废弃环氧树脂再生技术及应用研究
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摘要
热固性塑料作为塑料中的一大类,其制品已广泛渗入到生产和生活的各个领域,如用于制造建筑板材、汽车零部件、电子元器件、印制线路板(PCB)等。随着热固性塑料制品生产规模、需求不断扩大以及各类电子电器产品报废高峰期的到来,废弃热固性塑料,尤其是用于制造电子组件的环氧树脂塑料废弃量也随之剧增。靠传统的填埋或焚烧处理已不能满足可持续发展要求,然而热固性塑料不熔(溶)的特性又导致其不能像热塑性塑料那样采用重新加热熔融的方法将其再生利用。随着世界各国对电子废弃物资源化利用率要求越来越高,研发环境友好、经济可行的废弃环氧树脂再生技术势在必行,无论从资源循环利用还是环境保护角度看,都具有十分重要的意义。
本课题以电子元器件封装用固化环氧树脂的生产废弃料为研究对象,进行了废弃环氧树脂再生技术的研究,利用废弃环氧树脂回收粉料(以下简称废环氧粉)与聚氯乙烯(PVC),经共混、模压工艺制备了具有较好应用前景的复合材料,深入分析了复合材料结构和性能的关系及其界面结合机理,优化了材料的配方和工艺条件,并在工厂中试生产了一种实用的再生产品,拟最大限度地实现废弃环氧树脂的资源化,最后进一步开展了应用硅烷偶联剂提高复合材料性能的研究。
对废弃环氧树脂粉料的组成和性质进行了研究,采用红外光谱(FT-IR)、扫描电镜(SEM)和X射线能谱分析(EDS)等测试手段,分析得到该废环氧粉主要由形状不规则、表面粗糙的固化环氧树脂颗粒和球形的SiO2粉组成,粉料表面存在羟基、醚基、羰基、环氧基等活性和极性基团,并分析提出将废环氧粉与PVC共混,且以高填充量制备复合材料,具有一定的可行性。
采用模压成型法研究制备了废弃环氧树脂复合材料,研究了废环氧粉的粒径、填充量以及模压工艺参数对复合材料力学性能的影响,并找出最佳的模压工艺参数组合。结果表明：细粒径的废环氧粉对复合材料力学性能有利；随着废环氧粉填充量的增加,复合材料力学强度整体呈下降趋势,其中冲击强度下降最明显；当废环氧粉填充量达60%(质量分数,下同)时,在最佳模压工艺操作下,复合材料的拉仲强度、冲击强度、弯曲强度和弯曲模量分别为34.65MPa、5.2KJ/m2、60.94MPa和6.1GPa,远超过普通木塑复合材料性能。在高比例填充时(≥50%),废环氧粉已成为主体材料被利用,而PVC和其它添加剂只起到粘合剂的作用将废环氧粉粘合成一个整体,相对于目前将其作为低组分填料在热塑性塑料中的应用研究而言,本课题的研究在一定程度上有助于提高废环氧粉的再利用率,具有较好的实际意义。
探讨了废环氧粉/PVC复合材料的微观界面结构与性质,研究了在界面上可能发生的表面接枝反应并对反应过程进行了分析。将废环氧粉/PVC共混物经索氏抽提溶解掉物理吸附的PVC后,得到的残余物经FT-IR测试分析,结果证明PVC分子链在废环氧粉表面产生了化学接枝反应,该接枝反应可能是发生于废环氧粉中环氧基、羟基与PVC分子链间的亲核反应。说明废环氧粉与PVC界面间不但存在主要的次价键力作用,还存在强的主价键力作用,从而形成了多相性的整体网络结构,对复合效果起到关键的作用。SEM观察发现,废环氧粉和PVC基体间具有一定的界面相容性,两者接触面上有接枝交联点产生,但断面上界面处发生开裂和脱粘,说明界面结合力还有进一步提高的空间。
为了正确了解配方中各组分的作用及其相互影响,为接下来进一步投入生产试制产品作准备。本课题在转矩流变仪上模拟实际生产条件,研究了不同助剂和添加剂对废环氧粉/PVC共混体系流变性能的影响规律。研究表明：丙烯酸酯类加工助剂ACR-401主要在塑化初期促进体系塑化；抗冲改性剂CPE-135A在缩短塑化时间的同时,能提高材料的冲击强度但也使材料的拉伸强度降低,本课题以4-6份为宜；废环氧粉对润滑剂有较强吸附作用和削弱作用,并得到在CaSt2和石蜡两者等量配比时能发挥润滑协同效应,且此时材料的耐冲击性能最好。
在工厂进行了实用产品的生产研究,建立了采用锥形双螺杆挤出机挤出生产废弃环氧树脂再生产品的生产工艺流程,对各工艺环节和工艺参数进行了分析和优化。最终本课题成功生产了一种货运托盘,该托盘产品静载可达2000kg,动载为1000kg,已能达到市场上作为集装箱运输货物托盘的基本要求,而且还能满足货运托盘耐高温、耐冲击和耐酸度要求。对该生产线进行简单的成本效益分析表明,生产该托盘产品可带来一定的经济效益,同时还具有较好的环境效益和社会效益。
研究了偶联剂在改善废弃环氧树脂复合材料性能中的应用,以硅烷偶联剂KH-550为例,分析了其偶联作用机理,并与未添加偶联剂时复合材料的性能进行了对比分析。结果表明：KH-550不但能有效改善复合材料的力学性能,还有利于改进共混体系的塑化和加工热稳定性；SEM观察结果也说明KH-550提高了废环氧粉和PVC间的界面结合强度,因而宏观上表现出复合材料更佳的力学性能。添加偶联剂后,废环氧粉/PVC复合材料的拉伸强度和弯曲强度均超过了国内普通工程塑料的要求,进一步提升了复合材料的可应用领域和产品附加值。
对复合材料进行了动态热力学分析(DMA)和维卡软化点(VST)测试,结果说明：一方面,废环氧粉自身具有一定的增强耐热作用,因而使复合材料的储能模量、玻璃化转变温度和维卡软化点随废环氧粉含量的增加而提高；另一方面,废环氧粉与PVC相互作用形成了界面层,加入KH-550后使界面层强度提高,因而使复合材料的损耗模量和损耗因子峰值降低,复合材料的刚性和耐热性得到进一步改善。
本课题的研究成果不仅为废弃环氧树脂的再生利用提供了技术支持,而且为其它种类废弃热固性塑料的资源化技术研究提供了重要的科学依据。
Thermosetting plastic, as one large category of plastic, generally applied in structural parts, stress parts and functional parts, its products have been widely permeated into every realm of society, such as in producing of construction formwork, automotive components, electronic components, printed circuit boards (PCB) and so on. The amount of waste thermosetting plastic, especially cured epoxy resin which applied in manufacturing of electronic components, is increasing dramatically as the growing of production scale and demanding for thermosetting plastic, let alone the arrival of discarding peak of various electronic and electrical products. The waste is now mainly treated by simple landfill or incineration, which can not meet the requirement of sustainable development. Owing to non-melt and indissoluble properties of thermosetting plastic, its waste can not be recycled by re-melting method, which is commonly applied to reclaim waste thermoplastics. Either from resource-recycling, or from environmental protecting view of point, as the increasing level for utilization rate of e-waste around the world, it is an imperative issue to develop environment-friendly and economically feasible recycling technologies of waste cured epoxy resin.
In this paper the recycling and reutilization of waste cured epoxy resin have been studied. The research object in this thesis was the mold residue of epoxy molding compound, which was generated as industrial waste in the molding process of electronic components packages. A physical method has been applied for reusing waste cured epoxy resin powders (waste epoxy powders) into poly (vinyl chloride) (PVC) blend to prepare composites. The relationships between the structure and the properties of the composites have been studied, both of the formulations and process conditions have been optimized, meanwhile a regenerative product has been preliminary developed, with the aim to reclaim waste cured epoxy resin and maximize its reutilization. Furthermore, a coupling agent has also been applied and studied to improve properties of the composites.
The components and properties of waste epoxy powder have been studied by using infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and X-ray energy spectrum analysis (EDS). The results showed that waste epoxy powders mainly consisted of irregular cured epoxy resin particles with rough surface, and spherical silica powder. There are active and polar functional groups on the surface of the powder, such as hydroxyl groups, ether bonds, carbonyl, epoxy groups and so on, which make the powders have a certain activity. All the above functional groups make it possible to have both physical and chemical interactions between PVC chain and waste epoxy powders, which would contribute to miscibility between different phases in the blends, consequently the feasibility of blending waste epoxy powder with PVC resin, even at a high portion, was proposed.
In the laboratory stage, waste cured epoxy resin was reused to produce regenerative composites by compression molding method. The effects of filler size and content on the mechanical properties of composites were investigated; the optimized molding parameters have been explored. The results showed that the smaller size of waste epoxy powder was benefit to mechanical properties of the composites. Simply blending of waste epoxy powder without any surface modification and PVC would result in the significant decline of the mechanical properties of the composites, especial for the impact strength. When the powder content was up to 60wt%, under optimized molding conditions, waste epoxy powder/PVC composites showed excellent mechanical properties, with tensile strength of 34.65MPa, impact strength of 5.2 KJ/m2, flexural strength of 60.94MPa and flexural modulus of 6.1GPa, which displayed much better mechanical performance than ordinary wood-plastics composites. It should be noticed that when waste epoxy powders are added at high ratio (>50wt%), the powders can not be counted as a filler component of "PVC composites", but become the main material, while PVC and other additives only play the role of adhesive in the composites to bond the powders together. Compared to be just as a general filler in thermoplastic, waste epoxy powder can be the main material to be reused, which indicates a distinguished increment of reutilization rate and shows its good practical sense.
The structure and properties of the interface in waste epoxy powder/PVC composites have been studied; the mechanism of surface grafting reaction was also discussed. After dissolved PVC of the blends by Soxhlet extraction, the final residue was tested by FT-IR spectrometer, the results indicated that PVC chain had grafting onto the surface of waste epoxy powder, and concluded that the grafting reaction may attribute to nucleophilic substitution, which occur between hydroxyl or epoxy and PVC chain labile sites. A stable boundary layer structure was constructed, because there was not only the main physical adhesion (secondary bond force) existed, but also the strong chemical binding (primary bond force) existed between waste epoxy powder and PVC. SEM photos showed partly strong interfacial bonding, and crosslinking points on the interface, however, the interfacial cracking and debonding indicated that further improvement of interfacial bonding could be made in future.
In order to prepare for the next trial in workshop, it is very important to understand the roles of each component in formulations and their interactions to each other. The effects of different additives on rheological behavior of waste epoxy powder/PVC blends have been studied by torque rheometer. It can be concluded that the processing aid ACR-401 promotes the fusion of PVC mainly in initial stage; the impact modifier CPE-135A could shorten the fusion time, and improves the impact strength meanwhile decreases the tensile strength of the composites, in this experiment the proper content was 4-6 phr; the internal and external lubricating effects of the various lubricants are weakened by waste epoxy powder, due to its high portion and absorption of lubricants; When CaSt2 and wax with equivalent ratio are added, the best impact property of composites can be reached.
A practical product trial has been done in workshop, with the aim to develop a new process for making regeneration products by conical twin-screw extruder. In this paper, a kind of freight pallet has been developed successfully. The results of heap pressure, impact strength, heat and acid resistance tests showed that the produced pallet with static loading of 2000kg, dynamic loading of 1000kg, and good heat and acid resistance, all of which could meet the requirements for container transportation pallet. Results of simple cost-benefit analysis indicated that the developed regeneration technology would bring wonderful economic, social and eco-benefits.
Application of coulping agent on improving waste cured epoxy resin regeneration composites has been investigated. Take silane coupling agent KH-550 as an example, the effects of KH-550 and its coulping mechanism have been studied and analyzed. The results displayed that KH-550, could not only strengthen and toughen the composites, but also help improving plasticizing and processing stability of the blends; SEM photos also showed that KH-550 improved the interfacial bonding between waste epoxy powder and PVC, which leaded to better mechanical performance. Both of the tensile strength and flexural strength of the modified composites exceeded the requirements for national ordinary engineering plastic, which meant that higher value-added products could be manufactured and further scope of application would be prospected.
Dynamic mechanical thermal analysis(DMA) and Vicat softening temperature(VST) of the composites were measured. It can be concluded, in one aspect, the unmodified waste epoxy powder has some properties of strengthen and heat resistance, which could improve storage modulus, Tg and VST of the composites; in the other aspect, interfacial layer was formed owing to interactions between waste epoxy powder and PVC, and the interfacial layer was strengthened by adding KH-550, with declining trend of loss modulus and loss factor peak of the composites, it also indicated the improvement of rigidity and heat resistance of the composites after using KH-550.
本课题以电子元器件封装用固化环氧树脂的生产废弃料为研究对象,进行了废弃环氧树脂再生技术的研究,利用废弃环氧树脂回收粉料(以下简称废环氧粉)与聚氯乙烯(PVC),经共混、模压工艺制备了具有较好应用前景的复合材料,深入分析了复合材料结构和性能的关系及其界面结合机理,优化了材料的配方和工艺条件,并在工厂中试生产了一种实用的再生产品,拟最大限度地实现废弃环氧树脂的资源化,最后进一步开展了应用硅烷偶联剂提高复合材料性能的研究。
对废弃环氧树脂粉料的组成和性质进行了研究,采用红外光谱(FT-IR)、扫描电镜(SEM)和X射线能谱分析(EDS)等测试手段,分析得到该废环氧粉主要由形状不规则、表面粗糙的固化环氧树脂颗粒和球形的SiO2粉组成,粉料表面存在羟基、醚基、羰基、环氧基等活性和极性基团,并分析提出将废环氧粉与PVC共混,且以高填充量制备复合材料,具有一定的可行性。
采用模压成型法研究制备了废弃环氧树脂复合材料,研究了废环氧粉的粒径、填充量以及模压工艺参数对复合材料力学性能的影响,并找出最佳的模压工艺参数组合。结果表明：细粒径的废环氧粉对复合材料力学性能有利；随着废环氧粉填充量的增加,复合材料力学强度整体呈下降趋势,其中冲击强度下降最明显；当废环氧粉填充量达60%(质量分数,下同)时,在最佳模压工艺操作下,复合材料的拉仲强度、冲击强度、弯曲强度和弯曲模量分别为34.65MPa、5.2KJ/m2、60.94MPa和6.1GPa,远超过普通木塑复合材料性能。在高比例填充时(≥50%),废环氧粉已成为主体材料被利用,而PVC和其它添加剂只起到粘合剂的作用将废环氧粉粘合成一个整体,相对于目前将其作为低组分填料在热塑性塑料中的应用研究而言,本课题的研究在一定程度上有助于提高废环氧粉的再利用率,具有较好的实际意义。
探讨了废环氧粉/PVC复合材料的微观界面结构与性质,研究了在界面上可能发生的表面接枝反应并对反应过程进行了分析。将废环氧粉/PVC共混物经索氏抽提溶解掉物理吸附的PVC后,得到的残余物经FT-IR测试分析,结果证明PVC分子链在废环氧粉表面产生了化学接枝反应,该接枝反应可能是发生于废环氧粉中环氧基、羟基与PVC分子链间的亲核反应。说明废环氧粉与PVC界面间不但存在主要的次价键力作用,还存在强的主价键力作用,从而形成了多相性的整体网络结构,对复合效果起到关键的作用。SEM观察发现,废环氧粉和PVC基体间具有一定的界面相容性,两者接触面上有接枝交联点产生,但断面上界面处发生开裂和脱粘,说明界面结合力还有进一步提高的空间。
为了正确了解配方中各组分的作用及其相互影响,为接下来进一步投入生产试制产品作准备。本课题在转矩流变仪上模拟实际生产条件,研究了不同助剂和添加剂对废环氧粉/PVC共混体系流变性能的影响规律。研究表明：丙烯酸酯类加工助剂ACR-401主要在塑化初期促进体系塑化；抗冲改性剂CPE-135A在缩短塑化时间的同时,能提高材料的冲击强度但也使材料的拉伸强度降低,本课题以4-6份为宜；废环氧粉对润滑剂有较强吸附作用和削弱作用,并得到在CaSt2和石蜡两者等量配比时能发挥润滑协同效应,且此时材料的耐冲击性能最好。
在工厂进行了实用产品的生产研究,建立了采用锥形双螺杆挤出机挤出生产废弃环氧树脂再生产品的生产工艺流程,对各工艺环节和工艺参数进行了分析和优化。最终本课题成功生产了一种货运托盘,该托盘产品静载可达2000kg,动载为1000kg,已能达到市场上作为集装箱运输货物托盘的基本要求,而且还能满足货运托盘耐高温、耐冲击和耐酸度要求。对该生产线进行简单的成本效益分析表明,生产该托盘产品可带来一定的经济效益,同时还具有较好的环境效益和社会效益。
研究了偶联剂在改善废弃环氧树脂复合材料性能中的应用,以硅烷偶联剂KH-550为例,分析了其偶联作用机理,并与未添加偶联剂时复合材料的性能进行了对比分析。结果表明：KH-550不但能有效改善复合材料的力学性能,还有利于改进共混体系的塑化和加工热稳定性；SEM观察结果也说明KH-550提高了废环氧粉和PVC间的界面结合强度,因而宏观上表现出复合材料更佳的力学性能。添加偶联剂后,废环氧粉/PVC复合材料的拉伸强度和弯曲强度均超过了国内普通工程塑料的要求,进一步提升了复合材料的可应用领域和产品附加值。
对复合材料进行了动态热力学分析(DMA)和维卡软化点(VST)测试,结果说明：一方面,废环氧粉自身具有一定的增强耐热作用,因而使复合材料的储能模量、玻璃化转变温度和维卡软化点随废环氧粉含量的增加而提高；另一方面,废环氧粉与PVC相互作用形成了界面层,加入KH-550后使界面层强度提高,因而使复合材料的损耗模量和损耗因子峰值降低,复合材料的刚性和耐热性得到进一步改善。
本课题的研究成果不仅为废弃环氧树脂的再生利用提供了技术支持,而且为其它种类废弃热固性塑料的资源化技术研究提供了重要的科学依据。
Thermosetting plastic, as one large category of plastic, generally applied in structural parts, stress parts and functional parts, its products have been widely permeated into every realm of society, such as in producing of construction formwork, automotive components, electronic components, printed circuit boards (PCB) and so on. The amount of waste thermosetting plastic, especially cured epoxy resin which applied in manufacturing of electronic components, is increasing dramatically as the growing of production scale and demanding for thermosetting plastic, let alone the arrival of discarding peak of various electronic and electrical products. The waste is now mainly treated by simple landfill or incineration, which can not meet the requirement of sustainable development. Owing to non-melt and indissoluble properties of thermosetting plastic, its waste can not be recycled by re-melting method, which is commonly applied to reclaim waste thermoplastics. Either from resource-recycling, or from environmental protecting view of point, as the increasing level for utilization rate of e-waste around the world, it is an imperative issue to develop environment-friendly and economically feasible recycling technologies of waste cured epoxy resin.
In this paper the recycling and reutilization of waste cured epoxy resin have been studied. The research object in this thesis was the mold residue of epoxy molding compound, which was generated as industrial waste in the molding process of electronic components packages. A physical method has been applied for reusing waste cured epoxy resin powders (waste epoxy powders) into poly (vinyl chloride) (PVC) blend to prepare composites. The relationships between the structure and the properties of the composites have been studied, both of the formulations and process conditions have been optimized, meanwhile a regenerative product has been preliminary developed, with the aim to reclaim waste cured epoxy resin and maximize its reutilization. Furthermore, a coupling agent has also been applied and studied to improve properties of the composites.
The components and properties of waste epoxy powder have been studied by using infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and X-ray energy spectrum analysis (EDS). The results showed that waste epoxy powders mainly consisted of irregular cured epoxy resin particles with rough surface, and spherical silica powder. There are active and polar functional groups on the surface of the powder, such as hydroxyl groups, ether bonds, carbonyl, epoxy groups and so on, which make the powders have a certain activity. All the above functional groups make it possible to have both physical and chemical interactions between PVC chain and waste epoxy powders, which would contribute to miscibility between different phases in the blends, consequently the feasibility of blending waste epoxy powder with PVC resin, even at a high portion, was proposed.
In the laboratory stage, waste cured epoxy resin was reused to produce regenerative composites by compression molding method. The effects of filler size and content on the mechanical properties of composites were investigated; the optimized molding parameters have been explored. The results showed that the smaller size of waste epoxy powder was benefit to mechanical properties of the composites. Simply blending of waste epoxy powder without any surface modification and PVC would result in the significant decline of the mechanical properties of the composites, especial for the impact strength. When the powder content was up to 60wt%, under optimized molding conditions, waste epoxy powder/PVC composites showed excellent mechanical properties, with tensile strength of 34.65MPa, impact strength of 5.2 KJ/m2, flexural strength of 60.94MPa and flexural modulus of 6.1GPa, which displayed much better mechanical performance than ordinary wood-plastics composites. It should be noticed that when waste epoxy powders are added at high ratio (>50wt%), the powders can not be counted as a filler component of "PVC composites", but become the main material, while PVC and other additives only play the role of adhesive in the composites to bond the powders together. Compared to be just as a general filler in thermoplastic, waste epoxy powder can be the main material to be reused, which indicates a distinguished increment of reutilization rate and shows its good practical sense.
The structure and properties of the interface in waste epoxy powder/PVC composites have been studied; the mechanism of surface grafting reaction was also discussed. After dissolved PVC of the blends by Soxhlet extraction, the final residue was tested by FT-IR spectrometer, the results indicated that PVC chain had grafting onto the surface of waste epoxy powder, and concluded that the grafting reaction may attribute to nucleophilic substitution, which occur between hydroxyl or epoxy and PVC chain labile sites. A stable boundary layer structure was constructed, because there was not only the main physical adhesion (secondary bond force) existed, but also the strong chemical binding (primary bond force) existed between waste epoxy powder and PVC. SEM photos showed partly strong interfacial bonding, and crosslinking points on the interface, however, the interfacial cracking and debonding indicated that further improvement of interfacial bonding could be made in future.
In order to prepare for the next trial in workshop, it is very important to understand the roles of each component in formulations and their interactions to each other. The effects of different additives on rheological behavior of waste epoxy powder/PVC blends have been studied by torque rheometer. It can be concluded that the processing aid ACR-401 promotes the fusion of PVC mainly in initial stage; the impact modifier CPE-135A could shorten the fusion time, and improves the impact strength meanwhile decreases the tensile strength of the composites, in this experiment the proper content was 4-6 phr; the internal and external lubricating effects of the various lubricants are weakened by waste epoxy powder, due to its high portion and absorption of lubricants; When CaSt2 and wax with equivalent ratio are added, the best impact property of composites can be reached.
A practical product trial has been done in workshop, with the aim to develop a new process for making regeneration products by conical twin-screw extruder. In this paper, a kind of freight pallet has been developed successfully. The results of heap pressure, impact strength, heat and acid resistance tests showed that the produced pallet with static loading of 2000kg, dynamic loading of 1000kg, and good heat and acid resistance, all of which could meet the requirements for container transportation pallet. Results of simple cost-benefit analysis indicated that the developed regeneration technology would bring wonderful economic, social and eco-benefits.
Application of coulping agent on improving waste cured epoxy resin regeneration composites has been investigated. Take silane coupling agent KH-550 as an example, the effects of KH-550 and its coulping mechanism have been studied and analyzed. The results displayed that KH-550, could not only strengthen and toughen the composites, but also help improving plasticizing and processing stability of the blends; SEM photos also showed that KH-550 improved the interfacial bonding between waste epoxy powder and PVC, which leaded to better mechanical performance. Both of the tensile strength and flexural strength of the modified composites exceeded the requirements for national ordinary engineering plastic, which meant that higher value-added products could be manufactured and further scope of application would be prospected.
Dynamic mechanical thermal analysis(DMA) and Vicat softening temperature(VST) of the composites were measured. It can be concluded, in one aspect, the unmodified waste epoxy powder has some properties of strengthen and heat resistance, which could improve storage modulus, Tg and VST of the composites; in the other aspect, interfacial layer was formed owing to interactions between waste epoxy powder and PVC, and the interfacial layer was strengthened by adding KH-550, with declining trend of loss modulus and loss factor peak of the composites, it also indicated the improvement of rigidity and heat resistance of the composites after using KH-550.
引文
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