长纤维热塑性复合材料的制备，性能和成型
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摘要
汽车轻量化是节约能源、减少尾气排放的重要措施之一。中国是一个汽车消费大国,但是在汽车材料轻量化上,还处于应用不足以及技术匮乏的现状。以聚丙烯PP为基体的LFT复合材料(长纤维增强热塑性片材,long fiber reinforced thermoplastics sheet),具有轻质高强的优点,并且易于制造和实现成本优化,正在逐步成为工程塑料和金属材料的替代品,已是汽车轻量化使用的聚合物基复合材料首选。本文以此为背景,开发LFT-PP制备、应用的成套技术,并作相关基础研究。
首先,通过改进单螺杆挤出机,建成年产200吨在线混合LFT中试生产线,提供了一种简便的制备LFT-PP片材的方法。开发过程中发现,采用强化混合螺杆、结合适宜的分流板和挤出口模,以及直接无捻粗纱,能够制备力学性能良好的LFT-PP复合材料。
以自由流动螺杆为研究对象,考察了螺杆转速、混合长度、螺槽深度等因素对于RTD曲线(residence time distribution, RTD),以及平均停留时间(mean residence time)和标准化方差的影响。采用Yeh模型拟合RTD数据,柱塞流反应器(Plug flow reactor)分数P以及连续搅拌槽反应器(continuous stirred tank reactor)死体积分数d用作模型的双参数,并且将工艺参数和螺杆结构与纤维断裂和分散进行了关联。在RTD数据分析基础上,通过对纤维受到的熔体剪切作用分析,结合在线挤出过程中不同结构螺杆的混合特性,探讨了纤维断裂和分散的原因。从而为装置的进一步工程放大,实施LFT的工业化制备奠定必要的技术基础。
再次,考察了基体,纤维以及界面结合等因素对LFT-PP力学性能的影响,纤维含量增加是提高LFT-PP力学性能最基本的因素；增加纤维长度能够明显改善强度和韧性,提高纤维分散能够改善刚性；界面改性剂PP-g-MAH能够提高LFT-PP的强度和刚性,但是会降低韧性。
采用Kelly-Tyson模型、Cox混合定律以及强度-应变关系,结合纤维长度因子以及纤维分散度因子,分别对LFT-PP的拉伸强度、拉伸模量和冲击强度进行了模拟,试验数据和模拟数据的一致性良好。
添加界面改性剂PP-g-MAH会导致LFT-PP韧性下降,组合增强和界面优化可改善韧性,探讨了组合增韧效应。研究表明,组合增强以及采用弱极性界面相容剂PP-g-KH570,能够得到强度韧性均衡的材料,特别是PP/LGF/Nano-CaCO3组合增强体系,能够兼顾高强度高刚性和高韧性。
最后,对LFT-PP产品的流动模塑成型进行研究,考察LFT-PP片材预热,模内冷却过程的温度变化,以及模具温度和成型压力对LFT-PP流动模压的影响。结合发动机防护罩和汽车前端模块的模压试制,探讨坯料设计对模压成型的影响,提供了LFT-PP流动模塑成型的关键参数,并且对成型过程中可能出现的缺陷进行讨论,可以作为LFT-PP制品成型工艺的指导。
利用自主开发的在线混合LFT生产线,成功研制了适用于发动机防护罩的LFT-PP材料,通过模压工艺优化,试制了合格的产品,并得到工业应用,自2006年以来,累计生产片材超过100吨。制备以及成型技术均获得相关企业认可,并用于某企业国产车型的多种零部件。
Lightweight of automobile is one of the effective ways for energy-saving and emissions-reducing. With the development of our society, there is a big amount of vehicle consumption in China. However, lightweight of automobile is still in the status of lacking of application and technology. Long fiber reinforced thermoplastics sheet with PP matrix (LFT-PP) has advantages of light mass, high strength, easy molding and low cost. It is becoming a substitute for engineering plastics and metal material. It is the first choice of polymer composites for lightweight of automobile. In this context, this article will do some fundamental study based on the development of LFT-PP and application of technology.
First of all, a simple technique of LFT-PP manufacture is proposed with LFT production line of 200 ton annually by using in-line compounding from modified single screw extruder. It was found that improved mixing screw combining of moderate spreader-plate and extrusion die with direct zero twist roving can be used to manufacture LFT-PP with better mechanical properties.
In the case of free flow screw, the influences of different conditions such as variation of screw speed, mixing length, and channel depth on RTD (residence time distribution), MRT (mean residence time) and normal variance are investigated. Yeh model is applied for fitting RTD, and Percent of Plug flow reactor P, and dead volume of continuous stirred tank reactor d are two parameters. Process parameters and screw configurations are associated with fiber breakage and dispersing by P and d. Based on RTD data analysis and mixing characterizations of in-line compounding with different geometry screw of free flow screw, grooved screw, and pinned screw, the mechanism available for fiber breakage and dispersing was given with fiber shear analysis applied by the melt. It is technical fundament for further enlargement and industrialization of LFT-PP.
Secondly, the influences of matrix, fiber, and the interface on LFT-PP mechanical properties are investigated. The results show adding fiber contents is key factor for increasing mechanical properties. Strength and toughness could be enhanced by fiber length addition; on the other hand, stiffness could be increased by fiber dispersion improvement. At the same time, interfacial agent PP-g-MAH would increase the strength and stiffness, whereas reduce toughness.
By combining with fiber length factor and fiber dispersion factor, the consistency of tensile strength, tensile modulus and impact strength were simulated with Kelly-Tyson's model simulation, Cox mixing principle, and strength-strain relation are applied in the study respectively. It is found that experiment status and simulation status are favorable.
Adding interface agent PP-g-MAH would reduce the toughness of LFT-PP; however, hybrid reinforcement and interfacial optimization can be applied for improving the toughness of LFT-PP. The study shows good balance of strength and toughness could be achieved by interface optimization of PP-g-KH570. Meanwhile, excellent integration of high strength, high stiffness and high toughness could be from hybrid composite of LFT-PP filled by Nano-CaCO3.
Finally, flow molding of LFT-PP is investigated with temperature change of pre-heating and cooling process. In addition, the influences of tooling temperature and molding pressure on LFT-PP flow molding are studied. Blank design is optimized with compression molding of engine under shield and car front module, and key parameters of LFT-PP flow molding is listed, at the same time possible shortages and its resolutions of flow molding are summarized.
LFT-PP fitting for engine under shields is manufactured from in-house LFT-PP production line by in-line compounding, and qualified parts is molded with process optimization. Since 2006, and total volume of LFT-PP has increased for more than 100 ton. It has good economic returns and social benefits. In addition, manufacturing capacities and molding technique are accepted by cooperative companies. It is applied for many parts on specific domestic cars.
首先,通过改进单螺杆挤出机,建成年产200吨在线混合LFT中试生产线,提供了一种简便的制备LFT-PP片材的方法。开发过程中发现,采用强化混合螺杆、结合适宜的分流板和挤出口模,以及直接无捻粗纱,能够制备力学性能良好的LFT-PP复合材料。
以自由流动螺杆为研究对象,考察了螺杆转速、混合长度、螺槽深度等因素对于RTD曲线(residence time distribution, RTD),以及平均停留时间(mean residence time)和标准化方差的影响。采用Yeh模型拟合RTD数据,柱塞流反应器(Plug flow reactor)分数P以及连续搅拌槽反应器(continuous stirred tank reactor)死体积分数d用作模型的双参数,并且将工艺参数和螺杆结构与纤维断裂和分散进行了关联。在RTD数据分析基础上,通过对纤维受到的熔体剪切作用分析,结合在线挤出过程中不同结构螺杆的混合特性,探讨了纤维断裂和分散的原因。从而为装置的进一步工程放大,实施LFT的工业化制备奠定必要的技术基础。
再次,考察了基体,纤维以及界面结合等因素对LFT-PP力学性能的影响,纤维含量增加是提高LFT-PP力学性能最基本的因素；增加纤维长度能够明显改善强度和韧性,提高纤维分散能够改善刚性；界面改性剂PP-g-MAH能够提高LFT-PP的强度和刚性,但是会降低韧性。
采用Kelly-Tyson模型、Cox混合定律以及强度-应变关系,结合纤维长度因子以及纤维分散度因子,分别对LFT-PP的拉伸强度、拉伸模量和冲击强度进行了模拟,试验数据和模拟数据的一致性良好。
添加界面改性剂PP-g-MAH会导致LFT-PP韧性下降,组合增强和界面优化可改善韧性,探讨了组合增韧效应。研究表明,组合增强以及采用弱极性界面相容剂PP-g-KH570,能够得到强度韧性均衡的材料,特别是PP/LGF/Nano-CaCO3组合增强体系,能够兼顾高强度高刚性和高韧性。
最后,对LFT-PP产品的流动模塑成型进行研究,考察LFT-PP片材预热,模内冷却过程的温度变化,以及模具温度和成型压力对LFT-PP流动模压的影响。结合发动机防护罩和汽车前端模块的模压试制,探讨坯料设计对模压成型的影响,提供了LFT-PP流动模塑成型的关键参数,并且对成型过程中可能出现的缺陷进行讨论,可以作为LFT-PP制品成型工艺的指导。
利用自主开发的在线混合LFT生产线,成功研制了适用于发动机防护罩的LFT-PP材料,通过模压工艺优化,试制了合格的产品,并得到工业应用,自2006年以来,累计生产片材超过100吨。制备以及成型技术均获得相关企业认可,并用于某企业国产车型的多种零部件。
Lightweight of automobile is one of the effective ways for energy-saving and emissions-reducing. With the development of our society, there is a big amount of vehicle consumption in China. However, lightweight of automobile is still in the status of lacking of application and technology. Long fiber reinforced thermoplastics sheet with PP matrix (LFT-PP) has advantages of light mass, high strength, easy molding and low cost. It is becoming a substitute for engineering plastics and metal material. It is the first choice of polymer composites for lightweight of automobile. In this context, this article will do some fundamental study based on the development of LFT-PP and application of technology.
First of all, a simple technique of LFT-PP manufacture is proposed with LFT production line of 200 ton annually by using in-line compounding from modified single screw extruder. It was found that improved mixing screw combining of moderate spreader-plate and extrusion die with direct zero twist roving can be used to manufacture LFT-PP with better mechanical properties.
In the case of free flow screw, the influences of different conditions such as variation of screw speed, mixing length, and channel depth on RTD (residence time distribution), MRT (mean residence time) and normal variance are investigated. Yeh model is applied for fitting RTD, and Percent of Plug flow reactor P, and dead volume of continuous stirred tank reactor d are two parameters. Process parameters and screw configurations are associated with fiber breakage and dispersing by P and d. Based on RTD data analysis and mixing characterizations of in-line compounding with different geometry screw of free flow screw, grooved screw, and pinned screw, the mechanism available for fiber breakage and dispersing was given with fiber shear analysis applied by the melt. It is technical fundament for further enlargement and industrialization of LFT-PP.
Secondly, the influences of matrix, fiber, and the interface on LFT-PP mechanical properties are investigated. The results show adding fiber contents is key factor for increasing mechanical properties. Strength and toughness could be enhanced by fiber length addition; on the other hand, stiffness could be increased by fiber dispersion improvement. At the same time, interfacial agent PP-g-MAH would increase the strength and stiffness, whereas reduce toughness.
By combining with fiber length factor and fiber dispersion factor, the consistency of tensile strength, tensile modulus and impact strength were simulated with Kelly-Tyson's model simulation, Cox mixing principle, and strength-strain relation are applied in the study respectively. It is found that experiment status and simulation status are favorable.
Adding interface agent PP-g-MAH would reduce the toughness of LFT-PP; however, hybrid reinforcement and interfacial optimization can be applied for improving the toughness of LFT-PP. The study shows good balance of strength and toughness could be achieved by interface optimization of PP-g-KH570. Meanwhile, excellent integration of high strength, high stiffness and high toughness could be from hybrid composite of LFT-PP filled by Nano-CaCO3.
Finally, flow molding of LFT-PP is investigated with temperature change of pre-heating and cooling process. In addition, the influences of tooling temperature and molding pressure on LFT-PP flow molding are studied. Blank design is optimized with compression molding of engine under shield and car front module, and key parameters of LFT-PP flow molding is listed, at the same time possible shortages and its resolutions of flow molding are summarized.
LFT-PP fitting for engine under shields is manufactured from in-house LFT-PP production line by in-line compounding, and qualified parts is molded with process optimization. Since 2006, and total volume of LFT-PP has increased for more than 100 ton. It has good economic returns and social benefits. In addition, manufacturing capacities and molding technique are accepted by cooperative companies. It is applied for many parts on specific domestic cars.
引文
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