使用高压釜制备聚丙烯发泡珠粒（EPP）的理论及技术
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摘要
珠粒模塑发泡成型技术组合了预发泡珠粒生产技术和模压熔结成型技术，是目前唯一能生产各种复杂形状的低密度发泡制品的技术，这是挤出发泡成型技术和注塑发泡成型技术所无法实现的。珠粒模塑发泡制品具有含有大量气体的闭孔结构，故珠粒模塑发泡制品虽然质轻，但具有优异的抗冲击性能和隔热性能，被广泛应用于汽车制造、包装运输、建筑工程、化工工程、运动休闲等领域。聚丙烯发泡珠粒（EPP）模塑制品的使用温度高，且具有一系列优异的力学性能，因此，EPP模塑制品的性价比高，市场需求不断增长，尤其在汽车制造业的应用备受关注。然而，目前极少关于EPP制备技术的研究，尤其是关于EPP制备过程控制机理的研究。
本研究以制得具有适合于蒸汽模塑成型的双峰熔融结晶特性的、高发泡倍率的EPP为目的，设计和研制了制备EPP的高压釜实验装置，其中，采用可更换的排料口模组件设计，首次将释压条件的影响考虑到EPP制备过程中。通过系统地研究关键工艺参数对EPP的发泡效果和熔融结晶特性的影响，探讨了EPP制备过程的控制机理，为丰富和发展EPP制备技术的理论与实践提供了可资借鉴的第一手资料。
为了寻求既具有良好的发泡加工性能，同时经过发泡后具有双峰熔融结晶特性的聚丙烯（PP）材料，作为制备EPP的原料，采用EPP工业生产中常用的加工工艺条件，以CO_2作为发泡剂，对四种不同分子链结构的PP材料的发泡行为及其发泡试样的熔融结晶特性进行了研究。实验结果表明：支化PP分子链的高缠结程度有利于改善体系的发泡性能和稳定泡孔结构；线性PP的低熔体强度是导致其发泡性能极差的原因；嵌段共聚PP具有较高的结晶度，不利于CO_2的扩散和溶解；无规共聚PP分子链的规整性低，从而结晶度低，使CO_2更易于扩散和溶解。而四种PP材料经过发泡后，只有无规共聚PP呈现出适合于蒸汽模塑成型的双峰熔融结晶特性。
从发泡过程中气泡成核与气泡长大的相互竞争关系的角度出发，讨论了成核口模的压降速率和压力降对气泡成核的影响。通过建立PP颗粒在成核口模中的流动模型，分析了口模尺寸、系统流率和体系性质等参数对口模压降速率和压力降的影响，从而总结出获得高压降速率和压力降的途径。
以CO_2作为发泡剂，采用高压釜实验装置制备EPP的研究中，在最佳工艺条件下所获得的EPP的发泡倍率为15倍，泡孔密度为3.47×10~8个/cm~3，且泡孔尺寸呈现双峰特性，同时，EPP的双峰熔融结晶特性与JSP公司生产的EPP相当。通过分析加工压力、温度、气体饱和时间和释压条件（口模尺寸）对EPP制备过程的影响，发现：EPP的发泡倍率和泡孔密度随着加工压力的升高而提高；随着加工温度的升高，EPP的发泡倍率提高，但泡孔密度下降；随着加工压力的升高，EPP两个吸热峰熔点之间的温度差减小，低温吸热峰与高温吸热峰的面积比增加；随着加工温度的升高，EPP低温吸热峰与高温吸热峰的面积比增加，在高压下两个吸热峰熔点之间的温度差增加，但随着加工压力的下降，两个吸热峰熔点之间的温度差变化不大；随着气体饱和时间的增加，低温吸热峰与高温吸热峰的面积比减小，但两个吸热峰熔点之间的温度差变化不大。确定加工压力、温度和气体饱和时间后，保持口模直径不变，随着口模长度的增加（口模的压力降增加），EPP的发泡倍率下降，低温吸热峰与高温吸热峰的面积比减小，泡孔密度和两个吸热峰熔点之间的温度差变化不大；而当口模的压力降相同时，随着口模的压降速率降低，EPP的发泡倍率和泡孔密度均下降，低温吸热峰与高温吸热峰的面积比时而增加时而减小，两个吸热峰熔点之间的温度差变化不大。
In essence, bead foaming technology comprises two main processes: foamed beadfabrication and steam-cheating molding. Bead foaming technology is an innovativetechnology in the plastic foam industry that allows the manufacture of low-density polymericfoam products of a variety of shapes and densities, which is not achievable with conventionalfoam extrusion or injection mold processes. Owing to their high expansion ratio andclosed-cell morphologies, articles of molded foam beads are very light-in-weight and possesssuperior impact and thermal insulation properties. Because of these excellent properties,molded foam bead articles have been widely adopted in a broad spectrum of industries,including the automotive, transportation, construction, chemical engineering, sports,recreation, etc. An example of bead foams is expanded polypropylene (EPP). Products madewith EPP have high service temperature and excellent mechanical properties. Because of itslow cost-to-performance ratio, the market of EPP products has been consistently expanding,in particular, in the automotive industry. Despite its potential, research about themanufacturing technology of EPP, in particular, in the aspects of foaming mechanism andprocessing control of bead manufacturing is still very limited.
The goal of this research is to elucidate factors during the fabrication of EPP that wouldlead to the production of its double-peak melting/crystallization characteristic, which willaffect the sintering behaviour of the beads in the subsequent steam-chest molding process andthe quality of the final foamed bead products. A lab-scale autoclave EPP foaming system wasdesigned and constructed to facilitate the study of the influence of various critical processingparameters on EPP fabrication. This autoclave system adopted a modular die design to allowthe study of the influence of pressure drop and pressure drop rate during the depressurizationprocess of EPP manufacturing. Through the designed lab-scale autoclave EPP foaming system,this research investigated the effect and correlation of a variety of processing parameters onthe manipulation and control of the foaming properties and melting/crystallization behaviourof the EPP beads, thus explores the control mechanism of the EPP fabrication process. Thishelps to provide reference for further study of the theory and practice of EPP fabricationtechnology.
The double-peak melting/crystallization characteristic of EPP is a requisite for properbead sintering in the steam-chest molding process of bead foaming technology. This researchexamined the foaming behaviour of four different types of PP (branched, linear, blockcopolymer, and random copolymer PP) using a batch foaming visualization system in order to identify suitable EPP materials. As illustrated from the foam visualization experiments, themolecular chain structure significantly affected the foaming behaviour of PP. The high degreeof molecular chain entanglement of branched PP helped cell stabilization during foamexpansion. Linear PP had low melt strength, and hence, the foamability of this PP wasrelatively poor. The high crystallinity of block copolymer PP had hindered the diffusion anddissolution of carbon dioxide (CO_2). Random copolymer PP had relatively low degree ofmolecular chain regularity and crystallinity, allowing CO_2to dissolve into the matrix easily.Amongst the four types of PP examined, only random copolymer PP had yielded awell-distributed double-peak melting/crystallization characteristic after the foaming process.Based on the results, random copolymer PP is a suitable candidate for EPP fabrication.
Similar to other foaming techniques, cell nucleation and cell growth are two competingprocesses in EPP bead fabrication. Through the use of dies of different diameters (D) andlengths (L), this work investigated the correlation between pressure drop, pressure drop rate,cell nucleation rate and cell density. Through the study of the flow and depressurizationcharacteristic in the autoclave system, the model regarding the flow of PP pellets within thedie was established, and hence the effects of die geometry, volumetric flow rate and systemproperties on the pressure drop and pressure drop rate were analyzed. The requirements ofachieving high pressure drop and pressure drop rate for the production of EPP with high celldensity and expansion ratios were also identified.
With the designed lab-scale autoclave EPP foaming system and using CO_2as theblowing agent, EPP beads of different cell densities, expansion ratios, and double-peakmelting/crystallization characteristic were attained through varying processing parameters. Inthis work, the EPP beads manufactured under the optimized processing condition possessedan expansion ratio of15-fold, a cell density of3.47×10~8cells/cm3, bi-cellular foam structure,and melting/crystallization behaviour that equivalent to the EPP produced by JSP. Throughthe study of the effects of saturation pressure, saturation temperature, saturation time anddepressurization conditions (i.e., die geometry) on the EPP fabrication, the following resultscan be drawn: The expansion ratio and cell density increased as the saturation pressure. As thesaturation temperature increased, the expansion ratio increased while the cell densitydecreased. As the saturation pressure increased, the temperature difference of the double-peakdecreased, while the area ratio between low-melting-peak and high-melting-peak increased.As the saturation temperature increased, the area ratio between low-melting-peak andhigh-melting-peak increased, and the temperature difference of the double-peak increasedwhen the saturation pressure was high. However, as the saturation pressure decreased, the influence of the saturation temperature on the temperature difference of the double-peak wasnot obvous. As the saturation time increased, the area ratio between low-melting-peak andhigh-melting-peak decreased while the temperature difference of the double-peak changedlittle. When the saturation pressure, saturation temperature and saturation time were fixed, byincreasing the length of the dies with the same diameter (i.e., increasing the pressure drop),both the expansion ratio and the area ratio between low-melting-peak and high-melting-peakdecreased, while the cell density and the temperature difference of the double-peak changedlittle. By decreasing the pressure drop rate of the dies with the same pressure drop, both theexpansion ratio and cell density decreased, the area ratio between low-melting-peak andhigh-melting-peak sometimes increased and sometimes decreased, and the temperaturedifference of the double-peak changed little.
本研究以制得具有适合于蒸汽模塑成型的双峰熔融结晶特性的、高发泡倍率的EPP为目的，设计和研制了制备EPP的高压釜实验装置，其中，采用可更换的排料口模组件设计，首次将释压条件的影响考虑到EPP制备过程中。通过系统地研究关键工艺参数对EPP的发泡效果和熔融结晶特性的影响，探讨了EPP制备过程的控制机理，为丰富和发展EPP制备技术的理论与实践提供了可资借鉴的第一手资料。
为了寻求既具有良好的发泡加工性能，同时经过发泡后具有双峰熔融结晶特性的聚丙烯（PP）材料，作为制备EPP的原料，采用EPP工业生产中常用的加工工艺条件，以CO_2作为发泡剂，对四种不同分子链结构的PP材料的发泡行为及其发泡试样的熔融结晶特性进行了研究。实验结果表明：支化PP分子链的高缠结程度有利于改善体系的发泡性能和稳定泡孔结构；线性PP的低熔体强度是导致其发泡性能极差的原因；嵌段共聚PP具有较高的结晶度，不利于CO_2的扩散和溶解；无规共聚PP分子链的规整性低，从而结晶度低，使CO_2更易于扩散和溶解。而四种PP材料经过发泡后，只有无规共聚PP呈现出适合于蒸汽模塑成型的双峰熔融结晶特性。
从发泡过程中气泡成核与气泡长大的相互竞争关系的角度出发，讨论了成核口模的压降速率和压力降对气泡成核的影响。通过建立PP颗粒在成核口模中的流动模型，分析了口模尺寸、系统流率和体系性质等参数对口模压降速率和压力降的影响，从而总结出获得高压降速率和压力降的途径。
以CO_2作为发泡剂，采用高压釜实验装置制备EPP的研究中，在最佳工艺条件下所获得的EPP的发泡倍率为15倍，泡孔密度为3.47×10~8个/cm~3，且泡孔尺寸呈现双峰特性，同时，EPP的双峰熔融结晶特性与JSP公司生产的EPP相当。通过分析加工压力、温度、气体饱和时间和释压条件（口模尺寸）对EPP制备过程的影响，发现：EPP的发泡倍率和泡孔密度随着加工压力的升高而提高；随着加工温度的升高，EPP的发泡倍率提高，但泡孔密度下降；随着加工压力的升高，EPP两个吸热峰熔点之间的温度差减小，低温吸热峰与高温吸热峰的面积比增加；随着加工温度的升高，EPP低温吸热峰与高温吸热峰的面积比增加，在高压下两个吸热峰熔点之间的温度差增加，但随着加工压力的下降，两个吸热峰熔点之间的温度差变化不大；随着气体饱和时间的增加，低温吸热峰与高温吸热峰的面积比减小，但两个吸热峰熔点之间的温度差变化不大。确定加工压力、温度和气体饱和时间后，保持口模直径不变，随着口模长度的增加（口模的压力降增加），EPP的发泡倍率下降，低温吸热峰与高温吸热峰的面积比减小，泡孔密度和两个吸热峰熔点之间的温度差变化不大；而当口模的压力降相同时，随着口模的压降速率降低，EPP的发泡倍率和泡孔密度均下降，低温吸热峰与高温吸热峰的面积比时而增加时而减小，两个吸热峰熔点之间的温度差变化不大。
In essence, bead foaming technology comprises two main processes: foamed beadfabrication and steam-cheating molding. Bead foaming technology is an innovativetechnology in the plastic foam industry that allows the manufacture of low-density polymericfoam products of a variety of shapes and densities, which is not achievable with conventionalfoam extrusion or injection mold processes. Owing to their high expansion ratio andclosed-cell morphologies, articles of molded foam beads are very light-in-weight and possesssuperior impact and thermal insulation properties. Because of these excellent properties,molded foam bead articles have been widely adopted in a broad spectrum of industries,including the automotive, transportation, construction, chemical engineering, sports,recreation, etc. An example of bead foams is expanded polypropylene (EPP). Products madewith EPP have high service temperature and excellent mechanical properties. Because of itslow cost-to-performance ratio, the market of EPP products has been consistently expanding,in particular, in the automotive industry. Despite its potential, research about themanufacturing technology of EPP, in particular, in the aspects of foaming mechanism andprocessing control of bead manufacturing is still very limited.
The goal of this research is to elucidate factors during the fabrication of EPP that wouldlead to the production of its double-peak melting/crystallization characteristic, which willaffect the sintering behaviour of the beads in the subsequent steam-chest molding process andthe quality of the final foamed bead products. A lab-scale autoclave EPP foaming system wasdesigned and constructed to facilitate the study of the influence of various critical processingparameters on EPP fabrication. This autoclave system adopted a modular die design to allowthe study of the influence of pressure drop and pressure drop rate during the depressurizationprocess of EPP manufacturing. Through the designed lab-scale autoclave EPP foaming system,this research investigated the effect and correlation of a variety of processing parameters onthe manipulation and control of the foaming properties and melting/crystallization behaviourof the EPP beads, thus explores the control mechanism of the EPP fabrication process. Thishelps to provide reference for further study of the theory and practice of EPP fabricationtechnology.
The double-peak melting/crystallization characteristic of EPP is a requisite for properbead sintering in the steam-chest molding process of bead foaming technology. This researchexamined the foaming behaviour of four different types of PP (branched, linear, blockcopolymer, and random copolymer PP) using a batch foaming visualization system in order to identify suitable EPP materials. As illustrated from the foam visualization experiments, themolecular chain structure significantly affected the foaming behaviour of PP. The high degreeof molecular chain entanglement of branched PP helped cell stabilization during foamexpansion. Linear PP had low melt strength, and hence, the foamability of this PP wasrelatively poor. The high crystallinity of block copolymer PP had hindered the diffusion anddissolution of carbon dioxide (CO_2). Random copolymer PP had relatively low degree ofmolecular chain regularity and crystallinity, allowing CO_2to dissolve into the matrix easily.Amongst the four types of PP examined, only random copolymer PP had yielded awell-distributed double-peak melting/crystallization characteristic after the foaming process.Based on the results, random copolymer PP is a suitable candidate for EPP fabrication.
Similar to other foaming techniques, cell nucleation and cell growth are two competingprocesses in EPP bead fabrication. Through the use of dies of different diameters (D) andlengths (L), this work investigated the correlation between pressure drop, pressure drop rate,cell nucleation rate and cell density. Through the study of the flow and depressurizationcharacteristic in the autoclave system, the model regarding the flow of PP pellets within thedie was established, and hence the effects of die geometry, volumetric flow rate and systemproperties on the pressure drop and pressure drop rate were analyzed. The requirements ofachieving high pressure drop and pressure drop rate for the production of EPP with high celldensity and expansion ratios were also identified.
With the designed lab-scale autoclave EPP foaming system and using CO_2as theblowing agent, EPP beads of different cell densities, expansion ratios, and double-peakmelting/crystallization characteristic were attained through varying processing parameters. Inthis work, the EPP beads manufactured under the optimized processing condition possessedan expansion ratio of15-fold, a cell density of3.47×10~8cells/cm3, bi-cellular foam structure,and melting/crystallization behaviour that equivalent to the EPP produced by JSP. Throughthe study of the effects of saturation pressure, saturation temperature, saturation time anddepressurization conditions (i.e., die geometry) on the EPP fabrication, the following resultscan be drawn: The expansion ratio and cell density increased as the saturation pressure. As thesaturation temperature increased, the expansion ratio increased while the cell densitydecreased. As the saturation pressure increased, the temperature difference of the double-peakdecreased, while the area ratio between low-melting-peak and high-melting-peak increased.As the saturation temperature increased, the area ratio between low-melting-peak andhigh-melting-peak increased, and the temperature difference of the double-peak increasedwhen the saturation pressure was high. However, as the saturation pressure decreased, the influence of the saturation temperature on the temperature difference of the double-peak wasnot obvous. As the saturation time increased, the area ratio between low-melting-peak andhigh-melting-peak decreased while the temperature difference of the double-peak changedlittle. When the saturation pressure, saturation temperature and saturation time were fixed, byincreasing the length of the dies with the same diameter (i.e., increasing the pressure drop),both the expansion ratio and the area ratio between low-melting-peak and high-melting-peakdecreased, while the cell density and the temperature difference of the double-peak changedlittle. By decreasing the pressure drop rate of the dies with the same pressure drop, both theexpansion ratio and cell density decreased, the area ratio between low-melting-peak andhigh-melting-peak sometimes increased and sometimes decreased, and the temperaturedifference of the double-peak changed little.
引文
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