原位熔融缩聚改性的PET及其CO_2发泡过程研究
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摘要
聚对苯二甲酸乙二醇酯(简称PET)在工程塑料领域有着广泛的应用,轻量化是工程塑料应用领域对材料所提出的新要求,因此具有优异机械和物理性能的PET发泡材料备受关注。常规PET一般是分子量相对较低且分子量分布相对较窄的线性聚合物,熔体强度较低,发泡过程中气泡在PET熔体中的生长过程容易发生泡孔壁的破裂和泡孔的塌陷,因此发泡用PET基料必须通过改性以提高熔体强度；同时,PET具有强吸水性,在熔融过程中容易发生热、氧降解和水解,导致分子量急剧下降,熔体强度大幅降低,也不利于PET发泡。本文成功制备了发泡性能优异的改性PET；基于CO2在改性PET熔体中溶解度和改性PET熔体在C02环境下表面张力等基础数据的测定,模拟分析了改性PET的CO2发泡成核过程；创新提出了超临界CO2辅助的改性PET增粘和发泡一体化过程,并实验证实了其可行性和优越性,具体如下：
首先,采用原位聚合改性的方法制备了具有较高熔体强度改性PET。选取醇N和酸M两种多官能团化合物为第三单体原位聚合分别制备了具有长链支化结构的醇改性PET和酸改性PET,有效地提高了聚酯的熔体强度,当醇N的添加含量0.3wt%、酸M的添加含量0.8wt%时,改性PET的特性粘度Ⅳ从常规线性PET的0.659dL/g分别提高到0.860dL/g和0.865dL/g,熔融流动指数MFI从29.3g/10min分别减小到15.1g/lOmin和15.0g/10min。两种改性PET的结晶温度Tc,结晶焓△Hc,熔点Tm,,熔融焓△Hm均有所降低,复数粘度η*、储能模量G’和耗能模量G”较未改性PET均有显著提高,且呈现出剪切变稀的流动特性。以超临界CO2为发泡剂的间歇熔融发泡实验表明,两种改性PET在发泡温度265～280℃范围内可成功制备泡孔直径35～57μm、泡孔密度106～107cells/cm3的发泡样品,而同样条件下线性PET无法发泡,另外醇改性PET的发泡样品泡孔尺寸较酸改性PET的小、泡孔密度高。
其次,通过高温高压磁悬浮天平(MSB)测定表观溶解度、高温高压视窗釜进行溶胀度校正的方法研究了CO2在PET熔体中的溶解度。考察了温度、CO2压力对改性前后PET在CO2环境中的溶胀度和CO2溶解度的影响,结果表明,PET在CO2环境中的溶胀度和CO2溶解度均随温度的增加而减小,随压力增加而增加,但高压下溶胀度的增加趋势减缓并趋于某定值。与常规线性PET相比,改性PET具有较小的溶胀度和溶解度。在250～280℃,1～6MPa下CO2在PET熔体中的溶解行为符合亨利定律,4-6MPa下溶解度具有10-2(gCO2/g PET melt)的量级。利用S-L方程对PET熔体在1～14MPa下CO2中,的溶胀度进行了拟合,进而预测了较高压力下的CO2在PET熔体中的溶解度。
第三,利用对称悬滴法,在温度范围250～290℃,CO2压力范围0-14MPa内,测定了改性PET熔体在CO2环境下的表面张力。结果表明,改性PET熔体在CO2环境中的表面张力随着温度和CO2压力的增加呈现减小的趋势,且随着CO2压力的增加,改性PET熔体的表面张力对温度的依赖性减弱。由于长链支化结构的存在限制了其熔体的流动性,改性PET熔体较常规PET熔体具有较大的表面张力。基于实验数据,建立了改性PET熔体在CO2环境中表面张力的经验方程。
第四,对改性PET的CO2发泡成核过程进行了模拟分析。分别引入了成核能垒的校正因子F和Zeldovich因子的校正因子f0对经典成核公式进行修正：只引入F时发现,相同的发泡温度下F值随着饱和压力的增加呈现出上升的趋势；相同的饱和压力下F值随着温度的增加而线性增加。同时引入F以及f0时,拟合发泡实验结果显示,不同发泡温度下f0均具有10-21的量级,且数值较为接近；F值具有10-5～104的量级；固定f0为10-21后,F值同样随着饱和压力的增加而上升、随温度的增加而线性增加。
最后,研究了超临界CO2辅助的改性PET熔融缩聚增粘和发泡一体化过程。考察了CO2流量、CO2压力和处理时间对改性PET的熔体强度及其发泡材料泡孔形貌的影响,结果表明,相比N2,CO2能够有效地强化改性PET的熔融缩聚增粘过程,改性PET的特性粘度随着CO2流量、CO2压力和处理时间的增加而增加。在相同处理时间下,PET发泡样品的密度随着CO2流量的增加而减小；随着处理时间的增加,PET的热降解加剧,因而得到的PET发泡样品的密度呈现增加的趋势；而CO2压力对发泡样品的密度的影响是非单调的。对本文的实验体系来说,温度280℃,饱和压力8～14MPa,CO2流量3～5L/min,处理时间30～50min时,一体化过程制备的PET发泡样品的泡孔直径在32～62μm之间,泡孔密度在1×107～4×107cells/cm3之间。同时,对比进行了常规的“一步法”发泡过程、分步实施的超临界CO2的辅助改性PET熔融缩聚增粘和发泡过程,发现一体化过程提高了聚合物熔体强度、避免了PET再熔融降解,在相同或较短的处理时间内能够得到更优的泡孔结构。
Poly(ethylene terephthalate)(PET) is an important polymer for significant practical use in the field of engineering plastic. Besides excellent properties, light-weight is a new demand for engineering plastic. Thus, PET foams with both low density and high mechanical performance has been drawing great interests. Traditional PET is a sort of linear polymer with relative low molecular weight and narrow molecular weight distribution, and is characterized by its insufficient melt strength which is not compatible with foaming process. During bubble growth stage, bubble walls tend to fracture and bubbles tend to collapse. PET matrix, therefore, should be modified to improve its melt strength. Besides, PET has high affinity with moisture, and quite easy to degrade when exposed to heat and oxygen, making molecular weight and melt strength decrease sharply and thus, difficult to be foamed. In this study, modified PET with excellent foaming properties has been successfully prepared. Based on the determination of solubility of CO2in the modified PET melt and surface tension of the modified PET melt in CO2, cell nucleation in CO2foaming process has been simulated. A novel integrated process of supercritical CO2assisted melt polycondensation modification and foaming of PET is proposed, and the feasibility and advantage of this integrated process have been confirmed. The detailed works are as following:
In-situ preparation of foamable high melt strength modified PET. Acid M and alcohol N are selected as modifying monomers for the preparation of modified PET with long chain branching structure. The results show that the melt strength of modified PETs has been improved effectively. When the amount of alcohol N is0.3wt%and acid M is0.8wt%, the intrinsic viscosity (Ⅳ) of the modified PET can be increased to0.860dL/g and0.865dL/g, respectively as well as their melt flow index (MFI) can be decreased to15.1g/10min and15.0g/10min. Differential scanning calorimeter (DSC) tests reveal that the crystallization temperature T., enthalpy of crystallization△Hc, the melting temperature Tm and enthalpy of melting△Hm of modified PETs are all somewhat decreased due to the presence of the branched structures. Rheological test demonstrates that the complex viscosity, the storage modulus and loss modulus all increase compared with unmodified PET. A rapid depressurization batch molten PET foaming test using CO2as blowing agent is carried out and it is found that both modified PETs can be foamed in the temperature range of265-280℃. PET foams with average cell diameter of35～57μm, cell density of106-107cells/cm3can be successfully prepared, whereas traditional PET cannot be foamed under the same condition. In addition, the average cell diameter of alcohol N modified PET foam is smaller than that of acid M modified PET.
Solubility of CO2in PET melt. CO2solubility in PET is studied using magnetic suspension balance (MSB) combined with high-temperature and high-pressure view cell. The former is used to obtain apparent solubility and the latter to determine the swelling volume through direct observation in the presence of CO2, which is necessary to correct the gas buoyancy acting on PET melts in the MSB measurement. The effects of temperature and CO2pressure on the swelling ratio and CO2solubility in traditional and modified PET melt are investigated, respectively. The results show that swelling ratio of PET and CO2solubility both decrease with increasing temperature and increase with CO2pressure, however, the swelling ratio increases slowly and approaches a plateau region under higher pressure. Compared with traditional linear PET, modified PET displays both lower swelling ratio and solubility. Solubility value of CO2in PET melt has an order of magnitude of10-2(g CO2/g PET melt) at4～6MPa CO2pressure in the temperature range of250～280℃. and confirms with Henry's law within the pressure range of1～6MPa. S-L EOS is adopted to fit the swelling ratio in the CO2pressure range of1～14MPa, and CO2solubility at higher pressure is also predicted.
Surface tension of PET melt in CO2. Using the Axisymmetric Drop Shape Analysis-Profile method, surface tension of PET melt in CO2at temperatures of250to290℃and CO2pressure of0to14MPa is measured using high-temperature and high-pressure view cell. It is found that surface tensions of modified PET melt decrease with increase of either temperature or CO2pressure, and with CO2pressure increasing, the dependence of surface tension on temperature weakens. Modified PET shows a higher surface tension than traditional linear PET due to the more conformation restriction exhibited by its branched structure. Based on experiment, an empirical equation is proposed to predict the surface tension of modified PET in CO2.
Simulation and analysis of cell nucleation in modified PET foaming process. Classical nucleation model is adopted with the introduction of the correction factors both for the free energy barrier (F) and the Zeldovich factor (f0). With only F factor introduced, it is found that F value increases with saturation pressure once the foaming temperature is fixed, and when saturation pressure is fixed. F value increases linearly with temperature. With both F and f0introduced, it is observed that under the three foaming temperatures, fo values all have an order of magnitude of10-21and F values have an order of magnitude of10-5～10-4. When fo is fixed at10-21. it is found that F value also increases with saturation pressure and linearly increases with temperature.
Integrated process of supercritical CO2assisted melt polycondensation modification and foaming of PET. The influences of CO2flow rate, CO2pressure and treating time on melt strength of the modified PETs and cell morphologies of foamed PETs are investigated respectively. It is proved that compared with N2sweeping, CO2sweeping can effectively enhance the melt polycondensation of preliminary modified PET. The viscosity of the modified PET increases with CO2flow rate, CO2pressure and CO2treating time. It is found that foam density will decrease with increasing CO2flow rate for the same treating time while it will increase with increasing treating time due to thermal degradation. The influence of CO2pressure on the foam density is non-monotonic. For our experimental system, PET foams with an average diameter of32～62μm and cell density of1×107～4×107cells/cm3can be obtained under the saturation pressure8-14MPa, CO2flow rate3-5L/min, treating time30～50min and temperature280℃. Meanwhile,"one step" foaming method and separated process of supercritical CO2assisted melt polycondensation modification and foaming are carried out for comparison, and the results demonstrate that better cell morphologies can be obtained from the integrated process within the same or shorter time.
首先,采用原位聚合改性的方法制备了具有较高熔体强度改性PET。选取醇N和酸M两种多官能团化合物为第三单体原位聚合分别制备了具有长链支化结构的醇改性PET和酸改性PET,有效地提高了聚酯的熔体强度,当醇N的添加含量0.3wt%、酸M的添加含量0.8wt%时,改性PET的特性粘度Ⅳ从常规线性PET的0.659dL/g分别提高到0.860dL/g和0.865dL/g,熔融流动指数MFI从29.3g/10min分别减小到15.1g/lOmin和15.0g/10min。两种改性PET的结晶温度Tc,结晶焓△Hc,熔点Tm,,熔融焓△Hm均有所降低,复数粘度η*、储能模量G’和耗能模量G”较未改性PET均有显著提高,且呈现出剪切变稀的流动特性。以超临界CO2为发泡剂的间歇熔融发泡实验表明,两种改性PET在发泡温度265～280℃范围内可成功制备泡孔直径35～57μm、泡孔密度106～107cells/cm3的发泡样品,而同样条件下线性PET无法发泡,另外醇改性PET的发泡样品泡孔尺寸较酸改性PET的小、泡孔密度高。
其次,通过高温高压磁悬浮天平(MSB)测定表观溶解度、高温高压视窗釜进行溶胀度校正的方法研究了CO2在PET熔体中的溶解度。考察了温度、CO2压力对改性前后PET在CO2环境中的溶胀度和CO2溶解度的影响,结果表明,PET在CO2环境中的溶胀度和CO2溶解度均随温度的增加而减小,随压力增加而增加,但高压下溶胀度的增加趋势减缓并趋于某定值。与常规线性PET相比,改性PET具有较小的溶胀度和溶解度。在250～280℃,1～6MPa下CO2在PET熔体中的溶解行为符合亨利定律,4-6MPa下溶解度具有10-2(gCO2/g PET melt)的量级。利用S-L方程对PET熔体在1～14MPa下CO2中,的溶胀度进行了拟合,进而预测了较高压力下的CO2在PET熔体中的溶解度。
第三,利用对称悬滴法,在温度范围250～290℃,CO2压力范围0-14MPa内,测定了改性PET熔体在CO2环境下的表面张力。结果表明,改性PET熔体在CO2环境中的表面张力随着温度和CO2压力的增加呈现减小的趋势,且随着CO2压力的增加,改性PET熔体的表面张力对温度的依赖性减弱。由于长链支化结构的存在限制了其熔体的流动性,改性PET熔体较常规PET熔体具有较大的表面张力。基于实验数据,建立了改性PET熔体在CO2环境中表面张力的经验方程。
第四,对改性PET的CO2发泡成核过程进行了模拟分析。分别引入了成核能垒的校正因子F和Zeldovich因子的校正因子f0对经典成核公式进行修正：只引入F时发现,相同的发泡温度下F值随着饱和压力的增加呈现出上升的趋势；相同的饱和压力下F值随着温度的增加而线性增加。同时引入F以及f0时,拟合发泡实验结果显示,不同发泡温度下f0均具有10-21的量级,且数值较为接近；F值具有10-5～104的量级；固定f0为10-21后,F值同样随着饱和压力的增加而上升、随温度的增加而线性增加。
最后,研究了超临界CO2辅助的改性PET熔融缩聚增粘和发泡一体化过程。考察了CO2流量、CO2压力和处理时间对改性PET的熔体强度及其发泡材料泡孔形貌的影响,结果表明,相比N2,CO2能够有效地强化改性PET的熔融缩聚增粘过程,改性PET的特性粘度随着CO2流量、CO2压力和处理时间的增加而增加。在相同处理时间下,PET发泡样品的密度随着CO2流量的增加而减小；随着处理时间的增加,PET的热降解加剧,因而得到的PET发泡样品的密度呈现增加的趋势；而CO2压力对发泡样品的密度的影响是非单调的。对本文的实验体系来说,温度280℃,饱和压力8～14MPa,CO2流量3～5L/min,处理时间30～50min时,一体化过程制备的PET发泡样品的泡孔直径在32～62μm之间,泡孔密度在1×107～4×107cells/cm3之间。同时,对比进行了常规的“一步法”发泡过程、分步实施的超临界CO2的辅助改性PET熔融缩聚增粘和发泡过程,发现一体化过程提高了聚合物熔体强度、避免了PET再熔融降解,在相同或较短的处理时间内能够得到更优的泡孔结构。
Poly(ethylene terephthalate)(PET) is an important polymer for significant practical use in the field of engineering plastic. Besides excellent properties, light-weight is a new demand for engineering plastic. Thus, PET foams with both low density and high mechanical performance has been drawing great interests. Traditional PET is a sort of linear polymer with relative low molecular weight and narrow molecular weight distribution, and is characterized by its insufficient melt strength which is not compatible with foaming process. During bubble growth stage, bubble walls tend to fracture and bubbles tend to collapse. PET matrix, therefore, should be modified to improve its melt strength. Besides, PET has high affinity with moisture, and quite easy to degrade when exposed to heat and oxygen, making molecular weight and melt strength decrease sharply and thus, difficult to be foamed. In this study, modified PET with excellent foaming properties has been successfully prepared. Based on the determination of solubility of CO2in the modified PET melt and surface tension of the modified PET melt in CO2, cell nucleation in CO2foaming process has been simulated. A novel integrated process of supercritical CO2assisted melt polycondensation modification and foaming of PET is proposed, and the feasibility and advantage of this integrated process have been confirmed. The detailed works are as following:
In-situ preparation of foamable high melt strength modified PET. Acid M and alcohol N are selected as modifying monomers for the preparation of modified PET with long chain branching structure. The results show that the melt strength of modified PETs has been improved effectively. When the amount of alcohol N is0.3wt%and acid M is0.8wt%, the intrinsic viscosity (Ⅳ) of the modified PET can be increased to0.860dL/g and0.865dL/g, respectively as well as their melt flow index (MFI) can be decreased to15.1g/10min and15.0g/10min. Differential scanning calorimeter (DSC) tests reveal that the crystallization temperature T., enthalpy of crystallization△Hc, the melting temperature Tm and enthalpy of melting△Hm of modified PETs are all somewhat decreased due to the presence of the branched structures. Rheological test demonstrates that the complex viscosity, the storage modulus and loss modulus all increase compared with unmodified PET. A rapid depressurization batch molten PET foaming test using CO2as blowing agent is carried out and it is found that both modified PETs can be foamed in the temperature range of265-280℃. PET foams with average cell diameter of35～57μm, cell density of106-107cells/cm3can be successfully prepared, whereas traditional PET cannot be foamed under the same condition. In addition, the average cell diameter of alcohol N modified PET foam is smaller than that of acid M modified PET.
Solubility of CO2in PET melt. CO2solubility in PET is studied using magnetic suspension balance (MSB) combined with high-temperature and high-pressure view cell. The former is used to obtain apparent solubility and the latter to determine the swelling volume through direct observation in the presence of CO2, which is necessary to correct the gas buoyancy acting on PET melts in the MSB measurement. The effects of temperature and CO2pressure on the swelling ratio and CO2solubility in traditional and modified PET melt are investigated, respectively. The results show that swelling ratio of PET and CO2solubility both decrease with increasing temperature and increase with CO2pressure, however, the swelling ratio increases slowly and approaches a plateau region under higher pressure. Compared with traditional linear PET, modified PET displays both lower swelling ratio and solubility. Solubility value of CO2in PET melt has an order of magnitude of10-2(g CO2/g PET melt) at4～6MPa CO2pressure in the temperature range of250～280℃. and confirms with Henry's law within the pressure range of1～6MPa. S-L EOS is adopted to fit the swelling ratio in the CO2pressure range of1～14MPa, and CO2solubility at higher pressure is also predicted.
Surface tension of PET melt in CO2. Using the Axisymmetric Drop Shape Analysis-Profile method, surface tension of PET melt in CO2at temperatures of250to290℃and CO2pressure of0to14MPa is measured using high-temperature and high-pressure view cell. It is found that surface tensions of modified PET melt decrease with increase of either temperature or CO2pressure, and with CO2pressure increasing, the dependence of surface tension on temperature weakens. Modified PET shows a higher surface tension than traditional linear PET due to the more conformation restriction exhibited by its branched structure. Based on experiment, an empirical equation is proposed to predict the surface tension of modified PET in CO2.
Simulation and analysis of cell nucleation in modified PET foaming process. Classical nucleation model is adopted with the introduction of the correction factors both for the free energy barrier (F) and the Zeldovich factor (f0). With only F factor introduced, it is found that F value increases with saturation pressure once the foaming temperature is fixed, and when saturation pressure is fixed. F value increases linearly with temperature. With both F and f0introduced, it is observed that under the three foaming temperatures, fo values all have an order of magnitude of10-21and F values have an order of magnitude of10-5～10-4. When fo is fixed at10-21. it is found that F value also increases with saturation pressure and linearly increases with temperature.
Integrated process of supercritical CO2assisted melt polycondensation modification and foaming of PET. The influences of CO2flow rate, CO2pressure and treating time on melt strength of the modified PETs and cell morphologies of foamed PETs are investigated respectively. It is proved that compared with N2sweeping, CO2sweeping can effectively enhance the melt polycondensation of preliminary modified PET. The viscosity of the modified PET increases with CO2flow rate, CO2pressure and CO2treating time. It is found that foam density will decrease with increasing CO2flow rate for the same treating time while it will increase with increasing treating time due to thermal degradation. The influence of CO2pressure on the foam density is non-monotonic. For our experimental system, PET foams with an average diameter of32～62μm and cell density of1×107～4×107cells/cm3can be obtained under the saturation pressure8-14MPa, CO2flow rate3-5L/min, treating time30～50min and temperature280℃. Meanwhile,"one step" foaming method and separated process of supercritical CO2assisted melt polycondensation modification and foaming are carried out for comparison, and the results demonstrate that better cell morphologies can be obtained from the integrated process within the same or shorter time.
引文
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