WO2022105133A1 - 一种耐冷却液的pps复合材料及其制备方法与应用 - Google Patents

一种耐冷却液的pps复合材料及其制备方法与应用 Download PDF

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WO2022105133A1
WO2022105133A1 PCT/CN2021/091378 CN2021091378W WO2022105133A1 WO 2022105133 A1 WO2022105133 A1 WO 2022105133A1 CN 2021091378 W CN2021091378 W CN 2021091378W WO 2022105133 A1 WO2022105133 A1 WO 2022105133A1
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composite material
parts
resistant
pps
zone
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王文超
黄险波
叶南飚
吴小漫
赖风华
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
    • C08J5/10—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
    • 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
    • C08J5/0405—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
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L81/00—Compositions 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; Compositions of polysulfones; Compositions of derivatives of such polymers
    • C08L81/02—Polythioethers; Polythioether-ethers
    • 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
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2400/00—Characterised by the use of unspecified polymers
    • C08J2400/10—Polymers characterised by the presence of specified groups, e.g. terminal or pendant functional groups
    • C08J2400/106—Polymers characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing nitrogen atoms
    • 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
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/29—Compounds containing one or more carbon-to-nitrogen double bonds
    • 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
    • C08K5/548—Silicon-containing compounds containing sulfur
    • 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 cooling liquid-resistant PPS composite material and a preparation method and application thereof.
  • Polyphenylene sulfide has excellent heat resistance, solvent resistance, high dimensional stability, and also has 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 around the engine, 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 corrosive coolant liquids for a long time, which can easily lead to decomposition and cracking of the parts, resulting in abnormal operation of the engine.
  • the purpose of the present invention is to overcome the above-mentioned shortcomings of the prior art and provide a PPS composite material resistant to cooling liquid.
  • the technical solution adopted in the present invention is: a PPS composite material resistant to cooling liquid, including the following components by weight: 30-90 parts of PPS resin, 10-70 parts of reinforcing fibers, mercaptosilane coupling agent 0.05-3 parts and 0.1-6 parts of additives containing carbodiimide structure.
  • the chlorine content does not exceed 800 ppm.
  • the melt index of the PPS resin is 10-100g/10min under the test condition of 300°C and 1.2kg.
  • the reinforcing fibers are glass fibers, carbon fibers or whiskers.
  • the diameter of the fibers is 4-20 microns.
  • the cooling liquid-resistant PPS composite material includes the following components in parts by weight: 45-75 parts of PPS resin, 20-60 parts of reinforcing fibers, 0.1-0.9 parts of mercaptosilane coupling agent and carbodiimide-containing Structure additives 0.3-4 parts.
  • the mercaptosilane coupling agent is a coupling agent conforming to the RSiX 3 structure; wherein, R is an aliphatic amino group; X is a chlorine group, a methoxy group, an ethoxy group, a propoxy group, and an acetoxy group. A sort of.
  • the present invention also provides a method for preparing the cooling liquid-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 a twin-screw extruder Extrusion and granulation are carried out in the machine, and reinforcing fibers are added to the side feeding port to obtain a PPS composite material that is resistant to cooling liquid.
  • the rotating speed of the high-speed mixer is 300-500 r/min
  • the temperature of the twin-screw extruder is 190°C in the first zone, 270°C in the second zone, 280°C in the third zone, and the fourth zone in the order from the feeding section to the head. 285°C, five zones 285°C, six zones 285°C, seven zones 280°C, eight zones 280°C, nine zones 280°C.
  • the invention also discloses the application of the coolant-resistant PPS composite material in the peripheral material of an automobile engine.
  • the low-chlorine resin is used in the glass fiber reinforced PPS system, the mercaptosilane coupling agent is added to the system at the same time, and the additive containing the carbodiimide structure is mixed at the same time, which can obviously improve the cooling resistance of the PPS.
  • the addition of coupling agent can also increase the bonding force between resin and glass fiber and improve 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 low chlorine resin, chlorine content 800ppm, PPS 1330C, Zhejiang Xinhecheng Special Materials Co., Ltd.; melt index 30g/10min (300°C, 1.2kg);
  • PPS-3 low chlorine resin, chlorine content 1200ppm, melt index 5g/10min (300°C, 1.2kg), Kingfa Technology Co., Ltd.;
  • Glass fiber 1 ECS309A-3-H, diameter 10 microns, Chongqing International Composite Materials Co., Ltd.;
  • Carbon fiber PX35CA0250-65, Toray Corporation
  • RASCHIG Stabilizer 7000, molecular weight 362;
  • RASCHIG Stabilizer 9000, polymer polymer, molecular weight >1000.
  • the coolant-resistant PPS composites described in the examples and comparative examples of the present application are prepared by the following methods:
  • Coolant resistance test Immerse the tensile specimen in ethylene glycol and place the test device in a 135 degree oven to test the properties of the specimen after a certain period of time, test the initial tensile properties, the tensile properties after 1000h, 2000h After the tensile properties, the tensile properties test standards refer to ISO-527; and calculate the property decay rate;
  • the application sets Examples 1 to 13 and Comparative Examples 1 to 2.
  • the components, contents and properties of specific Examples 1 to 6 and Comparative Examples 1 to 2 are shown in Table 1.
  • the components and contents of Examples 7 to 13 are shown in Table 1.
  • the performance is shown in Table 2:
  • Comparing Example 1 with Comparative Examples 1 and 2 it can be seen that in Comparative Examples 1 and 2, only one of the mercaptosilane coupling agent and the additive containing carbodiimide structure is contained, and the 2000h performance retention rate in Comparative Examples 1 and 2 is It is worse than Example 1; by comparing Example 1 and Example 13, it can be seen that the melt index of the PPS resin in Example 13 under the test conditions of 300 ° C and 1.2 kg is not within the range of 10-100 g/10min, and its 2000h performance retention rate is poor. in Example 1.
  • Example 5 Comparing Example 1 with Example 5, it can be seen that the chlorine content of the PPS resin in Example 5 is 800 ppm, the chlorine content of the PPS resin in Example 1 is 1200 ppm, and the 2000h performance retention rate in Example 5 is better than Example 5 1.
  • Example 1 Comparing Example 1 with Example 6, it can be seen that the molecular weight of the carbodiimide structure additive in Example 1 is greater than 400, the molecular weight of the carbodiimide structure additive in Example 6 is less than 400, and the The 2000h performance retention rate is better than that of Example 6.

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

一种耐冷却液的PPS复合材料及其制备方法，包括如下重量份的成分：PPS树脂30-90份、增强纤维10-70份、巯基硅烷偶联剂0.05-3份和含有碳二亚胺结构的添加剂0.1-6份。所述PPS复合材料中，通过在玻纤增强PPS体系中采用低氯树脂，同时向体系中加入巯基硅烷偶联剂，同时配合以含有碳二亚胺结构的添加剂，可以提高PPS的耐冷却液性能。

Description

一种耐冷却液的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，尤其涉及一种耐冷却液的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腐蚀性的冷却液液体中，极易导致分解产生制件开裂，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冷却液的PPS复合材料。
为实现上述目的，本发明所采取的技术方案为：一种耐冷却液的PPS复合材料，包括如下重量份的成分：PPS树脂30-90份、增强纤维10-70份、巯基硅烷偶联剂0.05-3份和含有碳二亚胺结构的添加剂0.1-6份。
由于高温下长时间浸泡在冷却液中(多为多醇类物质)，容易引起PPS树脂降解而使得性能降低，通过加入碳二亚胺类物质、低氯PPS树脂，可以与PPS端基基团反应封端，降低反应活性，从而提高耐冷却液能力。
优选地，所述PPS树脂中，氯含量不超过800ppm。
优选地，所述PPS树脂在300℃、1.2kg测试条件下的熔融指数为10-100g/10min。
优选地，所述增强纤维为玻璃纤维、碳纤维或晶须。
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，所述的耐冷却液的PPS复合材料，包括如下重量份的成分：PPS树脂45-75份、增强纤维20-60份、巯基硅烷偶联剂0.1-0.9份和含有碳二亚胺结构的添加剂0.3-4份。
优选地，所述巯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。
优选地，所述含有碳二亚胺结构的添加剂为分子量大于400的含有-N＝C＝N-化合物。
同时，本发明还提供所述耐冷却液的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，得到耐冷却液的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：一区190℃，二区270℃，三区280℃，四区285℃，五区285℃，六区285℃，七区280℃，八区280℃，九区280℃。
同时，本发明还公开一种所述耐冷却液的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，同时向体系中加入巯基硅烷偶联剂，同时配合以含有碳二亚胺结构的添加剂，可以明显提高PPS的耐冷却液性能，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：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-3：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：ECS309A-3-H，直径10微米，重庆国际复合材料有限公司；
碳纤维：PX35CA0250-65，东丽株式会社；
晶须：DL-40H，深圳市超邦新能源材料有限公司
巯基硅烷偶联剂：KH-590，市售；
含有碳二亚胺结构的添加剂：
RASCHIG，Stabilizer 7000，分子量362；
RASCHIG，Stabilizer 9000，聚合物聚合物，分子量>1000。
本申请实施例及对比例所述耐冷却液的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，得到耐冷却液的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：一区190℃，二区270℃，三区280℃，四区285℃，五区285℃，六区285℃，七区280℃，八区280℃，九区280℃。
耐冷却液测试：将拉伸样条浸没在乙二醇中，并将测试装置至于135度烘箱中，测试一定时间后的样条性能，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1～13及对比例1～2，具体实施例1～6及对比例1～2中的成分、含量及性能如表1所示，实施例7～13中的成分、含量及性能如表2所示：
表1 实施例1～6和对比例1～2中的成分、含量及性能
Figure PCTCN2021091378-appb-000001
表2 实施例7～13中成分及含量
Figure PCTCN2021091378-appb-000002
将实施例1与对比例1、2对比可知，对比例1、2中只含有巯基硅烷偶联剂、含有碳二亚胺结构的添加剂中的一种，对比例1、2中2000h性能保持率差 于实施例1；将实施例1与实施例13对比可知，实施例13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2000h性能保持率差于实施例1。
将实施例1与实施例5对比可知，实施例5中的PPS树脂的氯含量为800ppm，实施例1中的PPS树脂的氯含量为1200ppm，实施例5中的2000h性能保持率优于实施例1。
将实施例1与实施例6对比可知，实施例1中的碳二亚胺结构的添加剂的分子量大于400，实施例6中的碳二亚胺结构的添加剂的分子量小于400，实施例1中的2000h性能保持率优于实施例6。
将实施例7～12对比可知，当“PPS树脂45-75份、增强纤维20-60份、巯基硅烷偶联剂0.1-0.9份和含有碳二亚胺结构的添加剂0.3-4份”时，2000h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. 一种耐冷却液的PPS复合材料，其特征在于，包括如下重量份的成分：PPS树脂30-90份、增强纤维10-70份、巯基硅烷偶联剂0.05-3份和含有碳二亚胺结构的添加剂0.1-6份。
  2. 如权利要求1所述的耐冷却液的PPS复合材料，其特征在于，所述PPS树脂中，氯含量为不超过800ppm。
  3. 如权利要求1或2所述的耐冷却液的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所述的耐冷却液的PPS复合材料，其特征在于，所述增强纤维为玻璃纤维、碳纤维或晶须。
  5. 如权利要求4所述的耐冷却液的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所述的耐冷却液的PPS复合材料，其特征在于，包括如下重量份的成分：PPS树脂45-75份、增强纤维20-60份、巯基硅烷偶联剂0.1-0.9份和含有碳二亚胺结构的添加剂0.3-4份。
  7. 如权利要求1所述的耐冷却液的PPS复合材料，其特征在于，所述巯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所述的耐冷却液的PPS复合材料，其特征在于，所述含有碳二亚胺结构的添加剂为分子量大于400的含有-N＝C＝N-化合物。
  9. 一种如权利要求1～8任一项所述耐冷却液的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，得到耐冷却液的PPS复合材料。
  10. 如权利要求9所述耐冷却液的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：一区190℃，二区270℃，三区280℃，四区285℃，五区285℃，六区285℃，七区280℃，八区280℃，九区280℃。
  11. 如权利要求1～8任一项所述耐冷却液的PPS复合材料在汽车发动机周边材料中的应用。
PCT/CN2021/091378 2020-11-23 2021-04-30 一种耐冷却液的pps复合材料及其制备方法与应用 WO2022105133A1 (zh)

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