of aminopropyl silane coupling agent and isocyanate end capping agent 0.4-3 servings.
  • the silane coupling agent is a coupling agent conforming to the RSiX 3 structure; wherein, R is an aliphatic amino group; X is one of chloro, methoxy, ethoxy, propoxy, and acetoxy kind.
  • TDI toluene diisocyanate
  • IPDI isophorone diisocyanate
  • MDI diphenylmethane diisocyanate
  • HMDI dicyclohexylmethane diisocyanate
  • HDI hexamethylene diisocyanate
  • LLI lysine diisocyanate
  • the present invention also provides a preparation method of the hydrolysis-resistant PPS composite material.
  • the method is as follows: mixing other components other than reinforcing fibers in a high-speed mixer to obtain a mixture; then adding the mixture to twin-screw extrusion The machine is extruded and granulated, and reinforcing fibers are added to the side feeding port to obtain a hydrolysis-resistant PPS composite material.
  • the rotating speed of the high-speed mixer is 300-500 rpm
  • the temperature of the twin-screw extruder is 190°C, 270°C, 280°C, 285°C, 285°C, 285°C, 280°C, 280°C, 280°C.
  • the present invention also discloses the application of the hydrolysis-resistant PPS composite material in the peripheral material of an automobile engine.
  • the PPS composite material of the present invention by adopting a low-chlorine resin in the glass fiber reinforced PPS system, adding an aminopropyl silane coupling agent to the system, and cooperating with an isocyanate structure-containing end capping agent, the water resistance of the PPS can be significantly improved.
  • the addition of coupling agent can also increase the bonding force between resin and glass fiber and improve the mechanical properties.
  • PPS-1 low chlorine resin, chlorine content 1200ppm, grade PPS 1350C, melt index 60g/10min (300°C, 1.2kg), Zhejiang Xinhecheng Special Materials Co., Ltd.;
  • PPS-2 ordinary resin, chlorine content 3000ppm, grade PPS 1150C, melt index 60g/10min (300°C, 1.2kg), Zhejiang Xinhecheng Special Materials Co., Ltd.;
  • PPS-3 low chlorine resin, chlorine content 800ppm, PPS 1330C, Zhejiang Xinhecheng Special Materials Co., Ltd.; melt index 30g/10min (300°C, 1.2kg);
  • PPS-4 ordinary resin, chlorine content 3000ppm, grade PPS 1130C, melt index 30g/10min (300°C, 1.2kg), Zhejiang Xinhecheng Special Materials Co., Ltd.;
  • PPS-5 low chlorine resin, chlorine content 1200ppm, melt index 5g/10min (300°C, 1.2kg), Kingfa Technology Co., Ltd.;
  • Glass fiber 1 Boulder group, E7CS10-03-584H; diameter 10 microns;
  • Carbon fiber PX35CA0250-65, Toray Corporation
  • Aminopropyl silane coupling agent KH-550, commercially available
  • Isocyanate blocking agent p-phenylenediisocyanate, commercially available.
  • hydrolysis-resistant PPS composite materials described in the examples and comparative examples of the present application are prepared by the following methods:
  • a high-speed mixer Mixing other components other than reinforcing fibers in a high-speed mixer to obtain a mixture; then adding the mixture to a twin-screw extruder for extrusion and granulation, and adding reinforcing fibers to the side feed port to obtain a hydrolysis-resistant PPS composite material;
  • the speed of the high-speed mixer is 400 rpm, and the temperature of the twin-screw extruder is 190°C, 270°C, 280°C, 285°C, 285°C, 285°C, 280°C, 280°C from the feeding section to the head. , 280°C.
  • Cooling liquid hydrolysis resistance test After mixing ethylene glycol and water in a ratio of 1:1, immerse the tensile specimen in it, and place the test device in a 130-degree oven to test the initial tensile properties, tensile strength after 1000 hours Tensile properties, tensile properties after 2000h, and the test standard of tensile properties refer to ISO-527; and calculate the property decay rate.
  • the present application sets Examples 1 to 10 and Comparative Examples 1 to 4.
  • the components, contents and properties of Examples 1 to 4 and Comparative Examples 1 to 4 are shown in Table 1.
  • the components and contents of Examples 5 to 10 are shown in Table 1.
  • the performance is shown in Table 2:
  • Example 2 Comparing Examples 2 to 3, it can be seen that the reinforcing fibers in Example 2 are glass fibers, and the reinforcing fibers in Example 3 are carbon fibers, and the performance retention rate in Example 2 is better than that in Example 3.
  • Example 1 Comparing Example 1 with Comparative Examples 2 and 3, it can be seen that in Comparative Examples 2 and 3, only one of aminopropylsilane coupling agent and isocyanate end-capping agent is contained, and the 2000h performance retention rate in Comparative Examples 2 and 3 is obviously poor.
  • Example 1 comparing Example 1 with Example 10, it can be seen that the melt index of the PPS resin in Example 10 under the test conditions of 300 ° C and 1.2 kg is not within the range of 10-100 g/10min, and its initial performance and performance retention rate worse than Example 1.

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  • Chemical & Material Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Reinforced Plastic Materials (AREA)

Abstract

本发明公开一种耐水解的PPS复合材料，包括如下重量份的成分：PPS树脂40-90份、增强纤维10-70份、氨丙基硅烷偶联剂0.1-2份和异氰酸酯封端剂0.2-5份；所述PPS树脂中，氯含量不超过1200ppm。本发明PPS复合材料中，通过在玻纤增强PPS体系中采用低氯树脂，同时向体系中加入氨丙基硅烷偶联剂，同时配合以含有异氰酸酯结构的封端剂，可以明显提高PPS的耐水解性能。同时，本发明还公开了所述PPS复合材料的制备方法。

Description

一种耐水解的PPS复合材料及其制备方法与应用 技术领域
本发明涉及高分子材料改性领域，尤其涉及一种耐水解的PPS复合材料及其制备方法与应用。
背景技术
聚苯硫醚(PPS)具有优异的耐热性、耐溶剂、高尺寸稳定性，还具有优良的介电性能、优良的阻燃性及力学性能，广泛应用于电子电气、汽车、机械、化工等领域。改性PPS约有近40％应用于汽车行业，尤其是应用于发动机周边，比如汽车水泵、汽车节温器。由于工作环境的特殊性，应用于该部分的制件长期暴露于高温水或者腐蚀性汽车液体中，极易导致水解产生制件开裂，引发发动机工作异常。
发明内容
基于此，本发明的目的在于克服上述现有技术的不足之处而提供一种耐水解的PPS复合材料。
为实现上述目的，本发明所采取的技术方案为：一种耐水解的PPS复合材料，包括如下重量份的成分：PPS树脂40-90份、增强纤维10-70份、氨丙基硅烷偶联剂0.1-2份和异氰酸酯封端剂0.2-5份；所述PPS树脂中，氯含量不超过1200ppm。
由于高温下长时间浸泡在含水溶液中，容易引起PPS树脂降解而使得性能降低，通过加入异氰酸酯类物质、低氯含量的PPS树脂，可以与PPS中的端基以及分子链中侧基基团反应封端，降低反应活性，从而提高耐水解能力，提升性能保持率。
优选地，所述PPS树脂中，氯含量为800ppm。
优选地，所述PPS树脂在300℃、1.2kg测试条件下的熔融指数为10-100 g/10min。
优选地，所述增强纤维为玻璃纤维或碳纤维。
更优选地，当所述增强纤维为玻璃纤维时，所述纤维的直径为4-20微米。
优选地，所述的耐水解的PPS复合材料，包括如下重量份的成分：PPS树脂50-70份、增强纤维30-50份、氨丙基硅烷偶联剂0.2-1.2份和异氰酸酯封端剂0.4-3份。
优选地，所述硅烷偶联剂为符合RSiX 3结构的偶联剂；其中，R为脂肪族氨基；X为氯基、甲氧基、乙氧基、丙氧基、乙酰氧基中的一种。
优选地，所述异氰酸酯封端剂为含有-N＝C＝O基团的化合物；更优选地，所述异氰酸酯封端剂为甲苯二异氰酸酯(TDI)、异佛尔酮二异氰酸酯(IPDI)、二苯基甲烷二异氰酸酯(MDI)、二环己基甲烷二异氰酸酯(HMDI)、六亚甲基二异氰酸酯(HDI)、赖氨酸二异氰酸酯(LDI)中的一种。
同时，本发明还提供所述耐水解的PPS复合材料的制备方法，所述方法为：将增强纤维之外的其他成分在高速混合机中进行混合，得到混合物；然后将混合物加入双螺杆挤出机中挤出、造粒，侧喂口加入增强纤维，得到耐水解的PPS复合材料。
优选地，高速混合机的转速为300～500转/分钟，双螺杆挤出机的温度从喂料段到机头依次为190℃、270℃、280℃、285℃、285℃、285℃、280℃、280℃、280℃。
此外，本发明还公开一种上述耐水解的PPS复合材料在汽车发动机周边材料中的应用。
相对于现有技术，本发明的有益效果为：
本发明PPS复合材料中，通过在玻纤增强PPS体系中采用低氯树脂，同时向体系中加入氨丙基硅烷偶联剂，同时配合以含有异氰酸酯结构的封端剂，可以明显提高PPS的耐水解性能，另外，偶联剂的加入也能增加树脂与玻纤的结 合力，提高力学性能。
具体实施方式
为更好的说明本发明的目的、技术方案和优点，下面将结合具体实施例对本发明作进一步说明。
实施例和对比例中用到的主要代表材料如下：
PPS-1：低氯树脂，氯含量1200ppm，牌号PPS 1350C，熔融指数60g/10min(300℃，1.2kg)，浙江新和成特种材料有限公司；
PPS-2：普通树脂，氯含量3000ppm，牌号PPS 1150C，熔融指数60g/10min(300℃，1.2kg)，浙江新和成特种材料有限公司；
PPS-3：低氯树脂，氯含量800ppm，PPS 1330C，浙江新和成特种材料有限公司；，熔融指数30g/10min(300℃，1.2kg)；
PPS-4：普通树脂，氯含量3000ppm，牌号PPS 1130C，熔融指数30g/10min(300℃，1.2kg)，浙江新和成特种材料有限公司；
PPS-5：低氯树脂，氯含量1200ppm，熔融指数5g/10min(300℃，1.2kg)，金发科技股份有限公司；
玻璃纤维1：巨石基团，E7CS10-03-584H；直径10微米；
碳纤维：PX35CA0250-65，东丽株式会社；
氨丙基硅烷偶联剂：KH-550，市售；
异氰酸酯封端剂：对苯二异氰酸酯，市售。
本申请实施例及对比例所述耐水解的PPS复合材料通过以下方法制备所得：
将增强纤维之外的其他成分在高速混合机中进行混合，得到混合物；然后将混合物加入双螺杆挤出机中挤出、造粒，侧喂口加入增强纤维，得到耐水解 的PPS复合材料；高速混合机的转速为400转/分钟，双螺杆挤出机的温度从喂料段到机头依次为190℃、270℃、280℃、285℃、285℃、285℃、280℃、280℃、280℃。
耐冷却液水解测试：将乙二醇与水按1：1的比例混合后，将拉伸样条浸没其中，并将测试装置置于130度烘箱中，测试初始拉伸性能、1000h后的拉伸性能、2000h后的拉伸性能，拉伸性能的测试标准参考ISO-527；并计算性能衰减率。
本申请设置实施例1～10及对比例1～4，具体实施例1～4及对比例1～4中的成分、含量及性能如表1所示，实施例5～10中的成分、含量及性能如表2所示：
表1 实施例1～4和对比例1～4中的成分、含量及性能
Figure PCTCN2021091367-appb-000001
表2 实施例5～10中成分及含量
Figure PCTCN2021091367-appb-000002
Figure PCTCN2021091367-appb-000003
将实施例1、4与对比例1、4对比可知，实施例1、4中的氯含量不超过1200ppm，对比例1、4中氯含量超过1200ppm，实施例1、4中的初始性能较高，性能保持率优于对比例1、4。
将实施例2～3对比可知，实施例2中的增强纤维为玻璃纤维，实施例3中的增强纤维为碳纤维，实施例2中的性能保持率优于实施例3。
将实施例1与对比例2、3对比可知，对比例2、3中只含有氨丙基硅烷偶联剂、异氰酸酯封端剂中的一种，对比例2、3中2000h性能保持率明显差于实施例1；将实施例1与实施例10对比可知，实施例10中PPS树脂在300℃、1.2kg测试条件下的熔融指数不在10-100g/10min范围内，其初始性能和性能保持率差于实施例1。
将实施例5～9对比可知，当“PPS树脂50-70份、增强纤维30-50份、氨丙基硅烷偶联剂0.2-1.2份和异氰酸酯封端剂0.4-3份”时，性能保持率更好。
最后所应当说明的是，以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的实质和范围。

Claims (11)

  1. 一种耐水解的PPS复合材料，其特征在于，包括如下重量份的成分：PPS树脂40-90份、增强纤维10-70份、氨丙基硅烷偶联剂0.1-2份和异氰酸酯封端剂0.2-5份；所述PPS树脂中，氯含量不超过1200ppm。
  2. 如权利要求1所述的耐水解的PPS复合材料，其特征在于，所述PPS树脂中，氯含量不超过800ppm。
  3. 如权利要求1或2所述的耐水解的PPS复合材料，其特征在于，所述PPS树脂在300℃、1.2kg测试条件下的熔融指数为10-100g/10min。
  4. 如权利要求1所述的耐水解的PPS复合材料，其特征在于，所述增强纤维为玻璃纤维或碳纤维。
  5. 如权利要求4所述的耐水解的PPS复合材料，其特征在于，当所述增强纤维为玻璃纤维时，所述纤维的直径为4-20微米。
  6. 如权利要求1所述的耐水解的PPS复合材料，其特征在于，包括如下重量份的成分：PPS树脂50-70份、增强纤维30-50份、氨丙基硅烷偶联剂0.2-1.2份和异氰酸酯封端剂0.4-3份。
  7. 如权利要求1所述的耐水解的PPS复合材料，其特征在于，所述氨丙基硅烷偶联剂为符合RSiX 3结构的偶联剂；其中，R为脂肪族氨基；X为氯基、甲氧基、乙氧基、丙氧基、乙酰氧基中的一种。
  8. 如权利要求1所述的耐水解的PPS复合材料，其特征在于，所述异氰酸酯封端剂为含有-N＝C＝O基团的化合物；优选地，所述异氰酸酯封端剂为甲苯二异氰酸酯、异佛尔酮二异氰酸酯、二苯基甲烷二异氰酸酯、二环己基甲烷二异氰酸酯、六亚甲基二异氰酸酯、赖氨酸二异氰酸酯中的一种。
  9. 一种如权利要求1～8任一项所述耐水解的PPS复合材料的制备方法，其特征在于，所述方法为：将增强纤维之外的其他成分在高速混合机中进行混合，得到混合物；然后将混合物加入双螺杆挤出机中挤出、造粒，侧喂口加入增强 纤维，得到耐水解的PPS复合材料。
  10. 如权利要求9所述耐水解的PPS复合材料的制备方法，其特征在于，高速混合机的转速为300～500转/分钟，双螺杆挤出机的温度从喂料段到机头依次为190℃、270℃、280℃、285℃、285℃、285℃、280℃、280℃、280℃。
  11. 如权利要求1～8任一项所述耐水解的PPS复合材料在汽车发动机周边材料中的应用。
PCT/CN2021/091367 2020-11-23 2021-04-30 一种耐水解的pps复合材料及其制备方法与应用 WO2022105132A1 (zh)

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