生物降解高分子纳米复合材料的制备与性能研究
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摘要
生物降解高分子材料近几年来越来越引起人们的兴趣和重视。在众多生物可降解高分子材料中，聚已内酯（PCL）和聚乳酸（PLA）由于其良好的力学性能、生物降解性和生物相容性而受到广泛关注。但是，PCL熔点低、稳定性差、受力容易变形等缺陷限制了其发展。而PLA的韧性、尺寸稳定性、气体阻隔性、降解速率慢的不足也限制了其进一步的发展。本论文结合这两种材料在通用材料使用方面的缺陷和不足，同时结合了纳米材料和复合材料的特点，选用表面含有大量羟基的刚性纳米粒子SiO_2对PCL和PLA进行改性，选用了不同的有机MMT对PLA进行改性，制备了性能优越的新型生物降解复合材料，并研究了纳米复合材料的力学性能、结晶性能、流变性能及热力学性能，主要内容和结论如下：
（1）通过熔融共混的方法制备了PCL/SiO_2纳米复合材料，并对其形态、流变行为、力学行为和生物降解性进行了研究。SiO_2纳米粒子在PCL中具有良好的分散性，当其含量不超过3wt%时，基本达到单分散，当SiO_2含量继续增加时出现团聚现象。当SiO_2纳米粒子含量达到9wt%时，SiO_2逾渗网络结构形成。在低频区，样品表现出类固响应，PCL分子链的长程运动受到很大的限制。加入SiO_2后，由于SiO_2和PCL基体的良好的相容性以及SiO_2在基体中较好的分散性，复合材料的拉伸强度、模量、屈服应力都得到了提高，并且复合材料仍然保持较好的柔软性。由于酶分子更容易进攻PCL分子链的酯基，所以PCL/SiO_2纳米复合材料的降解速率比纯PCL快。
（2）用DSC方法研究了在不同降温速率下纯PCL及其PCL/SiO_2纳米复合材料非等温熔融结晶，复合材料的结晶峰温度高于纯PCL的结晶峰温度。并且随着复合材料中SiO_2含量的增加，纯PCL及其复合材料的结晶峰温度先增高后降低。用DSC方法研究了在不同结晶温度下纯PCL及其PCL/SiO_2纳米复合材料等温熔融结晶动力学，复合材料的结晶速率比纯PCL的快。并且随着SiO_2含量的增加，结晶速率先增加后降低。等温和非等温结晶研究表明，加入SiO_2后，PCL结晶得到加强，并且加强的程度受SiO_2含量的影响。SiO_2对PCL结晶的影响有两方面：SiO_2的存在一方面为PCL结晶提供了异相成核剂，另一方面限制了PCL晶体的生长。所以当SiO_2含量从1wt%增加到9wt%时，PCL/SiO_2纳米复合材料等温和非等温结晶过程都是先增快后变慢。PCL/SiO_2纳米复合材料的结晶机理和晶体结构与纯PCL相比没有发生变化。
（3）通过熔融共混的方法制备了生物可降解PLA/SiO_2纳米复合材料，SiO_2含量分别为1、3、5、7、9wt%。SEM观察说明当SiO_2含量小于5wt%时，SiO_2纳米粒子在PLA中具有良好的分散性，只有少量团聚并且团聚尺寸小于100nm。当SiO_2含量超过5wt%时，一些团聚体可达到250nm。当SiO_2纳米粒子含量达到5wt%时，SiO_2逾渗网络结构形成。一旦逾渗网络结构形成，样品的模量随温度的升高而上升。PLA/SiO_2纳米复合材料的降解速率比纯PLA快。这一点对于PLA的实际应用具有重要的意义。并且进一步讨论了纯PLA及PLA/SiO_2纳米复合材料的降解机理，认为其发生的是表面侵蚀。
（4）选用了三种不同MMT通过熔融共混的方法制备了生物可降解PLA/MMT复合材料，MMT含量分别为0、1、3、5wt%。DSC测试结果说明MMT的加入促进了PLA的结晶过程，并且促进作用由强到弱的顺序为：MMT-Alk>MMT-COOH>MMT-OH。当MMT-Alk含量为3-5wt%时，复合材料形成流变网络逾渗结构，MMT-COOH含量大于5wt%时，MMT逾渗网络结构形成。一旦逾渗网络结构形成，样品的模量随温度的变化变化不大。而MMT-OH在测试范围内没有形成逾渗网络结构。
The interest in biodegradable polymers has recently gained exponential momentum,and, within that broad family, poly (ε-caprolactone)(PCL) and poly(lactic acid)(PLA)are promising materials because of its flexibility, good biodegradability andbiocompatibility. However, PCL has low melting point, poor stability, and tendency torack when stressed limited its widely applications. Other properties of PLA, such astoughness, dimensional stability, gas barrier properties and slow biodegradation rate, areoften not sufficient for its further processing and end-use applications. In the presentdissertation, based on the disadvantages of nanometer material and nanocomposites,biodegradable PCL/silica nanocomposites and PLA/silica at various silica loadingsranging from1to9wt%were prepared via direct melt compounding method. Inaddition to this, biodegradable PLA/organic clay were prepared too. Main contents andconclusions are as follows:
(1) Biodegradable PCL/silica nanocomposites with different silica loadings wereprepared through direct melt compounding method. When the silica content was <3wt%, the nanoparticles dispersed evenly in the PCL matrix and exhibited onlyaggregates with particle size of less than100nm. At a higher silica content (≥3wt%),the number of large aggregates increased markedly. Some of the aggregates evenexceeded the size of250nm. As the silica loadings reaches up to9wt%, percolatedsilica network structures can be formed. The sample exhibit evident solid-like response in the low frequency region. The long-range motion of PCL chains is highly restrained.The tensile strength, modulus and yield strength values of the nanocomposites wereenhanced by the incorporation of inorganic silica nanoparticles owing to the goodcompatibility of the silica with PCL matrix as well as uniform dispersion of silica; at thesame time, the nanocomposites still retained good ductility. The biodegradation rateshave been enhanced obviously in the PCL/silica nanocomposites than in neat PCL dueto a facile attack of the enzyme molecule toward the ester groups of PCL chains, whichmay be of great use and importance for the wider practical application of PCL.
(2) Nonisothermal melt crystallization of neat PCL and the PCL/silicananocomposites was studied with DSC at various cooling rates. The crystallization peaktemperature is higher in the nanocomposites than in neat PCL, which first increases anddecreases with increasing the silica loading. Isothermal melt crystallization kinetics ofneat PCL and the PCL/silica nanocomposites was also investigated with DSC atdifferent crystallization temperatures. The overall crystallization rate is faster in thenanocomposites than in neat PCL, which also first increases and then decreases withincreasing the silica loading. For both nonisothermal and isothermal melt crystallizationstudies, the crystallization of PCL is enhanced by the presence of silica, and theenhancement is influenced by the silica loading in the nanocomposites. The effect ofsilica on the crystallization is twofold: the presence of silica may provide a number ofheterogeneous nucleation sites for the PCL crystallization while the aggregates of silicamay restrict crystal growth of PCL. Therefore, the overall crystallization of PCL firstincreases and then decreases with increasing the silica loading from1to9wt%in the PCL/silica nanocomposites for both nonisothermal and isothermal melt crystallizationof PCL. However, the crystallization mechanism and crystal structure of PCL remainalmost unchanged after nanocomposites preparation.
(3) ESEM observation indicates that when the silica content was <5wt%, the silicadispersed evenly in the PLA matrix and exhibited only aggregates with particle size ofless than100nm. However, at a higher silica content (>5wt%), some of the aggregateseven exceeded the size of250nm. As the silica loadings reaches up to5wt%,percolated silica network structures can be formed. Once the percolated silica networkstructures formed, the modulus increases with increase of temperature evidently. Thebiodegradation rates have been enhanced obviously in the PLA/silica nanocompositesthan in neat PLA, which may be of great use and importance for the wider practicalapplication of PLA. The erosion mechanism of neat PLA and its nanocomposites wasfurther discussed, and the biodegradation of neat PLA and its nanocomposites mayproceed via surface erosion.
(4) Biodegradable PLA/clay nanocomposites with different clay loadings anddifferent kind of clay were prepared through direct melt compounding method. Thecrystallization of PLA is enhanced by the presence of clay from DSC test result and theenhancement order is: MMT-Alk>MMT-COOH>MMT-OH. As the MMT-ALk loadingsis3-5wt%, and MMT-COOH loading reaches up to5wt%, percolated clay networkstructures can be formed. Once the percolated clay network structures formed, themodulus increases with increase of temperature smally. Moreover, percolated claynetwork structures can not be formed on this condition.
（1）通过熔融共混的方法制备了PCL/SiO_2纳米复合材料，并对其形态、流变行为、力学行为和生物降解性进行了研究。SiO_2纳米粒子在PCL中具有良好的分散性，当其含量不超过3wt%时，基本达到单分散，当SiO_2含量继续增加时出现团聚现象。当SiO_2纳米粒子含量达到9wt%时，SiO_2逾渗网络结构形成。在低频区，样品表现出类固响应，PCL分子链的长程运动受到很大的限制。加入SiO_2后，由于SiO_2和PCL基体的良好的相容性以及SiO_2在基体中较好的分散性，复合材料的拉伸强度、模量、屈服应力都得到了提高，并且复合材料仍然保持较好的柔软性。由于酶分子更容易进攻PCL分子链的酯基，所以PCL/SiO_2纳米复合材料的降解速率比纯PCL快。
（2）用DSC方法研究了在不同降温速率下纯PCL及其PCL/SiO_2纳米复合材料非等温熔融结晶，复合材料的结晶峰温度高于纯PCL的结晶峰温度。并且随着复合材料中SiO_2含量的增加，纯PCL及其复合材料的结晶峰温度先增高后降低。用DSC方法研究了在不同结晶温度下纯PCL及其PCL/SiO_2纳米复合材料等温熔融结晶动力学，复合材料的结晶速率比纯PCL的快。并且随着SiO_2含量的增加，结晶速率先增加后降低。等温和非等温结晶研究表明，加入SiO_2后，PCL结晶得到加强，并且加强的程度受SiO_2含量的影响。SiO_2对PCL结晶的影响有两方面：SiO_2的存在一方面为PCL结晶提供了异相成核剂，另一方面限制了PCL晶体的生长。所以当SiO_2含量从1wt%增加到9wt%时，PCL/SiO_2纳米复合材料等温和非等温结晶过程都是先增快后变慢。PCL/SiO_2纳米复合材料的结晶机理和晶体结构与纯PCL相比没有发生变化。
（3）通过熔融共混的方法制备了生物可降解PLA/SiO_2纳米复合材料，SiO_2含量分别为1、3、5、7、9wt%。SEM观察说明当SiO_2含量小于5wt%时，SiO_2纳米粒子在PLA中具有良好的分散性，只有少量团聚并且团聚尺寸小于100nm。当SiO_2含量超过5wt%时，一些团聚体可达到250nm。当SiO_2纳米粒子含量达到5wt%时，SiO_2逾渗网络结构形成。一旦逾渗网络结构形成，样品的模量随温度的升高而上升。PLA/SiO_2纳米复合材料的降解速率比纯PLA快。这一点对于PLA的实际应用具有重要的意义。并且进一步讨论了纯PLA及PLA/SiO_2纳米复合材料的降解机理，认为其发生的是表面侵蚀。
（4）选用了三种不同MMT通过熔融共混的方法制备了生物可降解PLA/MMT复合材料，MMT含量分别为0、1、3、5wt%。DSC测试结果说明MMT的加入促进了PLA的结晶过程，并且促进作用由强到弱的顺序为：MMT-Alk>MMT-COOH>MMT-OH。当MMT-Alk含量为3-5wt%时，复合材料形成流变网络逾渗结构，MMT-COOH含量大于5wt%时，MMT逾渗网络结构形成。一旦逾渗网络结构形成，样品的模量随温度的变化变化不大。而MMT-OH在测试范围内没有形成逾渗网络结构。
The interest in biodegradable polymers has recently gained exponential momentum,and, within that broad family, poly (ε-caprolactone)(PCL) and poly(lactic acid)(PLA)are promising materials because of its flexibility, good biodegradability andbiocompatibility. However, PCL has low melting point, poor stability, and tendency torack when stressed limited its widely applications. Other properties of PLA, such astoughness, dimensional stability, gas barrier properties and slow biodegradation rate, areoften not sufficient for its further processing and end-use applications. In the presentdissertation, based on the disadvantages of nanometer material and nanocomposites,biodegradable PCL/silica nanocomposites and PLA/silica at various silica loadingsranging from1to9wt%were prepared via direct melt compounding method. Inaddition to this, biodegradable PLA/organic clay were prepared too. Main contents andconclusions are as follows:
(1) Biodegradable PCL/silica nanocomposites with different silica loadings wereprepared through direct melt compounding method. When the silica content was <3wt%, the nanoparticles dispersed evenly in the PCL matrix and exhibited onlyaggregates with particle size of less than100nm. At a higher silica content (≥3wt%),the number of large aggregates increased markedly. Some of the aggregates evenexceeded the size of250nm. As the silica loadings reaches up to9wt%, percolatedsilica network structures can be formed. The sample exhibit evident solid-like response in the low frequency region. The long-range motion of PCL chains is highly restrained.The tensile strength, modulus and yield strength values of the nanocomposites wereenhanced by the incorporation of inorganic silica nanoparticles owing to the goodcompatibility of the silica with PCL matrix as well as uniform dispersion of silica; at thesame time, the nanocomposites still retained good ductility. The biodegradation rateshave been enhanced obviously in the PCL/silica nanocomposites than in neat PCL dueto a facile attack of the enzyme molecule toward the ester groups of PCL chains, whichmay be of great use and importance for the wider practical application of PCL.
(2) Nonisothermal melt crystallization of neat PCL and the PCL/silicananocomposites was studied with DSC at various cooling rates. The crystallization peaktemperature is higher in the nanocomposites than in neat PCL, which first increases anddecreases with increasing the silica loading. Isothermal melt crystallization kinetics ofneat PCL and the PCL/silica nanocomposites was also investigated with DSC atdifferent crystallization temperatures. The overall crystallization rate is faster in thenanocomposites than in neat PCL, which also first increases and then decreases withincreasing the silica loading. For both nonisothermal and isothermal melt crystallizationstudies, the crystallization of PCL is enhanced by the presence of silica, and theenhancement is influenced by the silica loading in the nanocomposites. The effect ofsilica on the crystallization is twofold: the presence of silica may provide a number ofheterogeneous nucleation sites for the PCL crystallization while the aggregates of silicamay restrict crystal growth of PCL. Therefore, the overall crystallization of PCL firstincreases and then decreases with increasing the silica loading from1to9wt%in the PCL/silica nanocomposites for both nonisothermal and isothermal melt crystallizationof PCL. However, the crystallization mechanism and crystal structure of PCL remainalmost unchanged after nanocomposites preparation.
(3) ESEM observation indicates that when the silica content was <5wt%, the silicadispersed evenly in the PLA matrix and exhibited only aggregates with particle size ofless than100nm. However, at a higher silica content (>5wt%), some of the aggregateseven exceeded the size of250nm. As the silica loadings reaches up to5wt%,percolated silica network structures can be formed. Once the percolated silica networkstructures formed, the modulus increases with increase of temperature evidently. Thebiodegradation rates have been enhanced obviously in the PLA/silica nanocompositesthan in neat PLA, which may be of great use and importance for the wider practicalapplication of PLA. The erosion mechanism of neat PLA and its nanocomposites wasfurther discussed, and the biodegradation of neat PLA and its nanocomposites mayproceed via surface erosion.
(4) Biodegradable PLA/clay nanocomposites with different clay loadings anddifferent kind of clay were prepared through direct melt compounding method. Thecrystallization of PLA is enhanced by the presence of clay from DSC test result and theenhancement order is: MMT-Alk>MMT-COOH>MMT-OH. As the MMT-ALk loadingsis3-5wt%, and MMT-COOH loading reaches up to5wt%, percolated clay networkstructures can be formed. Once the percolated clay network structures formed, themodulus increases with increase of temperature smally. Moreover, percolated claynetwork structures can not be formed on this condition.
引文
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