淀粉基食品包装材料结构与增塑剂迁移的关系研究
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摘要
随着人们食品安全和环境保护等意识的不断提高，开发具有良好安全性和包装性能的环境友好型食品包装材料已成为当前食品包装领域的研究热点，基于可再生资源的生物降解天然高分子包装也越来越受到关注，其中，以来源丰富、价格低廉的淀粉制备的淀粉基食品包装材料被认为是最具应用前景的新型包装之一。然而，增塑剂作为这类新型包装材料设计制造中必需的加工助剂，在包装材料与食品接触后，不可避免地向食品体系中迁移，导致食品包装结构性能改变而逐渐丧失对食品的保护功能。因此，本论文以增塑剂迁移与淀粉基膜材内部微观结构、包装材料/食品模拟体系界面结构以及热加工过程参数等的相互影响为突破口，探讨在不同食品模拟体系及热加工过程中，淀粉基膜材内分子相互作用、结晶结构、微区有序聚集态结构等不同尺度结构的变化规律以及由此带来的对增塑剂迁移的影响，获得了制约增塑剂迁移的淀粉基膜材微观结构因素。
选择高取代度酯化淀粉（DS=2.49）为基材，以三乙酸甘油酯为增塑剂，运用现代分析技术深入研究了增塑剂分布状态及增塑剂与淀粉分子的相互作用以及由此导致的膜材结晶结构、微区有序聚集态结构和热力学性能的变化规律。结果表明，增塑剂添加到淀粉基膜材后，增塑剂和酯化淀粉之间产生了以范德华力为主的相互作用，导致增塑剂与酯化淀粉的醚键增强，而分子本身更活跃。同时，增塑剂扩大了淀粉分子链间距离，增大链段运动性，致使部分链段相互靠近并排列更规整，在原本相对有序的微区中形成分散的微晶结构，对分子链运动产生一定的限制作用。此外，微晶形成过程中，增塑剂分子被挤到临近无定形区域形成了“增塑剂富集区”，通过扩张无定形区给大分子运动提供更多的空间，促进了膜材内不同尺度的松弛过程，参与玻璃化转变的分子链段聚集体的尺度变大。
当淀粉基膜材与食品模拟体系接触后，基于食品模拟体系/增塑剂/膜材基体之间的亲和性差异，食品模拟体系溶剂对膜材产生不同溶胀作用后，导致增塑剂迁移过程不同。在亲和性小的蒸馏水和4%乙酸中，增塑剂前期迁移首先遵循菲克第二扩散定律，随着溶胀作用增强，迁移过程逐渐转变为非菲克扩散，整体迁移过程较符合一级动力学；而在亲和性大的65%乙醇和正己烷体系中，溶胀作用更剧烈，膜材松弛与增塑剂迁移速度相当，增塑剂迁移呈现非菲克扩散特征。
随着增塑剂迁出和食品模拟体系溶剂分子渗透，增塑剂/酯化淀粉间的相互作用力发生改变，增塑剂分子所处化学环境改变，醚键变得不稳定，增塑剂分子稳定性增强。同时，淀粉分子链内/间作用力加强，无定形链段发生收缩聚拢，有序微区整体被挤压，尺寸减小且呈现出多分散性，且微区内部微晶结构收缩。此外，增塑剂迁出弱化不同尺度上的分子链运动性，致密的聚集态结构和有序微区中微晶聚集对膜材中各级松弛过程产生更大限制。也就是说，在食品模拟体系的浸泡过程中，增塑剂分子受到的整体作用力增大，膜材形成更致密聚集态结构，增塑剂分子迁移和溶剂渗透需克服的内摩擦阻力增大，因此，淀粉基膜材增塑剂迁移过程受到抑制。据此，提出了不同食品模拟体系下淀粉基膜材结构变化对增塑剂影响迁移的机制模型。
在热加工过程中，更多水分子进入膜材内加剧溶胀作用，导致膜材聚集态结构发生改变，加速增塑剂迁出。而且，由于膜材有序微区分子链段排列紧密，热加工促进更多水分子渗透扩散到无定形区域，延缓了增塑剂迁移导致的分子链收缩。此外，热加工增强无定形链段运动性，导致有序微区边界的分子链排列成无定形态，有序微区整体缩小，且其内部微晶被轻微破坏，因此，对增塑剂迁出和水分子渗透的阻隔性减弱，更多水分子可进入膜材内溶解增塑剂分子。另外，增塑剂受热后分子运动强烈，因而增塑剂迁移在加热过程中加剧。据此，提出了热加工过程中膜材结构变化对增塑剂迁移影响的机制模型。
本论文提出了增塑剂迁移与膜材微结构、膜材/食品界面结构的关系及其在热加工过程中变化的模型，掌握了在不同食品模拟体系及热加工过程中食品包装材料多尺度结构变化以及由此带来的增塑剂迁移变化的规律，为进一步实现抑制淀粉基生物降解食品包装材料中增塑剂迁移、合理设计及安全使用淀粉基材料提供了基础数据和理论参考。
Alongwith increasing attention focused on food safety and protecting environment, theeco-friendly food packaging material with favorable safety and qualified performance hasbecome the research hotspot in the food packaging industry. Consequently, biodegradablenatural polymer packaging based on renewable resources has attracted more and moreinteresting. Thereinto, as an abundant natural resource with low price, starch has been appliedto produce the starch-based food packaging material, which is considered as one of the mostpromising novel packaging. However, it is hardly possible to avoid plasticizer, which is anessential processing agent involved in the design and manufacture of this novel packagingmaterial, migrating from the matrix into the food system. The plasticizer migration wouldchange the structure and performance of the packaging material, which could lead to thegradual decay of the protection to the food inside. Therefore, in this academic dissertation, itwas proposed as the breakthrough that the relations between plasticizer migration andstructural changes of the starch-based film, including the microstructure and the interfacecontacted with food system, as well as during thermal processing. Moreover, the interaction,crystalline structure and ordered aggregation structure on multiple scales, which changedwhen the material contacted with different food simulants and involved in thermal processingwere discussed, as well as the effect from these structural changes. Finally, themicro-structural factors of starch-based film that restricted the plasticizer migration wereobtained.
Hydrophobic starch ester with high substitute degree (DS=2.49) and triacetin were chosenas the base material and plasticizer. Modern analytical techniques were applied to detect theeffect from plasticizer distribution and plasticizer-starch ester interaction on the crystallinestructure, microstructure and thermodynamics properties. Results showed that new interaction(mainly as Van der Waals force) formed to enhance C-O in plasticizer and starch estermolecules and activate the whole molecules. Meanwhile, the distance betweenmacromolecular chains was enlarged, and the chain mobility was increased to approach toeach other and arranged in more order, which facilitated crystallite formation dispersed withinthe ordered microregion, restricting the chain mobility to some extent. Simultaneously, the plasticizer molecules previously distributed within crystallite were squeezed to formamorphous “plasticizer-rich domain”. The amorphous region was enlarged to provide largerfree volume for macromolecular chains, thus promoting relaxations on different scale. Inaddition, the dimension of chain aggregation involved in glass-rubber transition increased.
When starch-based film contacted with the food stimulants, based on the different affinityamong simulants, plasticizer and film matrix, the diverse swelling behavior occurred,resulting in different migration process. Distilled water and4%acetic acid aqueous with lowaffinity exerted mild swelling effect on the films, and the migration obeyed the Fick’s secondlaw. The non-Fickian model of diffusion then began with the enhanced swelling, while thewhole plasticizer migration obeyed first-order kinetics. Comparatively, the swelling effectfrom65%ethanol aqueous and n-hexane was more obvious, which caused the comparablefilm relaxation and plasticizer diffusion, non-Fickian diffusion thus occurred.
Alongwith the plasticizer migration and the permeation of solvent in food simulants, theplasticizer-starch ester interaction and the chemical surroundings for plasticizer were changed,reducing the stability of C-O and stabilizing the plasticizer molecules. At the same time, theinter-and intra-macromolecular interaction was enhanced to make the amorphous chainsshrink, which compressed the whole ordered microregion with smaller and polydispersed size,the crystallite inside was compressed as well. The mobility of macromolecular chains wasdirectly weakened because of the plasticizer migration. The formed compact aggregationstructure and the crystallite exerted more intense restriction on the relaxations within the film.It was meant that when immersed in food simulants, more compact aggregation structureformed to exert more intense effort on plasticizer molecules. Consequently, it was moredifficult for solvent diffusion and further plasticizer migration. Accordingly, the physicalmodel of influencing mechanism was established to describe the structural changes affectingplasticizer migration in different food simulants.
During the thermal processing, more distilled water entered into the film matrix toaggravate the swelling, result in aggregation structural changes and thus accelerate theplasticizer migration. Due to the compact structure within the ordered microregion, morewater molecules were promoted to permeate the amorphous region, so as to delaying themacromolecular shrink after plasticizer migration. On the other hand, the chains mobility was enhanced by thermal treatment, which caused the macromolecules at the edge of the orderedmicroregion to become amorphous. The whole ordered microregion was decreased withslightly destructive crystallite inside, the blocking effect on plasticizer migration and waterpermeation was thus weakened. More water entered the film matrix to dissolve plasticizer,and thermal treatment increased the plasticizer mobility as well, consequently, the plasticizermigration was facilitated. Accordingly, the mechanism model describing the structuralchanges affecting plasticizer migration during thermal processing was proposed.
The relevance connected plasticizer migration with microstructure and interface structurethe starch-based film, as well as the changes during thermal processing, was proposed in thisdissertation. Moreover, the multilevel structural changes of the material and its effect onplasticizer migration were understood, which could provide basic data and theory forrestraining plasticizer migration from biodegradable starch-based food packaging material andguiding the reasonable design and safe application of this novel packaging material.
选择高取代度酯化淀粉（DS=2.49）为基材，以三乙酸甘油酯为增塑剂，运用现代分析技术深入研究了增塑剂分布状态及增塑剂与淀粉分子的相互作用以及由此导致的膜材结晶结构、微区有序聚集态结构和热力学性能的变化规律。结果表明，增塑剂添加到淀粉基膜材后，增塑剂和酯化淀粉之间产生了以范德华力为主的相互作用，导致增塑剂与酯化淀粉的醚键增强，而分子本身更活跃。同时，增塑剂扩大了淀粉分子链间距离，增大链段运动性，致使部分链段相互靠近并排列更规整，在原本相对有序的微区中形成分散的微晶结构，对分子链运动产生一定的限制作用。此外，微晶形成过程中，增塑剂分子被挤到临近无定形区域形成了“增塑剂富集区”，通过扩张无定形区给大分子运动提供更多的空间，促进了膜材内不同尺度的松弛过程，参与玻璃化转变的分子链段聚集体的尺度变大。
当淀粉基膜材与食品模拟体系接触后，基于食品模拟体系/增塑剂/膜材基体之间的亲和性差异，食品模拟体系溶剂对膜材产生不同溶胀作用后，导致增塑剂迁移过程不同。在亲和性小的蒸馏水和4%乙酸中，增塑剂前期迁移首先遵循菲克第二扩散定律，随着溶胀作用增强，迁移过程逐渐转变为非菲克扩散，整体迁移过程较符合一级动力学；而在亲和性大的65%乙醇和正己烷体系中，溶胀作用更剧烈，膜材松弛与增塑剂迁移速度相当，增塑剂迁移呈现非菲克扩散特征。
随着增塑剂迁出和食品模拟体系溶剂分子渗透，增塑剂/酯化淀粉间的相互作用力发生改变，增塑剂分子所处化学环境改变，醚键变得不稳定，增塑剂分子稳定性增强。同时，淀粉分子链内/间作用力加强，无定形链段发生收缩聚拢，有序微区整体被挤压，尺寸减小且呈现出多分散性，且微区内部微晶结构收缩。此外，增塑剂迁出弱化不同尺度上的分子链运动性，致密的聚集态结构和有序微区中微晶聚集对膜材中各级松弛过程产生更大限制。也就是说，在食品模拟体系的浸泡过程中，增塑剂分子受到的整体作用力增大，膜材形成更致密聚集态结构，增塑剂分子迁移和溶剂渗透需克服的内摩擦阻力增大，因此，淀粉基膜材增塑剂迁移过程受到抑制。据此，提出了不同食品模拟体系下淀粉基膜材结构变化对增塑剂影响迁移的机制模型。
在热加工过程中，更多水分子进入膜材内加剧溶胀作用，导致膜材聚集态结构发生改变，加速增塑剂迁出。而且，由于膜材有序微区分子链段排列紧密，热加工促进更多水分子渗透扩散到无定形区域，延缓了增塑剂迁移导致的分子链收缩。此外，热加工增强无定形链段运动性，导致有序微区边界的分子链排列成无定形态，有序微区整体缩小，且其内部微晶被轻微破坏，因此，对增塑剂迁出和水分子渗透的阻隔性减弱，更多水分子可进入膜材内溶解增塑剂分子。另外，增塑剂受热后分子运动强烈，因而增塑剂迁移在加热过程中加剧。据此，提出了热加工过程中膜材结构变化对增塑剂迁移影响的机制模型。
本论文提出了增塑剂迁移与膜材微结构、膜材/食品界面结构的关系及其在热加工过程中变化的模型，掌握了在不同食品模拟体系及热加工过程中食品包装材料多尺度结构变化以及由此带来的增塑剂迁移变化的规律，为进一步实现抑制淀粉基生物降解食品包装材料中增塑剂迁移、合理设计及安全使用淀粉基材料提供了基础数据和理论参考。
Alongwith increasing attention focused on food safety and protecting environment, theeco-friendly food packaging material with favorable safety and qualified performance hasbecome the research hotspot in the food packaging industry. Consequently, biodegradablenatural polymer packaging based on renewable resources has attracted more and moreinteresting. Thereinto, as an abundant natural resource with low price, starch has been appliedto produce the starch-based food packaging material, which is considered as one of the mostpromising novel packaging. However, it is hardly possible to avoid plasticizer, which is anessential processing agent involved in the design and manufacture of this novel packagingmaterial, migrating from the matrix into the food system. The plasticizer migration wouldchange the structure and performance of the packaging material, which could lead to thegradual decay of the protection to the food inside. Therefore, in this academic dissertation, itwas proposed as the breakthrough that the relations between plasticizer migration andstructural changes of the starch-based film, including the microstructure and the interfacecontacted with food system, as well as during thermal processing. Moreover, the interaction,crystalline structure and ordered aggregation structure on multiple scales, which changedwhen the material contacted with different food simulants and involved in thermal processingwere discussed, as well as the effect from these structural changes. Finally, themicro-structural factors of starch-based film that restricted the plasticizer migration wereobtained.
Hydrophobic starch ester with high substitute degree (DS=2.49) and triacetin were chosenas the base material and plasticizer. Modern analytical techniques were applied to detect theeffect from plasticizer distribution and plasticizer-starch ester interaction on the crystallinestructure, microstructure and thermodynamics properties. Results showed that new interaction(mainly as Van der Waals force) formed to enhance C-O in plasticizer and starch estermolecules and activate the whole molecules. Meanwhile, the distance betweenmacromolecular chains was enlarged, and the chain mobility was increased to approach toeach other and arranged in more order, which facilitated crystallite formation dispersed withinthe ordered microregion, restricting the chain mobility to some extent. Simultaneously, the plasticizer molecules previously distributed within crystallite were squeezed to formamorphous “plasticizer-rich domain”. The amorphous region was enlarged to provide largerfree volume for macromolecular chains, thus promoting relaxations on different scale. Inaddition, the dimension of chain aggregation involved in glass-rubber transition increased.
When starch-based film contacted with the food stimulants, based on the different affinityamong simulants, plasticizer and film matrix, the diverse swelling behavior occurred,resulting in different migration process. Distilled water and4%acetic acid aqueous with lowaffinity exerted mild swelling effect on the films, and the migration obeyed the Fick’s secondlaw. The non-Fickian model of diffusion then began with the enhanced swelling, while thewhole plasticizer migration obeyed first-order kinetics. Comparatively, the swelling effectfrom65%ethanol aqueous and n-hexane was more obvious, which caused the comparablefilm relaxation and plasticizer diffusion, non-Fickian diffusion thus occurred.
Alongwith the plasticizer migration and the permeation of solvent in food simulants, theplasticizer-starch ester interaction and the chemical surroundings for plasticizer were changed,reducing the stability of C-O and stabilizing the plasticizer molecules. At the same time, theinter-and intra-macromolecular interaction was enhanced to make the amorphous chainsshrink, which compressed the whole ordered microregion with smaller and polydispersed size,the crystallite inside was compressed as well. The mobility of macromolecular chains wasdirectly weakened because of the plasticizer migration. The formed compact aggregationstructure and the crystallite exerted more intense restriction on the relaxations within the film.It was meant that when immersed in food simulants, more compact aggregation structureformed to exert more intense effort on plasticizer molecules. Consequently, it was moredifficult for solvent diffusion and further plasticizer migration. Accordingly, the physicalmodel of influencing mechanism was established to describe the structural changes affectingplasticizer migration in different food simulants.
During the thermal processing, more distilled water entered into the film matrix toaggravate the swelling, result in aggregation structural changes and thus accelerate theplasticizer migration. Due to the compact structure within the ordered microregion, morewater molecules were promoted to permeate the amorphous region, so as to delaying themacromolecular shrink after plasticizer migration. On the other hand, the chains mobility was enhanced by thermal treatment, which caused the macromolecules at the edge of the orderedmicroregion to become amorphous. The whole ordered microregion was decreased withslightly destructive crystallite inside, the blocking effect on plasticizer migration and waterpermeation was thus weakened. More water entered the film matrix to dissolve plasticizer,and thermal treatment increased the plasticizer mobility as well, consequently, the plasticizermigration was facilitated. Accordingly, the mechanism model describing the structuralchanges affecting plasticizer migration during thermal processing was proposed.
The relevance connected plasticizer migration with microstructure and interface structurethe starch-based film, as well as the changes during thermal processing, was proposed in thisdissertation. Moreover, the multilevel structural changes of the material and its effect onplasticizer migration were understood, which could provide basic data and theory forrestraining plasticizer migration from biodegradable starch-based food packaging material andguiding the reasonable design and safe application of this novel packaging material.
引文
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