WO2022110668A1 - 一种疏水性高cti聚苯硫醚组合物及其制备方法与应用 - Google Patents

一种疏水性高cti聚苯硫醚组合物及其制备方法与应用 Download PDF

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WO2022110668A1
WO2022110668A1 PCT/CN2021/092809 CN2021092809W WO2022110668A1 WO 2022110668 A1 WO2022110668 A1 WO 2022110668A1 CN 2021092809 W CN2021092809 W CN 2021092809W WO 2022110668 A1 WO2022110668 A1 WO 2022110668A1
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polyphenylene sulfide
parts
coupling agent
cti
sulfide composition
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PCT/CN2021/092809
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English (en)
French (fr)
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何志帅
黄险波
叶南飚
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
    • 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

Definitions

  • the invention relates to the technical field of engineering plastics, in particular to a hydrophobic high CTI polyphenylene sulfide composition and a preparation method and application thereof.
  • Polyphenylene sulfide has excellent high temperature resistance, dimensional stability, chemical resistance, creep resistance and self-flame retardant properties, and is widely used in electrical and electronic, automotive, and precision instruments.
  • PPS Polyphenylene sulfide
  • the main chain of PPS is composed of a large number of benzene rings, when the PPS surface is discharged, the benzene ring structure will be broken to generate free radicals, and a conductive carbon layer will be formed on the surface, resulting in poor tracking performance (CTI for short) of PPS.
  • CTI of PPS is less than 150V.
  • the CTI of PPS is mainly improved by adding a large amount of inorganic fillers.
  • the Chinese patent with publication number CN102924921A proposes to improve the CTI of polyphenylene sulfide by the compounding technology of chopped glass fiber and ultra-fine filler minerals.
  • the toughness is mainly improved by adding tougheners and CTI at the same time.
  • Such as the Chinese patent with publication number CN 104194337 it is proposed to adopt high-flow PPS resin, use polyethylene and ethylene-methyl acrylate-glycidyl methacrylate random terpolymer or polyolefin elastic graft glycidyl ester. The blend improves toughness, and the prepared PPS material has better toughness and CTI properties.
  • the Chinese patent with publication number CN 109679345 proposes that the fluidity of the polyphenylene sulfide composite material and the tracking resistance of the material can be improved through the compounding of low molecular weight polymer plasticizers and modifiers.
  • the object of the present invention is to overcome the deficiencies of the above-mentioned prior art and provide a hydrophobic high CTI polyphenylene sulfide composition.
  • the polyphenylene sulfide composition has good dimensional stability, toughness and high rigidity while having high CTI performance.
  • a hydrophobic high CTI polyphenylene sulfide composition comprising the following components by weight: 30-80 parts of polyphenylene sulfide, 10-60 parts of glass fiber, 0.2-2 parts of coupling agent, 0.2-2 parts of fluorosilicone oil and 0.1-2 parts of antioxidant.
  • the hydrophobic high CTI polyphenylene sulfide composition includes the following components in parts by weight: 45-70 parts of polyphenylene sulfide, 30-55 parts of glass fiber, 0.5-1 part of coupling agent, fluorosilicone oil 0.8-1.5 parts and antioxidants 0.2-0.5 parts.
  • the compatibility of the PPS and the glass fiber material is improved by the coupling agent, and the rigidity and toughness of the material are further improved. Due to the low surface energy and superhydrophobicity of silicone oil, during the injection molding process, the low surface energy will accumulate on the surface of the material, which has little effect on the rigidity of the material. At the same time, after the fluorosilicone oil accumulates on the surface, the superhydrophobicity will greatly reduce the wetting of the PPS by the electrolyte, which can significantly improve the CTI of the PPS material.
  • the coupling agent is at least one of a silane coupling agent, a titanate coupling agent, and an aluminate coupling agent.
  • the coupling agent is at least one of aminosilane coupling agent and methoxysilane coupling agent.
  • the fluorosilicone oil has a viscosity of 300-9000 mPa.s measured by a silicone oil viscometer at 25°C.
  • the fluorosilicone oil has a viscosity of 500-1500 mPa.s measured by a silicone oil viscometer at 25°C.
  • the diameter of the glass fibers is 6-10 mm.
  • the glass fiber is any glass fiber that can be used for PPS, preferably a special glass fiber suitable for PPS through surface modification, such as a special glass fiber for PPS produced by Jushi.
  • the antioxidant is at least one of a phenolic antioxidant, a phosphite antioxidant, and a metal passivator. More preferably, the antioxidant is a combination of Y-001, 412S and MD1024.
  • the polyphenylene sulfide is a linear polyphenylene sulfide having a certain reactive cross-linking point that can react with a coupling agent.
  • the present invention also provides a preparation method of the hydrophobic high CTI polyphenylene sulfide composition, the method is:
  • the components except the glass fibers are dispersed in a high-speed mixer according to the formula ratio, and then enter a twin-screw extruder, and the glass fibers are subjected to side-feed extrusion and granulation to obtain the hydrophobic high CTI polyphenylene sulfide composition;
  • the rotating speed of the high-speed mixer is 300-500rpm/min;
  • the feeding of glass fiber is 100-300kg/h;
  • the extrusion temperature is 270-300°C.
  • the invention also discloses the application of the hydrophobic high CTI polyphenylene sulfide composition in electronics, automobiles and precision instruments.
  • the compatibility of the PPS and the glass fiber material is improved by the coupling agent, and the rigidity and toughness of the material are further improved. Due to the low surface energy and superhydrophobicity of silicone oil, during the injection molding process, the low surface energy will accumulate on the surface of the material, which has little effect on the rigidity of the material. At the same time, after the fluorosilicone oil accumulates on the surface, the superhydrophobicity will greatly reduce the wetting of the PPS by the electrolyte, which can significantly improve the CTI of the PPS material.
  • each performance test standard is as follows:
  • Polyphenylene sulfide 1 PPS 1150C, linear polyphenylene ether, Xinhecheng;
  • Polyphenylene sulfide 2 PPS 21150C, cross-linked polyphenylene ether, Xinhecheng;
  • Glass fiber 1 glass fiber diameter is 8-10mm, boulder;
  • Glass fiber 2 The diameter of glass fiber is 12-15mm, which is commercially available;
  • Coupling agent 1 aminosilane coupling agent, KH 550, commercially available;
  • Coupling agent 2 trimethoxysilane, WD-21, commercially available;
  • Coupling agent 3 titanate coupling agent, KR-TTS, commercially available
  • Toughening agent PTW, DuPont
  • Fluorosilicone oil 1 methyl-terminated polytrifluoropropyl silicone oil with a viscosity of 500 mPa.s measured by a silicone oil viscometer at 25°C, commercially available;
  • Fluorosilicone oil 2 methyl-terminated polytrifluoropropyl silicone oil with a viscosity of 1000 mPa.s measured by a silicone oil viscometer at 25°C, commercially available;
  • Fluorosilicone oil 3 methyl-terminated polytrifluoropropyl silicone oil with a viscosity of 1500 mPa.s measured by a silicone oil viscometer at 25°C, commercially available;
  • Fluorosilicone oil 4 methyl-terminated polytrifluoropropyl silicone oil with a viscosity of 2000 mPa.s measured by a silicone oil viscometer at 25°C, commercially available;
  • Fluorosilicone oil 5 Polytrifluoropropyl silicone oil with a viscosity of 10000mPa.s measured by a silicone oil viscometer at 25°C, commercially available;
  • Antioxidant combination of phenolic antioxidant Y-001, phosphite antioxidant 412S and metal passivator MD1024, the weight ratio of the three is: 1:2:2; commercially available;
  • Examples 1 to 13 and Comparative Examples 1 to 4 are set, and the content of each component in Examples 1 to 8 is shown in Table 1; ;
  • the preparation method of described hydrophobicity high CTI polyphenylene sulfide composition is as follows:
  • the components except the glass fibers are dispersed in a high-speed mixer according to the formula ratio, and then enter a twin-screw extruder, and the glass fibers are subjected to side-feed extrusion and granulation to obtain the hydrophobic high CTI polyphenylene sulfide composition;
  • the rotating speed of the high-speed mixer is 400rpm/min; the feeding of glass fiber is 300kg/h; and the extrusion temperature is 300°C.
  • Example 1 Comparing Example 1 with Example 2, it can be seen that the diameter of the glass fiber in Example 1 is in the range of 6-10 mm, the diameter of the glass fiber in Example 2 is not within the above range, and the flexural modulus, notch in Example 1 Impact strength, shrinkage rate and CTI are all better than Example 2;
  • the viscosity (25°C) of fluorosilicone oil in Examples 1, 5, and 6 is in the range of 500-1500mPa.s, and the viscosity (25°C) of fluorosilicone oil in Example 7 is 300-9000mPa.
  • the viscosity (25°C) of the fluorosilicone oil in Example 8 is not in the range of 300-9000mPa.s, and the flexural modulus, notched impact strength, shrinkage rate, and CTI of Examples 1, 5, 6, and 7 are better than those of the implementation.
  • Example 8 the flexural modulus, notched impact strength, shrinkage, and CTI of Examples 1, 5, and 6 are all better than those of Example 7;
  • Examples 9 and 10 satisfy the requirements of "45-70 parts of polyphenylene sulfide, 30-55 parts of glass fiber, 0.5-1 part of coupling agent, and 0.8-1 part of fluorosilicone oil. 1.5 parts and antioxidant 0.2-0.5 parts”, the notched impact strength, shrinkage rate and CTI of Examples 9-10 are better than Examples 11 and 12;
  • Comparative Example 1 Comparing Example 1 with Comparative Examples 1 to 4, it can be seen that Comparative Examples 1 and 2 do not contain the coupling agent and fluorosilicone oil of the present application, and the flexural modulus, notched impact strength, shrinkage rate and CTI of both are worse than those of Example 1. .
  • the fluorosilicone oil When the fluorosilicone oil is not contained in Comparative Example 3, its CTI is much lower than that of Example 1.
  • the coupling agent of the present application When the coupling agent of the present application is not included in Comparative Example 4, its CTI is greatly improved, but the flexural modulus, notched impact strength, shrinkage rate and CTI are all worse than those of Example 1;
  • Example 13 Comparing Example 1 and Example 13, it can be seen that the cross-linked polyphenylene sulfide material is inferior to Example 1 in terms of flexural modulus, notched impact strength and CTI.

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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)

Abstract

本发明公开一种疏水性高CTI聚苯硫醚组合物，包括如下重量份的成分：聚苯硫醚30-80份、玻璃纤维10-60份、偶联剂0.2-2份、氟硅油0.2-2份和抗氧剂0.1-2份。本发明所述疏水性高CTI聚苯硫醚组合物中，通过偶联剂来提高PPS和玻纤材料的相容性，进一步来提高材料的刚性和韧性的同时，通过加入氟硅油，利用氟硅油低表面能和超疏水特点，在注塑过程中会由于低表面能会聚集在材料表面，对材料的刚性影响较小。同时氟硅油聚集在表面后，由于超疏水的特点会大大降低电解液对PPS的润湿，可以明显提高PPS的材料的CTI。

Description

一种疏水性高CTI聚苯硫醚组合物及其制备方法与应用 技术领域
本发明涉及工程塑料技术领域，尤其涉及一种疏水性高CTI聚苯硫醚组合物及其制备方法与应用。
背景技术
聚苯硫醚(PPS)具有优异的耐高温性、尺寸稳定性、耐化学、耐蠕变性能和自阻燃性能，在电子电气、汽车、精密仪器中应用广泛。但是由于PPS主链是由大量的苯环组成，在PPS表面进行放电时，苯环结构会发生断裂产生自由基，在表面形成导电碳层，导致PPS的漏电起痕性能(简称CTI)较差，一般情况下，PPS的CTI小于150V。
随着电子电器安全性能的不断提高，对CTI的要求越来越高，目前主要通过添加大量的无机填料来提高PPS的CTI。如公开号为CN102924921A的中国专利提出以短切玻璃纤维与超细填充矿物的混配复合技术提高聚苯硫醚CTI，CTI可达到225V以上，但是大量的填充会造成材料的韧性大幅下降。
针对材料韧性下降的问题，目前主要是通过加入增韧剂来韧性的同时提高CTI。如公开号为CN 104194337的中国专利，提出通过采用高流动PPS树脂、用聚乙烯和乙烯-丙烯酸甲酯-甲基丙烯酸缩水甘油酯无规三元共聚物或聚烯烃弹性接枝缩水甘油酯的共混物提高韧性，制备的PPS材料具有较好的韧性和CTI性能。公开号为CN 109679345的中国专利，提出通过低分子量聚合物增塑剂和改性剂的复配可以提高聚苯硫醚复合材料的流动性和材料耐漏电起痕性能。同时利用少量导电填充剂和聚酰胺树脂配合达到了传统高填充量聚苯硫醚复合材料相同的耐漏电起痕性能，但是增韧剂的加入会造成材料尺寸稳定性和刚度的下降。
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疏水 性高CTI聚苯硫醚组合物。所述聚苯硫醚组合物，在具有高CTI性能的同时，具有较好的尺寸稳定性、韧性和高刚性。
为实现上述目的，本发明所采取的技术方案为：一种疏水性高CTI聚苯硫醚组合物，包括如下重量份的成分：聚苯硫醚30-80份、玻璃纤维10-60份、偶联剂0.2-2份、氟硅油0.2-2份和抗氧剂0.1-2份。
优选地，所述的疏水性高CTI聚苯硫醚组合物，包括如下重量份的成分：聚苯硫醚45-70份、玻璃纤维30-55份、偶联剂0.5-1份、氟硅油0.8-1.5份和抗氧剂0.2-0.5份。
本发明所述疏水性高CTI聚苯硫醚组合物中，通过偶联剂来提高PPS和玻纤材料的相容性，进一步来提高材料的刚性和韧性的同时，通过加入氟硅油，利用氟硅油低表面能和超疏水特点，在注塑过程中会由于低表面能会聚集在材料表面，对材料的刚性影响较小。同时氟硅油聚集在表面后，由于超疏水的特点会大大降低电解液对PPS的润湿，可以明显提高PPS的材料的CTI。
优选地，所述偶联剂为硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂中的至少一种。
更优选地，所述偶联剂为氨基硅烷偶联剂、甲氧基硅烷偶联剂中的至少一种。
优选地，所述氟硅油在25℃下，采用硅油粘度计测试的粘度为300-9000mPa.s。
更优选地，所述氟硅油在25℃下，采用硅油粘度计测试的粘度为500-1500mPa.s。
优选地，所述玻璃纤维的直径为6-10mm。所述的玻璃纤维为任何可以用于PPS的玻璃纤维，优选通过表面改性适用于PPS的专用玻纤，如巨石生产的PPS专用玻纤。
优选地，所述抗氧剂为酚类抗氧剂、亚磷酸酯类抗氧剂、金属钝化剂中的 至少一种。更优选地，所述抗氧剂为Y-001、412S和MD1024的组合。
优选地，所述聚苯硫醚为具有一定反应交联点可以与偶联剂反应的线性型聚苯硫醚。
同时，本发明还提供一种所述疏水性高CTI聚苯硫醚组合物的制备方法，所述方法为：
将除玻璃纤维之外的各成分按照配方比例经过高速混合机分散后，进入双螺杆挤出机，玻璃纤维进行侧喂挤出造粒，得到所述疏水性高CTI聚苯硫醚组合物；其中，高速混合机的转速为300-500rpm/min；玻璃纤维的喂料为100-300kg/h；挤出温度为270-300℃。
同时，本发明还公开一种所述的疏水性高CTI聚苯硫醚组合物在电子电气、汽车、精密仪器中的应用。
相对于现有技术，本发明的有益效果为：
本发明所述疏水性高CTI聚苯硫醚组合物中，通过偶联剂来提高PPS和玻纤材料的相容性，进一步来提高材料的刚性和韧性的同时，通过加入氟硅油，利用氟硅油低表面能和超疏水特点，在注塑过程中会由于低表面能会聚集在材料表面，对材料的刚性影响较小。同时氟硅油聚集在表面后，由于超疏水的特点会大大降低电解液对PPS的润湿，可以明显提高PPS的材料的CTI。
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。以下实施例只是本发明的典型例，本发明的保护范围并不局限于此。
以下实施例和对比例中，各性能测试标准如下：
弯曲模量：按照标准ISO 178:2019进行测试，弯曲速率为2mm/min；
CTI：按照标准IEC 60112：2009进行测试；
缺口冲击强度：按照标准ISO 180:2000/Amd2:2013进行测试；
材料收缩率：按照标准ISO294-4：2018进行测试。
实施例和对比例中用到的材料如下：
聚苯硫醚1：PPS 1150C，线性型聚苯醚，新和成；
聚苯硫醚2：PPS 21150C，交联型聚苯醚，新和成；
玻璃纤维1：玻纤直径为8-10mm，巨石；
玻璃纤维2：玻纤直径为12-15mm，市售；
偶联剂1：氨基硅烷偶联剂，KH 550，市售；
偶联剂2：三甲氧基硅烷，WD-21，市售；
偶联剂3：钛酸酯偶联剂，KR-TTS，市售；
增韧剂：PTW，杜邦；
氟硅油1：25℃下，采用硅油粘度计测试的粘度为500mPa.s的甲基封端的聚三氟丙基硅油，市售；
氟硅油2：25℃下，采用硅油粘度计测试的粘度为1000mPa.s的甲基封端的聚三氟丙基硅油，市售；
氟硅油3：25℃下，采用硅油粘度计测试的粘度为1500mPa.s的甲基封端的聚三氟丙基硅油，市售；
氟硅油4：25℃下，采用硅油粘度计测试的粘度为2000mPa.s的甲基封端的聚三氟丙基硅油，市售；
氟硅油5：25℃下，采用硅油粘度计测试的粘度为10000mPa.s的聚三氟丙基硅油，市售；
抗氧剂：酚类抗氧剂Y-001、亚磷酸酯类抗氧剂412S和金属钝化剂MD1024组合，三者重量比为：1:2:2；市售；
本申请设置实施例1～13及对比例1～4，实施例1～8的各成分含量如表1所示；实施例9～13及对比例1～4的各成分含量如表2所示；所述疏水性高CTI聚苯硫醚组合物的制备方法如下：
将除玻璃纤维之外的各成分按照配方比例经过高速混合机分散后，进入双螺杆挤出机，玻璃纤维进行侧喂挤出造粒，得到所述疏水性高CTI聚苯硫醚组合物；其中，高速混合机的转速为400rpm/min；玻璃纤维的喂料为300kg/h；挤出温度为300℃。
表1 实施例1～8中的成分、含量及性能数据
Figure PCTCN2021092809-appb-000001
表2 实施例9～13和对比例1～4中的成分、含量及性能数据
Figure PCTCN2021092809-appb-000002
将实施例1与实施例2对比可知，实施例1中玻璃纤维的直径为6-10mm范围内，实施例2中的玻璃纤维的直径不在上述范围内，实施例1中的弯曲模量、缺口冲击强度、收缩率、CTI均优于实施例2；
将实施例1、3、4进行对比可知，实施例1、3中的偶联剂为氨基硅烷偶联剂、甲氧基硅烷偶联剂中的一种，实施例4中的偶联剂为钛酸酯偶联剂，实施 例1、3的弯曲模量、缺口冲击强度、收缩率、CTI均优于实施例4；
将1、5～8进行对比可知，实施例1、5、6中氟硅油粘度(25℃)为500-1500mPa.s范围内，实施例7中氟硅油粘度(25℃)为300-9000mPa.s范围内，实施例8中氟硅油粘度(25℃)不在300-9000mPa.s范围内，实施例1、5、6、7的弯曲模量、缺口冲击强度、收缩率、CTI均优于实施例8，实施例1、5、6的弯曲模量、缺口冲击强度、收缩率、CTI均优于实施例7；
将实施例9、10与实施例11、12对比可知，实施例9、10满足“聚苯硫醚45-70份、玻璃纤维30-55份、偶联剂0.5-1份、氟硅油0.8-1.5份和抗氧剂0.2-0.5份”，实施例9-10的缺口冲击强度、收缩率、CTI均优于实施例11、12；
将实施例1与对比例1～4对比可知，对比例1、2中不含有本申请偶联剂、氟硅油，两者弯曲模量、缺口冲击强度、收缩率、CTI均差于实施例1。对比例3中不含氟硅油时，其CTI远低于实施例1。对比例4中不含本申请的偶联剂时，其CTI大大提升，但是弯曲模量、缺口冲击强度、收缩率、CTI均差于实施例1；
将实施例1和实施例13对比可知，使用交联型聚苯硫醚材料其在弯曲模量、缺口冲击强度、CTI上均差于实施例1。
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. 一种疏水性高CTI聚苯硫醚组合物，其特征在于，包括如下重量份的成分：聚苯硫醚30-80份、玻璃纤维10-60份、偶联剂0.2-2份、氟硅油0.2-2份和抗氧剂0.1-2份。
  2. 如权利要求1所述的疏水性高CTI聚苯硫醚组合物，其特征在于，包括如下重量份的成分：聚苯硫醚45-70份、玻璃纤维30-55份、偶联剂0.5-1份、氟硅油0.8-1.5份和抗氧剂0.2-0.5份。
  3. 如权利要求1～2任一项所述的疏水性高CTI聚苯硫醚组合物，其特征在于，所述偶联剂为硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂中的至少一种。
  4. 如权利要求3所述的疏水性高CTI聚苯硫醚组合物，其特征在于，所述偶联剂为氨基硅烷偶联剂、甲氧基硅烷偶联剂中的至少一种。
  5. 如权利要求1～2任一项所述的疏水性高CTI聚苯硫醚组合物，其特征在于，所述氟硅油在25℃下，采用硅油粘度计测试的粘度为300-9000mPa.s。
  6. 如权利要求5所述的疏水性高CTI聚苯硫醚组合物，其特征在于，所述氟硅油在25℃下，采用硅油粘度计测试的粘度为500-1500mPa.s。
  7. 如权利要求1所述的疏水性高CTI聚苯硫醚组合物，其特征在于，所述玻璃纤维的直径为6-10mm。
  8. 如权利要求1所述的疏水性高CTI聚苯硫醚组合物，其特征在于，所述抗氧剂为酚类抗氧剂、亚磷酸酯类抗氧剂、金属钝化剂中的至少一种。
  9. 如权利要求1所述的疏水性高CTI聚苯硫醚组合物，其特征在于，所述聚苯硫醚为线性型聚苯硫醚。
  10. 一种如权利要求1～9任一项所述疏水性高CTI聚苯硫醚组合物的制备方法，其特征在于，所述方法为：
    将除玻璃纤维之外的各成分按照配方比例经过高速混合机分散后，进入双螺杆挤出机，玻璃纤维进行侧喂挤出造粒，得到所述疏水性高CTI聚苯硫醚组 合物；其中，高速混合机的转速为300-500rpm/min；玻璃纤维的喂料为100-300kg/h；挤出温度为270-300℃。
  11. 一种如权利要求1～9任一项所述的疏水性高CTI聚苯硫醚组合物在电子电气、汽车、精密仪器中的应用。
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