瓶级回收PET的流变及其抗熔滴纤维的性能研究
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摘要
聚对苯二甲酸乙二酯(PET)主要用于纤维生产,而在非纤维领域的应用则主要是制造食品、饮料的包装容器及薄膜。由于PET具有高强度、高刚性、良好的耐热性及尺寸稳定性等综合性能,PET瓶的生产近年来得到很大的发展,由此也带来了废弃PET瓶产生的环境污染。因此,回收利用废弃PET不但可以减少环境污染,而且可以降低生产成本,节省资源。此外,PET纤维属于熔融性可燃纤维,燃烧时容易形成熔滴,熔滴容易带来包括烫伤等在内的二次伤害,因此需要对PET纤维进行抗熔滴改性。
本文首先对瓶片PET和纤维级PET的流变性能进行了对比研究,然后在回收PET瓶片(rPET)基体中添加一种抗熔滴树脂进行共混,研究了rPET/抗熔滴树脂共混熔体的流变性能,最后制备了rPET/抗熔滴树脂共混纤维,将共混纤维进行后处理,共混纤维内部的硅树脂水解交联生成三维网状的热固性树脂,燃烧时该树脂对涤纶熔滴起到包覆、加速炭化并增加成炭量的作用,以达到抗熔滴的目的。本文通过熔体流动速率仪和RH7双柱型毛细管流变仪、SEM、FTIR、XRD、TG、DSC、KES-G1万能试验机以及抗熔滴测试等手段研究了共混熔体的流变性能、共混纤维及抗熔滴纤维的性能,主要研究内容和结论如下:
(1)利用RH7双柱型毛细管流变仪对PET瓶片与纺丝级PET熔体的流变性能进行了对比研究。讨论剪切速率和温度对表观粘度、非牛顿指数、结构粘度指数及粘流活化能的影响。结果表明:两种熔体都属于非牛顿假塑性流体,表观粘度都随着剪切速率和温度的增加而降低;在相同的温度下,瓶片PET熔体的非牛顿指数比纺丝级PET熔体的小,而结构粘度指数则比后者大;两种熔体的粘流活化能均随剪切速率的增大而减小。
(2)采用熔体流动速率仪和RH7双柱型毛细管流变仪对rPET、rPET/抗熔滴共混物熔体进行了流变性能的测试,结果表明:共混物的熔融指数随着抗熔滴树脂含量的增加而增大;表观粘度随着温度的升高和剪切速率的增加逐渐减小,熔体表现假塑性流体的特性;非牛顿指数n随着温度升高而逐渐增大;结构粘度指数随着温度的升高而逐渐降低。粘流活化能随剪切速率的增加而减小。在研究范围内,随着抗熔滴树脂含量的增加,共混物熔体的非牛顿指数越大,结构粘度指数、零切粘度和粘流活化能越小。
(3)SEM、XRD等研究表明,与纯rPET纤维相比,共混纤维的表面较粗糙,并且纤维的结晶结构并没有随着抗熔滴树脂的加入而发生变化,当抗熔滴树脂含量为5%时,共混纤维的结晶度下降到27.18%;万能试验机的结果显示,抗熔滴rPET纤维的断裂强度为134.49Mpa,低于纯rPET纤维的断裂强度。TG、DSC、抗熔滴性能等测试表明,随着抗熔滴树脂含量的增加,共混纤维的熔点和最大热分解速率逐渐变小,单位时间(1min)内熔滴数量减少,共混纤维的成炭量逐渐增加,抗熔滴性能逐渐增强。
Besides fiber production, polyethylene terephthalate (PET) is applied in food, beverages containers and packaging films manufacturing in large quantity. The reuse and recycling of bottle grade PET is of great importance in terms of environmental protection and resources saving. In addition, polyester fibers are thermoplastic and flammable, when burning they tend to form molten drops, which can bring burns and other secondary damages, so the modification of polyester fibers is necessary to improve the performance of anti-dripping.
In this paper, the rheological properties of bottle (rPET) and fiber grade polyester were analyzed and compared, then an anti-dripping resin was added to rPET resin and the rheological properties of melt blends were studied. At last, the rPET/anti-dripping resin blended fibers were prepared. The thermoplastic anti-dripping copolymer in polyester fiber will hydrolyze and crosslink into a three-dimensional thermosetting network after putting blended fibers in the water. The thermosetting anti-dripping resin can warp the melting drops and then accelerate charring, and thus the anti-dripping effect was achieved. The melt rheological properties of blends, performance of the blending fiber and anti-dripping fiber were studied by means of melt flow rate indexer, double capillary rheometer RH 7D, SEM, FTIR, XRD, TG, DSC, KES-G1 MULTI-PURPOSE TENSILE TESTER and anti-dropping tests.
The main research contents and conclusions are listed as follows:
(1) The melt rheological properties of bottle and fiber grade polyester were comparatively studied by double capillary rheometer RH 7D. The influence of shear rate and temperature on the apparent viscosity, non-Newtonian index, structural viscosity index, and activation energy for viscous flow were discussed. The results show that the two kinds of melt belong to non-Newtonian pseudoplastic fluid and the apparent viscosity decreases with the increasing of shear rate and temperature. At the same temperature, the non-Newtonian index of bottle grade melt is smaller than that of fiber grade polyester, but the structural viscosity index is larger than fiber grade polyester. The activation energy for viscous flow of two kinds of melt decreases with the increasing of shear rate.
(2) The melt rheological properties of rPET and blends of rPET/anti-dripping resin were studied by melt flow rate indexer and double capillary rheometer RH 7D. The results show that the melt index of rPET/anti-dripping resin blends increased along with increasing of the anti-dripping resin content; the apparent viscosity gradually decreased with raising temperature and shear rate, their melts showed non-Newtonian pseudoplastic fluid characteristics; the non-Newton index gradually increased with the increasing of temperature; the structural viscosity index decreases with the increasing of temperature. The activation energy for viscous flow of melt decreases with the increasing of shear rate. Within the framework of the study, with the increase of anti-dripping resin content, non-Newton index of rPET/anti-dripping resin blends melt increased, the structural viscosity index, zero shear viscosity and the activation energy of viscosity flow reduced.
(3) SEM, XRD results showed that the blending fibers' surface was rough compared with the traditional pure rPET fibers, and the crystal structure of blending fibers was unchanged with the addition of anti-dripping resin. The crystallinity decreased to 26% when the ratio of anti-dripping resin was 27.18%. The results of KES-G1 showed that the fracture intensity of anti-dripping polyester fibers was 134.49Mpa that was lower than pure polyester fibers'. TG, DSC and the anti-dripping performance test indicated that the melting point, the maximum thermal decomposition rate of the blending fibers and the number of drops of the anti-dripping fibers in unit time (1min) were decreased with the increase of anti-dripping resin content. The char residue of blending fibers was increased and the anti-dripping effect got gradually strengthened when raised the content of anti-dripping resin.
本文首先对瓶片PET和纤维级PET的流变性能进行了对比研究,然后在回收PET瓶片(rPET)基体中添加一种抗熔滴树脂进行共混,研究了rPET/抗熔滴树脂共混熔体的流变性能,最后制备了rPET/抗熔滴树脂共混纤维,将共混纤维进行后处理,共混纤维内部的硅树脂水解交联生成三维网状的热固性树脂,燃烧时该树脂对涤纶熔滴起到包覆、加速炭化并增加成炭量的作用,以达到抗熔滴的目的。本文通过熔体流动速率仪和RH7双柱型毛细管流变仪、SEM、FTIR、XRD、TG、DSC、KES-G1万能试验机以及抗熔滴测试等手段研究了共混熔体的流变性能、共混纤维及抗熔滴纤维的性能,主要研究内容和结论如下:
(1)利用RH7双柱型毛细管流变仪对PET瓶片与纺丝级PET熔体的流变性能进行了对比研究。讨论剪切速率和温度对表观粘度、非牛顿指数、结构粘度指数及粘流活化能的影响。结果表明:两种熔体都属于非牛顿假塑性流体,表观粘度都随着剪切速率和温度的增加而降低;在相同的温度下,瓶片PET熔体的非牛顿指数比纺丝级PET熔体的小,而结构粘度指数则比后者大;两种熔体的粘流活化能均随剪切速率的增大而减小。
(2)采用熔体流动速率仪和RH7双柱型毛细管流变仪对rPET、rPET/抗熔滴共混物熔体进行了流变性能的测试,结果表明:共混物的熔融指数随着抗熔滴树脂含量的增加而增大;表观粘度随着温度的升高和剪切速率的增加逐渐减小,熔体表现假塑性流体的特性;非牛顿指数n随着温度升高而逐渐增大;结构粘度指数随着温度的升高而逐渐降低。粘流活化能随剪切速率的增加而减小。在研究范围内,随着抗熔滴树脂含量的增加,共混物熔体的非牛顿指数越大,结构粘度指数、零切粘度和粘流活化能越小。
(3)SEM、XRD等研究表明,与纯rPET纤维相比,共混纤维的表面较粗糙,并且纤维的结晶结构并没有随着抗熔滴树脂的加入而发生变化,当抗熔滴树脂含量为5%时,共混纤维的结晶度下降到27.18%;万能试验机的结果显示,抗熔滴rPET纤维的断裂强度为134.49Mpa,低于纯rPET纤维的断裂强度。TG、DSC、抗熔滴性能等测试表明,随着抗熔滴树脂含量的增加,共混纤维的熔点和最大热分解速率逐渐变小,单位时间(1min)内熔滴数量减少,共混纤维的成炭量逐渐增加,抗熔滴性能逐渐增强。
Besides fiber production, polyethylene terephthalate (PET) is applied in food, beverages containers and packaging films manufacturing in large quantity. The reuse and recycling of bottle grade PET is of great importance in terms of environmental protection and resources saving. In addition, polyester fibers are thermoplastic and flammable, when burning they tend to form molten drops, which can bring burns and other secondary damages, so the modification of polyester fibers is necessary to improve the performance of anti-dripping.
In this paper, the rheological properties of bottle (rPET) and fiber grade polyester were analyzed and compared, then an anti-dripping resin was added to rPET resin and the rheological properties of melt blends were studied. At last, the rPET/anti-dripping resin blended fibers were prepared. The thermoplastic anti-dripping copolymer in polyester fiber will hydrolyze and crosslink into a three-dimensional thermosetting network after putting blended fibers in the water. The thermosetting anti-dripping resin can warp the melting drops and then accelerate charring, and thus the anti-dripping effect was achieved. The melt rheological properties of blends, performance of the blending fiber and anti-dripping fiber were studied by means of melt flow rate indexer, double capillary rheometer RH 7D, SEM, FTIR, XRD, TG, DSC, KES-G1 MULTI-PURPOSE TENSILE TESTER and anti-dropping tests.
The main research contents and conclusions are listed as follows:
(1) The melt rheological properties of bottle and fiber grade polyester were comparatively studied by double capillary rheometer RH 7D. The influence of shear rate and temperature on the apparent viscosity, non-Newtonian index, structural viscosity index, and activation energy for viscous flow were discussed. The results show that the two kinds of melt belong to non-Newtonian pseudoplastic fluid and the apparent viscosity decreases with the increasing of shear rate and temperature. At the same temperature, the non-Newtonian index of bottle grade melt is smaller than that of fiber grade polyester, but the structural viscosity index is larger than fiber grade polyester. The activation energy for viscous flow of two kinds of melt decreases with the increasing of shear rate.
(2) The melt rheological properties of rPET and blends of rPET/anti-dripping resin were studied by melt flow rate indexer and double capillary rheometer RH 7D. The results show that the melt index of rPET/anti-dripping resin blends increased along with increasing of the anti-dripping resin content; the apparent viscosity gradually decreased with raising temperature and shear rate, their melts showed non-Newtonian pseudoplastic fluid characteristics; the non-Newton index gradually increased with the increasing of temperature; the structural viscosity index decreases with the increasing of temperature. The activation energy for viscous flow of melt decreases with the increasing of shear rate. Within the framework of the study, with the increase of anti-dripping resin content, non-Newton index of rPET/anti-dripping resin blends melt increased, the structural viscosity index, zero shear viscosity and the activation energy of viscosity flow reduced.
(3) SEM, XRD results showed that the blending fibers' surface was rough compared with the traditional pure rPET fibers, and the crystal structure of blending fibers was unchanged with the addition of anti-dripping resin. The crystallinity decreased to 26% when the ratio of anti-dripping resin was 27.18%. The results of KES-G1 showed that the fracture intensity of anti-dripping polyester fibers was 134.49Mpa that was lower than pure polyester fibers'. TG, DSC and the anti-dripping performance test indicated that the melting point, the maximum thermal decomposition rate of the blending fibers and the number of drops of the anti-dripping fibers in unit time (1min) were decreased with the increase of anti-dripping resin content. The char residue of blending fibers was increased and the anti-dripping effect got gradually strengthened when raised the content of anti-dripping resin.
引文
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