WO2022016788A1 - 一种超高断裂伸长率的pps复合材料及其制备方法 - Google Patents

一种超高断裂伸长率的pps复合材料及其制备方法 Download PDF

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WO2022016788A1
WO2022016788A1 PCT/CN2020/136307 CN2020136307W WO2022016788A1 WO 2022016788 A1 WO2022016788 A1 WO 2022016788A1 CN 2020136307 W CN2020136307 W CN 2020136307W WO 2022016788 A1 WO2022016788 A1 WO 2022016788A1
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pps
composite material
ultra
break
high elongation
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王文超
黄险波
叶南飚
何志帅
仇禄
禹权
丁超
赖风华
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Kingfa Science and Technology Co Ltd
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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

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  • the invention relates to the field of polymer material modification, in particular to a PPS composite material with ultra-high elongation at break and a preparation method 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.
  • PPS Polyphenylene sulfide
  • the toughness of PPS is poor, and the impact strength and elongation at break are low, especially the elongation at break. Even if the PPS is toughened, the elongation at break is generally below 15%, which is difficult to further improve.
  • the purpose of the present invention is to overcome the above-mentioned shortcomings of the prior art and provide a PPS composite material with ultra-high elongation at break.
  • the technical scheme adopted in the present invention is: a PPS composite material with ultra-high elongation at break, comprising the following components by weight: 50-95 parts of PPS resin, 0.5-8 parts of montmorillonite, 3-30 parts of toughening agent and 0.1-2 parts of antioxidant, the PPS resin is an acidified linear PPS resin.
  • PPS end groups are difficult to control, and contain groups such as terminal chlorine groups, sodium mercapto groups, sulfhydryl groups, etc., and the reactivity is not high.
  • the acidified PPS resin is washed with an acidic solution during the synthesis process. Compared with ordinary PPS, it contains more reactive groups such as carboxyl groups and mercapto groups, so it has higher reactivity with reactive tougheners.
  • the present invention is based on this selection of acidified PPS as the base resin.
  • the acidified linear PPS resin has a melt index of less than 500 g/10min under the test conditions of 316°C and 5kg.
  • the toughening agent is ethylene-epoxy/acid anhydride type copolymer, ethylene-acrylate-epoxy/acid anhydride type terpolymer, ethylene/ At least one of butadiene-styrene-epoxy/acid anhydride type terpolymers.
  • ethylene-epoxy/acid anhydride type copolymers represent: ethylene-epoxy type copolymers or ethylene-acid anhydride type copolymers; ethylene-acrylate-epoxy/acid anhydride type terpolymers represent : ethylene-acrylate-epoxy terpolymer or ethylene-acrylate-acid anhydride terpolymer; ethylene/butadiene-styrene-epoxy/acid anhydride terpolymer Representative: ethylene-styrene -Epoxy terpolymer, ethylene-styrene-acid anhydride terpolymer, butadiene-styrene-epoxy terpolymer, butadiene-styrene-acid anhydride terpolymer.
  • the antioxidant is at least one of hindered phenol antioxidants, hindered amine antioxidants, and phosphite antioxidants, A mixture of at least one thio-type antioxidant.
  • the weight average molecular weight of the antioxidant is not less than 300.
  • the present invention also provides a preparation method of the PPS composite material with the ultra-high elongation at break. Extrusion and granulation are carried out in a screw extruder to obtain the PPS composite material with the ultra-high elongation at break.
  • 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 toughening agent improves the interfacial bonding force between the montmorillonite and the PPS resin.
  • the surrounding PPS resin has a disordered elastic transition area. During the stress stretching process, the polymer chains wrapped around the montmorillonite gradually disentangle, which greatly improves the elongation at break, and the elongation at break can be Reach more than 30%; and the product has good appearance and white color.
  • Acidified linear PPS resin 1 (PPS1), melt index is 120g/10min (316°C, 5kg), PPS 3412, Zhejiang Xinhecheng Special Materials Co., Ltd.;
  • Acidified linear PPS resin 2 (PPS2), melt index is 500g/10min (316°C, 5kg), PPS 3450, Zhejiang Xinhecheng Special Materials Co., Ltd.;
  • Toughening agent ethylene-acrylate-epoxy type toughening agent, ethylene-methyl acrylate-glycidyl methacrylate (GMA) terpolymer structure; LOTADER AX8900, Arkema, France;
  • Antioxidant the mixture of antioxidant 1790 (hindered phenol antioxidant) and antioxidant 168 (phosphite antioxidant), the weight ratio of the two is 2:1;
  • PPS composite materials with ultra-high elongation at break described in the examples and comparative examples of the present application are prepared by the following methods:
  • the components are added to a high-speed mixer and mixed for 1 minute to obtain a mixed material, and then the mixed material is added to a twin-screw extruder for extrusion and granulation to obtain the PPS composite material with the ultra-high elongation at break; wherein , 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. °C, 280 °C.
  • the application sets Examples 1 to 8 and Comparative Examples 1 to 4.
  • the components and content selections in specific Examples 1 to 8 and Comparative Examples 1 to 4 are shown in Table 1, and the performance data are shown in Table 2:
  • the number of bendings is by injection molding a 0.8mm thick spline, and it is repeatedly bent from both sides until it is broken or obvious cracks appear, and the number of bendings at the time of breaking is recorded.
  • Example 4 As can be seen from Table 2, comparing Example 4 with Comparative Examples 1, 2, and 3, it is found that regardless of the lack of toughening agent, montmorillonite or antioxidant in the formula, the corresponding elongation at break and bending The number of folds decreased significantly; comparing Example 4 with Example 5, it was found that when the melt index of the PPS resin at 316°C and 5kg was less than 500g/10min, the elongation at break and the number of folds corresponded to Example 4. Compared with Example 5 and Comparative Example 4, it is found that under the PPS resin with the same melt index, the elongation at break and the bending times of the acidified linear PPS resin are obviously better than those of ordinary PPS resin.

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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

一种超高断裂伸长率的PPS复合材料及其制备方法，包括如下重量份的成分：PPS树脂50-95份、蒙脱土0.5-8份、增韧剂3-30份和抗氧剂0.1-2份，所述PPS树脂为酸化线性PPS树脂。PPS复合材料中，通过在酸化PPS增韧体系中加入少量具有多层层状结构的蒙脱土，断裂伸长率可达到30％以上；且得到的PPS产品耐弯折性能优异；且得到产品外观好、颜色白。

Description

一种超高断裂伸长率的PPS复合材料及其制备方法 技术领域
本发明涉及高分子材料改性领域，尤其涉及一种超高断裂伸长率的PPS复合材料及其制备方法。
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。但是PPS的韧性较差，冲击强度和断裂伸长率都较低，尤其是断裂伸长率，即使经过增韧处理的PPS，其断裂伸长率一般也都在15％以下，难以进一步提高。
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超高断裂伸长率的PPS复合材料。
为实现上述目的，本发明所采取的技术方案为：一种超高断裂伸长率的PPS复合材料，包括如下重量份的成分：PPS树脂50-95份、蒙脱土0.5-8份、增韧剂3-30份和抗氧剂0.1-2份，所述PPS树脂为酸化线性PPS树脂。
普通合成的PPS端基难以控制，含有比如端氯基团、巯基钠、巯基等基团，反应活性不高。而酸化PPS树脂为合成过程中经过酸性溶液淋洗，相比较普通的PPS，其含有更多的羧基、巯基等反应性基团，因此与反应型增韧剂有更高的反应活性。本发明基于此选择酸化PPS作为基础树脂。
优选地，所述酸化线性PPS树脂在316℃、5kg测试条件下的熔融指数小于500g/10min。
优选地，所述的超高断裂伸长率的PPS复合材料，所述增韧剂为乙烯-环氧/酸酐型共聚物、乙烯-丙烯酸酯-环氧/酸酐型三元共聚物、乙烯/丁二烯-苯乙烯- 环氧/酸酐型三元共聚物中的至少一种。本申请增韧剂的选择中，乙烯-环氧/酸酐型共聚物代表：乙烯-环氧型共聚物或乙烯-酸酐型共聚物；乙烯-丙烯酸酯-环氧/酸酐型三元共聚物代表：乙烯-丙烯酸酯-环氧型三元共聚物或乙烯-丙烯酸酯-酸酐型三元共聚物；乙烯/丁二烯-苯乙烯-环氧/酸酐型三元共聚物代表：乙烯-苯乙烯-环氧型三元共聚物、乙烯-苯乙烯-酸酐型三元共聚物、丁二烯-苯乙烯-环氧型三元共聚物、丁二烯-苯乙烯-酸酐型三元共聚物。
优选地，所述的超高断裂伸长率的PPS复合材料，所述抗氧剂为受阻酚抗氧剂、受阻胺类抗氧剂中的至少一种，与亚磷酸酯类抗氧剂、硫代类抗氧剂中的至少一种组成的混合物。
更优选地，所述抗氧剂的重均分子量不小于300。
同时，本发明还提供一种所述超高断裂伸长率的PPS复合材料的制备方法，所述方法为：将各成分加入到高速混合机中混合，得到混合料，然后将混合料加入双螺杆挤出机中进行挤出、造粒，得到所述超高断裂伸长率的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℃。
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，增韧剂提高了蒙脱土与PPS树脂之间的界面结合力，通过在酸化PPS增韧体系中加入少量具有多层层状结构的蒙脱土，使得蒙脱土周围的PPS树脂存在一个无序的弹性过渡区域，在受力拉伸过程中，缠绕于蒙脱土周围的高分子链逐渐解缠结，大大提高了断裂伸长率，其断裂伸长率可达到30％以上；且得到产品外观好、颜色白。
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：
酸化线性PPS树脂1(PPS1)，熔融指数为120g/10min(316℃、5kg)，PPS 3412，浙江新和成特种材料有限公司；
酸化线性PPS树脂2(PPS2)，熔融指数为500g/10min(316℃、5kg)，PPS 3450，浙江新和成特种材料有限公司；
普通PPS树脂(PPS3)，熔融指数为500g/10min(316℃、5kg)，PPS 1150C，浙江新和成特种材料有限公司；
蒙脱土：NB-802(S)，江西伟普科技有限公司；
增韧剂：乙烯-丙烯酸酯-环氧型增韧剂，乙烯-丙烯酸甲酯-甲基丙烯酸缩水甘油酯(GMA)三元共聚物结构；LOTADER AX8900，法国阿科玛公司；
抗氧剂：抗氧剂1790(受阻酚抗氧剂)与抗氧剂168(亚磷酸酯抗氧剂)的混合物，二者混合重量比为2:1；
本申请实施例及对比例所述超高断裂伸长率的PPS复合材料通过以下方法制备所得：
将各成分加入到高速混合机中混合1分钟，得到混合料，然后将混合料加入双螺杆挤出机中进行挤出、造粒，得到所述超高断裂伸长率的PPS复合材料；其中，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℃。
本申请设置实施例1～8及对比例1～4，具体实施例1～8及对比例1～4中的成分及含量选择如表1所示，性能数据如表2所示：
表1实施例1～8和对比例1～4中的成分及含量
Figure PCTCN2020136307-appb-000001
Figure PCTCN2020136307-appb-000002
表2实施例1～8和对比例1～4性能数据
Figure PCTCN2020136307-appb-000003
弯折次数通过注塑0.8mm厚样条，反复从两边折弯，直至折断或出现明显裂纹，记录折断时的弯折次数。
从表2可以看出，将实施例4与对比例1、2、3进行对比发现，配方中不论缺少增韧剂、蒙脱土还是抗氧剂，均会使得相应的断裂伸长率与弯折次数显著下降；将实施例4与实施例5对比发现，当PPS树脂在316℃、5kg测试条件下的熔融指数小于500g/10min时，其对应实施例4的断裂伸长率与弯折次数均 高于实施例5；将实施例5与对比例4对比发现，同等熔融指数的PPS树脂下，酸化线性PPS树脂的断裂伸长率与弯折次数明显优于普通PPS树脂。
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 (7)

  1. 一种超高断裂伸长率的PPS复合材料，其特征在于，包括如下重量份的成分：PPS树脂50-95份、蒙脱土0.5-8份、增韧剂3-30份和抗氧剂0.1-2份，所述PPS树脂为酸化线性PPS树脂。
  2. 如权利要求1所述的超高断裂伸长率的PPS复合材料，其特征在于，所述酸化线性PPS树脂在316℃、5kg测试条件下的熔融指数小于500g/10min。
  3. 如权利要求1所述的超高断裂伸长率的PPS复合材料，其特征在于，所述增韧剂为乙烯-环氧/酸酐型共聚物、乙烯-丙烯酸酯-环氧/酸酐型三元共聚物、乙烯/丁二烯-苯乙烯-环氧/酸酐型三元共聚物中的至少一种。
  4. 如权利要求1所述的超高断裂伸长率的PPS复合材料，其特征在于，所述抗氧剂为受阻酚类抗氧剂、受阻胺类抗氧剂中的至少一种，与亚磷酸酯类抗氧剂、硫代类抗氧剂中的至少一种组成的混合物。
  5. 如权利要求4所述的超高断裂伸长率的PPS复合材料，其特征在于，所述抗氧剂的重均分子量不小于300。
  6. 一种如权利要求1～5任一项所述超高断裂伸长率的PPS复合材料的制备方法，其特征在于，所述方法为：将各成分加入到高速混合机中混合，得到混合料，然后将混合料加入双螺杆挤出机中进行挤出、造粒，得到所述超高断裂伸长率的PPS复合材料。
  7. 如权利要求6所述超高断裂伸长率的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℃。
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