新型聚碳酸亚丙酯/蒙脱土纳米复合材料的制备、性能及降解行为研究
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摘要
由CO2和环氧丙烷发生开环共聚反应生成的可降解塑料聚碳酸亚丙酯(PPC)的推广和使用是治理“白色污染”的有效途径,但低热稳定性和较差的力学性能使其应用范围受限。本文采用聚合物/层状硅酸盐纳米复合材料的研究思路,用有机阳离子修饰的蒙脱土改性PPC,达到提高其热稳定性和力学性能等的目的。
为更好地说明有机修饰剂、蒙脱土(MMT)和PPC基质之间的相互作用对纳米复合材料结构、性能的影响,本文选用三种不同结构类型和体积大小的有机阳离子：咪唑季铵盐(HHMIB)、盐酸氨基酸盐(AUA)和低聚聚苯乙烯季铵盐(COPS),利用MMT的阳离子交换性分别对其进行修饰,通过测试修饰前后C含量的变化或利用热重分析(TG)计算出实际插层的阳离子量即交换容量。结果表明HHMIB的插层能力最弱,达到的交换容量仅为64.6mmol/100g; AUA的交换容量达到92.3mmol/100g;由于在插层之前先对MMT作了端面的硅烷化修饰,增大了MMT的亲油性,使COPS的交换容量达到97.6mmol/100g。X射线衍射(XRD)结果表明HHMIB插层后MMT的层间距由1.52nm增至2.60nm；由于AUA的体积最小,其插层后MMT的层间距只增至1.62nm；由于COPS的体积最大,其插层后MMT的层间距增至3.53nm以上。
用上述有机蒙脱土分别和PPC熔融共混制备出三种不同蒙脱土质量分数的PPC/MMT复合材料,对复合材料的结构、热稳定性、力学性能和耐介质性进行了研究。XRD和透射电镜(TEM)显示聚碳酸亚丙酯／咪唑盐化-蒙脱土复合材料(PPC/H-MMT)和聚碳酸亚丙酯/盐酸氨基酸盐化-蒙脱土复合材料(PPC/A-MMT)是蒙脱土层间距分别为3nm和2nm的插层型纳米复合材料；聚碳酸亚丙酯/硅烷化-低聚聚苯乙烯化-蒙脱土复合材料(PPC/A-C-MMT)是剥离型纳米复合材料。TG分析表明相比PPC复合材料的热稳定性都提高：PPC/H-MMT、PPC/A-MMT和PPC/A-C-MMT的onset分别最大提高了64℃、41℃和82℃,T10%分别最大提高了64℃、46℃和76℃,T50%分别最大提高了47℃、27℃和47℃。剥离型结构产生的“纳米效应”使PPC/A-C-MMT热稳定性最高,相比PPC显著提升。静态拉伸力学性能测试显示复合材料的力学性能发生明显变化：相比PPC, PPC/H-MMT、PPC/A-MMT、PPC/A-C-MMT的拉伸强度分别最大增加了34.6%、78.4%和549%；弹性模量分别最大增加了69.7%、1425%和4382%；断裂伸长率分别最大降低了34%、52.3%和99.3%,但PPC/H-MMT和PPC/A-MMT的断裂伸长率绝对值很大,分别为900%和650%,材料依然具有优良的韧性,PPC/A-C-MMT的断裂伸长率为10.18%,韧性减弱,脆性增大。PPC/A-C-MMT的强度和硬度发生突跃性的改变同样是归功于剥离型结构产生的“纳米效应”。动态力学性能测试(DMA)显示复合材料的储能模量都高于PPC,刚性都得到增强；随着温度的升高,发生状态转变的温度都比PPC滞后：PPC/H-MMT、PPC/A-MMT和PPC/A-C-MMT由玻璃态向玻璃态-高弹态混合态转变的温度分别最大提高了约5℃、16℃和24℃,玻璃化转变温度(Tg)分别最大提高了2.4℃、10℃和18.5℃。将材料浸泡在水或机油中一定时问后,通过测试质量的变化表征其耐介质性。结果显示PPC的吸水率是4.4%,PPC/H-MMT的最大吸水率是13%,耐水性减弱；PPC/A-MMT和PPC/A-C-MMT的最大吸水率分别为3%和2%左右,耐水性增强。复合材料的吸油率很低,都在0.9%之内,具有优良的耐油性。
复合材料材料分别在自然条件下光降解和土埋恒温恒湿条件下生物降解180天后,用凝胶渗透色谱法测试降解前后PPC的分子量表征其降解性。纯PPC的光降解率为83.9%;PPC/H-MMT、PPC/A-MMT和PPC/A-C-MMT的最大光降解率分别为82.6%、82.0%和65.4%。PPC的生物降解率为74.9%；PPC/H-MMT、PPC/A-MMT和PPC/A-C-MMT的最大生物降解率分别为78.1%、64.7%和28.4%。除了PPC/H-MMT的生物降解性比PPC增强,其它复合材料的光降解性和生物降解性相比PPC都下降。PPC/A-C-MMT的生物降解性偏低,但最大光降解率可达到65.4%,依然是光降解性较好的复合材料；其它两种复合材料具有良好的降解性。
生物降解后PPC/MMT纳米复合材料对土壤质量的影响未见报道。本文用稀释平板计数法测定生物降解后填埋复合材料的土壤微生物菌落总数,氯仿熏蒸浸提法测定土壤微生物生物量碳。测试结果表明：复合材料的生物降解性越高,土壤中的微生物菌落总数和微生物生物量碳越高,土壤的肥力和生物活性越高；填埋复合材料的土壤的生物活性都比未填埋材料的土壤的生物活性高,都可提高土壤质量,使土壤生态系统良性循环,因此这三种复合材料的使用不会带来环境污染,是生态环境材料。又由于复合材料都具有较高的降解性,且具有比PPC高的热稳定性和力学性能,预计这三种复合材料特别是PPC/A-MMT和PPC/A-C-MMT的大力推广和使用会有效缓解由传统塑料使用带来的“白色污染”问题。
Degradable poly (propylene carbonate)(PPC) is derived from carbon dioxide and propylene oxide through ring-opening copolymerization. Its wide use would be an effective method to prevent "white pollution". However, low thermal stability and mechanical property have greatly limited its application. In this thesis, we try to build polymer/layered silicate nanocomposite, and organic cation was utilized to modify montmorillonite (MMT) to improve thermal stability and mechanical property of PPC.
In order to illustrate interactions among organic modifier, MMT and PPC matrix which have an effect on performance of nanocomposite, Three organic cations with various structure and volume, i.e. imidazole quaternary ammonium salt (HHMIB), hydrochloric-amino acid salt (AUA), polystyrene oligomer quaternary ammonium salt (COPS) were adopted to modify MMT respectively. MMT modification was based on cation-exchange and actual amount of intercalated cation was calculated through change of C content or thermal gravimetric analysis (TG). It were indicated that intercalating ability of HHMIB was weakest, actual cation exchange capacity was only64.6mmol/100g; AUA was92.3mmol/100g; COPS was 97.6mmol/100g due to improved lipophilicity of MMT caused by silane-modification before intercalation. X-ray diffraction (XRD) showed that interlayer spacing of MMT was enlarged from1.52nm to2.60nm,1.62nm and over3.53nm after being intercalated by HHMIB, AUA and COPS respectively. The interlayer spacing of MMT modified by AUA is smallest because of its smallest volume and that of MMT modified by COPS is largest because of its largest volume.
Three kinds of PPC/MMT nanocomposites with different mass fractions of MMT were prepared by melt blending using organic montmorillonites mentioned above. Structure, thermal stability, mechanical property and medium resistance of the composites were studied systematically. It was illustrated that poly (propylene carbonate)/imidazole salt modified-montmorillonite (PPC/H-MMT) and poly (propylene carbonate)/hydrochloric-amino acid salt modified-montmorillonite (PPC/A-MMT) were all intercalated nanocomposites with enlarged interlayer spacing of3nm and2nm respectively through XRD and transmission electron microscope (TEM) characterizations. It was similarly indicated that poly (propylene carbonate)/silane and polystyrene-modified-montmorillonite (PPC/A-C-MMT) was exfoliated nanocomposite. TG results demonstrated that thermal stabilities of the three composites were all improved. Maximum increments of ronset of PPC/H-MMT, PPC/A-MMT and PPC/A-C-MMT were64℃,41℃and82℃; maximum increments of T10%were64℃,46℃and76℃; maximum increments of T50%were47℃,27℃and47℃, respectively. Nano-effect derived from exfoliated structure made thermal stability of PPC/A-C-MMT to be significantly improved compared to PPC and to be highest of the three composites. Static tensile test demonstrated that mechanical properties of the composites changed. Maximum increments of tensile strength of PPC/H-MMT, PPC/A-MMT and PPC/A-C-MMT were34.6%,78.4%and549%; maximum increments of elastic modulus were69.7%,1425%和4382%. In addition the maximum decrements of elongation at break were34%,52.3%and99.3%, respectively. However, PPC/H-MMT and PPC/A-MMT still kept excellent toughness because of their large absolute value of900%and650%. Elongation at break of PPC/A-C-MMT was10.18%, its toughness decreased and brittleness increased. Significant reinforcement in strength and hardness of PPC/A-C-MMT was also owed to nano-effect caused by exfoliated structure. Dynamic mechanical property analyses (DMA) showed that rigidity of the three composites were all enhanced for their strengthened storage modulus. It was also showed by DMA that state transition of the composites lagged than pure PPC with increasing temperature:transition temperatures from glass state to glass-high elastic mixed state of PPC/H-MMT, PPC/A-MMT and PPC/A-C-MMT increased about5℃,16℃and24℃, glass temperatures increased2.4℃,10℃and18.5℃respectively. Medium resistances of the composites were characterized through detecting changes in quality after being soaked in water or oil for a certain time. Water absorption of PPC was4.4%, maximum water absorption of PPC/H-MMT, PPC/A-MMT, and PPC/A-C-MMT were about13%,3%and2%respectively. Accordingly, water resistance of PPC/H-MMT was wakened and that of PPC/A-MMT, PPC/A-C-MMT were enhanced. Oil absorption of all composites kept within0.9%and they had good oil resistance.
Molecular weight of PPC was detected by gel permeation chromatography. Degradability was characterized through changes in molecular weight of PPC when the composites were placed in natural environment or buried in soil for180days. It was founded that photodegradation ratio and biodegradation ratio of pure PPC were83.9%and74.9%, maximum photodegradation ratio of PC/H-MMT, PPC/A-MMT, PPC/A-C-MMT were82.6%,82.0%,65.4%, maximum biodegradation ratio of the three composites were78.1%,64.7%,28.4%, respectively. The degradability of composites was all decreased in addition to improved biodegradability of PC/H-MMT. Results indicated that PPC/H-MMT, PPC/A-MMT have better degradability, and although biodegradability of PPC/A-C-MMT is low, its photodegradation ratio can reached65.4%which make it still a good photodegradable material.
Influence of PPC/MMT nanocomposite on soil quality after biodegradation was not reported. Total numbers of microbial colonies in soil were determined by adopting dilution method of plate counting, microbial biomass carbon was detected through chloroform fumigation-extraction method in this work. Results indicated that the greater degradability of the composite was, the more number of microbial colonies and microbial biomass carbon in soil were, and the higher bioactivity and soil fertility were. Fertility of soil filled with composites was better than virgin soil, the composites can amend soil quality and make soil ecosystem in beneficial cycle. Therefore, the three composites are eco-materials and using them will not cause environmental pollution. Furthermore, because of good degradability and better thermal stability and mechanical property than PPC, we can predict that their wide use especial PPC/A-MMT and PPC/A-C-MMT will effectively mitigate "white pollution" caused by use of conventional plastics.
为更好地说明有机修饰剂、蒙脱土(MMT)和PPC基质之间的相互作用对纳米复合材料结构、性能的影响,本文选用三种不同结构类型和体积大小的有机阳离子：咪唑季铵盐(HHMIB)、盐酸氨基酸盐(AUA)和低聚聚苯乙烯季铵盐(COPS),利用MMT的阳离子交换性分别对其进行修饰,通过测试修饰前后C含量的变化或利用热重分析(TG)计算出实际插层的阳离子量即交换容量。结果表明HHMIB的插层能力最弱,达到的交换容量仅为64.6mmol/100g; AUA的交换容量达到92.3mmol/100g;由于在插层之前先对MMT作了端面的硅烷化修饰,增大了MMT的亲油性,使COPS的交换容量达到97.6mmol/100g。X射线衍射(XRD)结果表明HHMIB插层后MMT的层间距由1.52nm增至2.60nm；由于AUA的体积最小,其插层后MMT的层间距只增至1.62nm；由于COPS的体积最大,其插层后MMT的层间距增至3.53nm以上。
用上述有机蒙脱土分别和PPC熔融共混制备出三种不同蒙脱土质量分数的PPC/MMT复合材料,对复合材料的结构、热稳定性、力学性能和耐介质性进行了研究。XRD和透射电镜(TEM)显示聚碳酸亚丙酯／咪唑盐化-蒙脱土复合材料(PPC/H-MMT)和聚碳酸亚丙酯/盐酸氨基酸盐化-蒙脱土复合材料(PPC/A-MMT)是蒙脱土层间距分别为3nm和2nm的插层型纳米复合材料；聚碳酸亚丙酯/硅烷化-低聚聚苯乙烯化-蒙脱土复合材料(PPC/A-C-MMT)是剥离型纳米复合材料。TG分析表明相比PPC复合材料的热稳定性都提高：PPC/H-MMT、PPC/A-MMT和PPC/A-C-MMT的onset分别最大提高了64℃、41℃和82℃,T10%分别最大提高了64℃、46℃和76℃,T50%分别最大提高了47℃、27℃和47℃。剥离型结构产生的“纳米效应”使PPC/A-C-MMT热稳定性最高,相比PPC显著提升。静态拉伸力学性能测试显示复合材料的力学性能发生明显变化：相比PPC, PPC/H-MMT、PPC/A-MMT、PPC/A-C-MMT的拉伸强度分别最大增加了34.6%、78.4%和549%；弹性模量分别最大增加了69.7%、1425%和4382%；断裂伸长率分别最大降低了34%、52.3%和99.3%,但PPC/H-MMT和PPC/A-MMT的断裂伸长率绝对值很大,分别为900%和650%,材料依然具有优良的韧性,PPC/A-C-MMT的断裂伸长率为10.18%,韧性减弱,脆性增大。PPC/A-C-MMT的强度和硬度发生突跃性的改变同样是归功于剥离型结构产生的“纳米效应”。动态力学性能测试(DMA)显示复合材料的储能模量都高于PPC,刚性都得到增强；随着温度的升高,发生状态转变的温度都比PPC滞后：PPC/H-MMT、PPC/A-MMT和PPC/A-C-MMT由玻璃态向玻璃态-高弹态混合态转变的温度分别最大提高了约5℃、16℃和24℃,玻璃化转变温度(Tg)分别最大提高了2.4℃、10℃和18.5℃。将材料浸泡在水或机油中一定时问后,通过测试质量的变化表征其耐介质性。结果显示PPC的吸水率是4.4%,PPC/H-MMT的最大吸水率是13%,耐水性减弱；PPC/A-MMT和PPC/A-C-MMT的最大吸水率分别为3%和2%左右,耐水性增强。复合材料的吸油率很低,都在0.9%之内,具有优良的耐油性。
复合材料材料分别在自然条件下光降解和土埋恒温恒湿条件下生物降解180天后,用凝胶渗透色谱法测试降解前后PPC的分子量表征其降解性。纯PPC的光降解率为83.9%;PPC/H-MMT、PPC/A-MMT和PPC/A-C-MMT的最大光降解率分别为82.6%、82.0%和65.4%。PPC的生物降解率为74.9%；PPC/H-MMT、PPC/A-MMT和PPC/A-C-MMT的最大生物降解率分别为78.1%、64.7%和28.4%。除了PPC/H-MMT的生物降解性比PPC增强,其它复合材料的光降解性和生物降解性相比PPC都下降。PPC/A-C-MMT的生物降解性偏低,但最大光降解率可达到65.4%,依然是光降解性较好的复合材料；其它两种复合材料具有良好的降解性。
生物降解后PPC/MMT纳米复合材料对土壤质量的影响未见报道。本文用稀释平板计数法测定生物降解后填埋复合材料的土壤微生物菌落总数,氯仿熏蒸浸提法测定土壤微生物生物量碳。测试结果表明：复合材料的生物降解性越高,土壤中的微生物菌落总数和微生物生物量碳越高,土壤的肥力和生物活性越高；填埋复合材料的土壤的生物活性都比未填埋材料的土壤的生物活性高,都可提高土壤质量,使土壤生态系统良性循环,因此这三种复合材料的使用不会带来环境污染,是生态环境材料。又由于复合材料都具有较高的降解性,且具有比PPC高的热稳定性和力学性能,预计这三种复合材料特别是PPC/A-MMT和PPC/A-C-MMT的大力推广和使用会有效缓解由传统塑料使用带来的“白色污染”问题。
Degradable poly (propylene carbonate)(PPC) is derived from carbon dioxide and propylene oxide through ring-opening copolymerization. Its wide use would be an effective method to prevent "white pollution". However, low thermal stability and mechanical property have greatly limited its application. In this thesis, we try to build polymer/layered silicate nanocomposite, and organic cation was utilized to modify montmorillonite (MMT) to improve thermal stability and mechanical property of PPC.
In order to illustrate interactions among organic modifier, MMT and PPC matrix which have an effect on performance of nanocomposite, Three organic cations with various structure and volume, i.e. imidazole quaternary ammonium salt (HHMIB), hydrochloric-amino acid salt (AUA), polystyrene oligomer quaternary ammonium salt (COPS) were adopted to modify MMT respectively. MMT modification was based on cation-exchange and actual amount of intercalated cation was calculated through change of C content or thermal gravimetric analysis (TG). It were indicated that intercalating ability of HHMIB was weakest, actual cation exchange capacity was only64.6mmol/100g; AUA was92.3mmol/100g; COPS was 97.6mmol/100g due to improved lipophilicity of MMT caused by silane-modification before intercalation. X-ray diffraction (XRD) showed that interlayer spacing of MMT was enlarged from1.52nm to2.60nm,1.62nm and over3.53nm after being intercalated by HHMIB, AUA and COPS respectively. The interlayer spacing of MMT modified by AUA is smallest because of its smallest volume and that of MMT modified by COPS is largest because of its largest volume.
Three kinds of PPC/MMT nanocomposites with different mass fractions of MMT were prepared by melt blending using organic montmorillonites mentioned above. Structure, thermal stability, mechanical property and medium resistance of the composites were studied systematically. It was illustrated that poly (propylene carbonate)/imidazole salt modified-montmorillonite (PPC/H-MMT) and poly (propylene carbonate)/hydrochloric-amino acid salt modified-montmorillonite (PPC/A-MMT) were all intercalated nanocomposites with enlarged interlayer spacing of3nm and2nm respectively through XRD and transmission electron microscope (TEM) characterizations. It was similarly indicated that poly (propylene carbonate)/silane and polystyrene-modified-montmorillonite (PPC/A-C-MMT) was exfoliated nanocomposite. TG results demonstrated that thermal stabilities of the three composites were all improved. Maximum increments of ronset of PPC/H-MMT, PPC/A-MMT and PPC/A-C-MMT were64℃,41℃and82℃; maximum increments of T10%were64℃,46℃and76℃; maximum increments of T50%were47℃,27℃and47℃, respectively. Nano-effect derived from exfoliated structure made thermal stability of PPC/A-C-MMT to be significantly improved compared to PPC and to be highest of the three composites. Static tensile test demonstrated that mechanical properties of the composites changed. Maximum increments of tensile strength of PPC/H-MMT, PPC/A-MMT and PPC/A-C-MMT were34.6%,78.4%and549%; maximum increments of elastic modulus were69.7%,1425%和4382%. In addition the maximum decrements of elongation at break were34%,52.3%and99.3%, respectively. However, PPC/H-MMT and PPC/A-MMT still kept excellent toughness because of their large absolute value of900%and650%. Elongation at break of PPC/A-C-MMT was10.18%, its toughness decreased and brittleness increased. Significant reinforcement in strength and hardness of PPC/A-C-MMT was also owed to nano-effect caused by exfoliated structure. Dynamic mechanical property analyses (DMA) showed that rigidity of the three composites were all enhanced for their strengthened storage modulus. It was also showed by DMA that state transition of the composites lagged than pure PPC with increasing temperature:transition temperatures from glass state to glass-high elastic mixed state of PPC/H-MMT, PPC/A-MMT and PPC/A-C-MMT increased about5℃,16℃and24℃, glass temperatures increased2.4℃,10℃and18.5℃respectively. Medium resistances of the composites were characterized through detecting changes in quality after being soaked in water or oil for a certain time. Water absorption of PPC was4.4%, maximum water absorption of PPC/H-MMT, PPC/A-MMT, and PPC/A-C-MMT were about13%,3%and2%respectively. Accordingly, water resistance of PPC/H-MMT was wakened and that of PPC/A-MMT, PPC/A-C-MMT were enhanced. Oil absorption of all composites kept within0.9%and they had good oil resistance.
Molecular weight of PPC was detected by gel permeation chromatography. Degradability was characterized through changes in molecular weight of PPC when the composites were placed in natural environment or buried in soil for180days. It was founded that photodegradation ratio and biodegradation ratio of pure PPC were83.9%and74.9%, maximum photodegradation ratio of PC/H-MMT, PPC/A-MMT, PPC/A-C-MMT were82.6%,82.0%,65.4%, maximum biodegradation ratio of the three composites were78.1%,64.7%,28.4%, respectively. The degradability of composites was all decreased in addition to improved biodegradability of PC/H-MMT. Results indicated that PPC/H-MMT, PPC/A-MMT have better degradability, and although biodegradability of PPC/A-C-MMT is low, its photodegradation ratio can reached65.4%which make it still a good photodegradable material.
Influence of PPC/MMT nanocomposite on soil quality after biodegradation was not reported. Total numbers of microbial colonies in soil were determined by adopting dilution method of plate counting, microbial biomass carbon was detected through chloroform fumigation-extraction method in this work. Results indicated that the greater degradability of the composite was, the more number of microbial colonies and microbial biomass carbon in soil were, and the higher bioactivity and soil fertility were. Fertility of soil filled with composites was better than virgin soil, the composites can amend soil quality and make soil ecosystem in beneficial cycle. Therefore, the three composites are eco-materials and using them will not cause environmental pollution. Furthermore, because of good degradability and better thermal stability and mechanical property than PPC, we can predict that their wide use especial PPC/A-MMT and PPC/A-C-MMT will effectively mitigate "white pollution" caused by use of conventional plastics.
引文
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