纤维素纳米纤丝/丙烯酸树脂复合材料的研究
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摘要
纤维素在制备成纳米尺度后具有高长径比、高纯度、高结晶度、高杨氏模量、高强度、可降解以及好的生物相容性等优点。由于这些特别的性能及其重要的应用价值，生物质纤维素纳米纤丝成为近年来纤维素研究领域的研究热点。本论文内容大概包括：（1）研究生物质纤维素纳米丝的制备方法；（2）比较不同纤维素原材料对制备生物质纤维素纳米纤丝的影响；（3）比较不同机械分离对制备生物质纤维素纳米纤丝的影响；（4）分析生物质纤维素纳米纤丝的微观特征、其薄膜的力学性能和热稳定性；（5）研究生物质纤维素纳米纤丝/丙烯酸树脂复合材料的力学性能、热稳定性和透光性；（6）比较不同含量生物质纤维素纳米纤丝对纳米复合材料的性能影响。试验后得出以下结论：
1.以木粉为主要原料，利用化学预处理去除了木粉中的木质素与大部分半纤维素并用HCl进行了开纤处理，然后借助机械研磨处理制备出高长径比的、网状结构的木质纤维素纳米纤丝。
2.利用化学预处理结合机械研磨处理，分别从木材、瓦楞纸浆和棉花三种生物原材料中分离出纤维素纳米纤丝，三种生物质纤维素纳米纤丝均具有高长径比与网状结构的特点。原料中“低”纤维素含量的木质纤维素纳米纤丝和瓦楞纸浆纤维素纳米纤丝的纤丝化程度非常均匀，而高纤维素含量的棉花纤维素纳米纤丝中仍存在部分纤丝聚集体。比较三种原料制备出的纤维素纳米纤丝的力学性能与热稳定性，得出机械研磨处理的棉花纤维素纳米纤丝的拉伸强度和弹性模量较木质纤维素纳米纤丝和瓦楞纸浆纤维素纳米纤丝略高，分别达到87.38MPa和3463.23MPa；而CTE值较木质纤维素纳米纤丝和瓦楞纸浆纤维素纳米纤丝略低，达到14ppm·K-1；棉花纤维素纳米纤丝薄膜的拉伸断面效果不及木质纤维素纳米纤丝和瓦楞纸浆纤维素纳米纤丝。
3.不同机械处理所制备纤维素纳米纤丝均具有高长径比的网状结构，其中高强度超声/研磨/高压均质处理后的效果最好。比较四种机械处理得到的纳米纤丝薄膜的力学性能与热稳定性，高强度超声/研磨/高压均质处理的拉伸强度和弹性模量比其他机械处理都高，分别达到159.78MPa和6467.23MPa，CTE却最低，达到12ppm·K-1，其拉伸断面效果也最好。
4.将制备的木质纤维素纳米纤丝薄膜浸渍在透明丙烯酸树脂ABPE10中，加压浸渍比未加压浸渍的薄膜透明。木质纤维素纳米纤丝的加入提高了丙烯酸树脂ABPE10的拉伸强度与弹性模量，分别达到了56.52MPa和2613.84MPa，同时降低了树脂的热膨胀系数（23ppm·K-1），但是也降低了纯丙烯酸树脂ABPE10的光的透过率。
5.在丙烯酸树脂ABPE10中加入不同含量的木质纤维素纳米纤丝薄膜，得到了不同纳米复合薄膜的透明度肉眼很难区分，但其拉伸强度和弹性模量随着纤维含量的增加而增加，CTE值和光的透过率随之降低。
6.基于本论文制备出的这种强度大、热稳定性好的生物质纤维素纳米纤丝透明复合薄膜有望应用在可弯曲性OLED的基底材料中。
Recently, cellulose nanofibers (CNFs) have attracted wide attention by researchers due totheir high aspect ratio, high purity, high crystallinity, high Young modulus, high strength,biodegradable and good biocompatibility. In this thesis, the main contents are:(1) Study inpreparation of biomass CNFs;(2) Comparison with different effects that raw materials have onproperties of biomass CNFs film;(3) Comparison with different effects that mechanicalseparations have on properties of biomass CNFs;(4) Analysis on the micromorphology ofbiomass CNFs and mechanical properties, thermostability of their films;(5)Study in mechanicalproperties, thermostability and regular transmittance of biomass CNFs/ABPE10composites;(6)Comparison with different effects that fiber contents have on properties of CNFs/ABPE10composites. The main conclusions are as follows:
1. The use of chemical pretreatment removed lignin and most of the hemicellulose in woodraw material, and using HCl could help to open fibers. Then, with grinding treatment, the highaspect ratio, mesh tangle morphology of wood CNFs were prepared.
2. After chemical pretreatment combining with grinding, we could extract CNFs fromwood, corrugated paper pulp and cotton. All of the nanofibers had high aspect ratio and meshtangle morphology. CNFs of the wood and corrugated paper which contain “low” cellulosewere fibrillated well while some of the aggregates existed in cotton CNFs. When CNFs fromdifferent raw materials were compared, tensile strength and elastic modulus of cotton CNFsfilm were obtained,87.38MPa and3464.23MPa, respectively, which were higher than CNFs ofwood and corrugated paper. However, the CTE of cotton CNFs film (14ppm·K-1) was lowerthan the other two kinds of CNFs. Besides, the fracture surface of cotton CNFs film was worsethan film of wood CNFs and corrugated paper CNFs.
3. All of the CNFs extracted by different mechanical treatment had high aspect ratio andmesh tangle morphology. High intensity ultrasonication/grinding/high pressure homogeneitytreatment was the best method in them. Tensile strength and elastic modulus of it were thegreatest,159.78MPa and6467.23MPa, respectively. CTE of it was the lowest, which was only12ppm· K-1. Moreover, the fracture surface of CNFs treated by high intensityultrasonication/grinding/high pressure homogeneity was excellent.
4. Wood CNFs film was impregnated in transparent acrylic resins ABPE10under pressureto prepare wood CNFs/ABPE10composites, which was more transparent than the nonpresssureone. When adding CNFs to acrylic resins, the tensile strength and elastic modulus ofnanocomposites were improved to56.52MPa and2613.84MPa, respectively, while CTE wasreduced to23ppm·K-1. The regular transmittance of composites was also decreased.
5. Different CNFs contents were added to acrylic resins to prepare different nanocomposites which transparency could hardly be distinguished. However, with the CNFscontent increased, the tensile strength and elastic modulus of nanocomposites were improved,while the CTE and regular transmittance decreased.
6. Based on the paper, the CNFs reinforced nanocomposites which were strong andthermostable have the potential to be used as base substrate for flexible organic light-emittingdiode displays (FOLEDs).
1.以木粉为主要原料，利用化学预处理去除了木粉中的木质素与大部分半纤维素并用HCl进行了开纤处理，然后借助机械研磨处理制备出高长径比的、网状结构的木质纤维素纳米纤丝。
2.利用化学预处理结合机械研磨处理，分别从木材、瓦楞纸浆和棉花三种生物原材料中分离出纤维素纳米纤丝，三种生物质纤维素纳米纤丝均具有高长径比与网状结构的特点。原料中“低”纤维素含量的木质纤维素纳米纤丝和瓦楞纸浆纤维素纳米纤丝的纤丝化程度非常均匀，而高纤维素含量的棉花纤维素纳米纤丝中仍存在部分纤丝聚集体。比较三种原料制备出的纤维素纳米纤丝的力学性能与热稳定性，得出机械研磨处理的棉花纤维素纳米纤丝的拉伸强度和弹性模量较木质纤维素纳米纤丝和瓦楞纸浆纤维素纳米纤丝略高，分别达到87.38MPa和3463.23MPa；而CTE值较木质纤维素纳米纤丝和瓦楞纸浆纤维素纳米纤丝略低，达到14ppm·K-1；棉花纤维素纳米纤丝薄膜的拉伸断面效果不及木质纤维素纳米纤丝和瓦楞纸浆纤维素纳米纤丝。
3.不同机械处理所制备纤维素纳米纤丝均具有高长径比的网状结构，其中高强度超声/研磨/高压均质处理后的效果最好。比较四种机械处理得到的纳米纤丝薄膜的力学性能与热稳定性，高强度超声/研磨/高压均质处理的拉伸强度和弹性模量比其他机械处理都高，分别达到159.78MPa和6467.23MPa，CTE却最低，达到12ppm·K-1，其拉伸断面效果也最好。
4.将制备的木质纤维素纳米纤丝薄膜浸渍在透明丙烯酸树脂ABPE10中，加压浸渍比未加压浸渍的薄膜透明。木质纤维素纳米纤丝的加入提高了丙烯酸树脂ABPE10的拉伸强度与弹性模量，分别达到了56.52MPa和2613.84MPa，同时降低了树脂的热膨胀系数（23ppm·K-1），但是也降低了纯丙烯酸树脂ABPE10的光的透过率。
5.在丙烯酸树脂ABPE10中加入不同含量的木质纤维素纳米纤丝薄膜，得到了不同纳米复合薄膜的透明度肉眼很难区分，但其拉伸强度和弹性模量随着纤维含量的增加而增加，CTE值和光的透过率随之降低。
6.基于本论文制备出的这种强度大、热稳定性好的生物质纤维素纳米纤丝透明复合薄膜有望应用在可弯曲性OLED的基底材料中。
Recently, cellulose nanofibers (CNFs) have attracted wide attention by researchers due totheir high aspect ratio, high purity, high crystallinity, high Young modulus, high strength,biodegradable and good biocompatibility. In this thesis, the main contents are:(1) Study inpreparation of biomass CNFs;(2) Comparison with different effects that raw materials have onproperties of biomass CNFs film;(3) Comparison with different effects that mechanicalseparations have on properties of biomass CNFs;(4) Analysis on the micromorphology ofbiomass CNFs and mechanical properties, thermostability of their films;(5)Study in mechanicalproperties, thermostability and regular transmittance of biomass CNFs/ABPE10composites;(6)Comparison with different effects that fiber contents have on properties of CNFs/ABPE10composites. The main conclusions are as follows:
1. The use of chemical pretreatment removed lignin and most of the hemicellulose in woodraw material, and using HCl could help to open fibers. Then, with grinding treatment, the highaspect ratio, mesh tangle morphology of wood CNFs were prepared.
2. After chemical pretreatment combining with grinding, we could extract CNFs fromwood, corrugated paper pulp and cotton. All of the nanofibers had high aspect ratio and meshtangle morphology. CNFs of the wood and corrugated paper which contain “low” cellulosewere fibrillated well while some of the aggregates existed in cotton CNFs. When CNFs fromdifferent raw materials were compared, tensile strength and elastic modulus of cotton CNFsfilm were obtained,87.38MPa and3464.23MPa, respectively, which were higher than CNFs ofwood and corrugated paper. However, the CTE of cotton CNFs film (14ppm·K-1) was lowerthan the other two kinds of CNFs. Besides, the fracture surface of cotton CNFs film was worsethan film of wood CNFs and corrugated paper CNFs.
3. All of the CNFs extracted by different mechanical treatment had high aspect ratio andmesh tangle morphology. High intensity ultrasonication/grinding/high pressure homogeneitytreatment was the best method in them. Tensile strength and elastic modulus of it were thegreatest,159.78MPa and6467.23MPa, respectively. CTE of it was the lowest, which was only12ppm· K-1. Moreover, the fracture surface of CNFs treated by high intensityultrasonication/grinding/high pressure homogeneity was excellent.
4. Wood CNFs film was impregnated in transparent acrylic resins ABPE10under pressureto prepare wood CNFs/ABPE10composites, which was more transparent than the nonpresssureone. When adding CNFs to acrylic resins, the tensile strength and elastic modulus ofnanocomposites were improved to56.52MPa and2613.84MPa, respectively, while CTE wasreduced to23ppm·K-1. The regular transmittance of composites was also decreased.
5. Different CNFs contents were added to acrylic resins to prepare different nanocomposites which transparency could hardly be distinguished. However, with the CNFscontent increased, the tensile strength and elastic modulus of nanocomposites were improved,while the CTE and regular transmittance decreased.
6. Based on the paper, the CNFs reinforced nanocomposites which were strong andthermostable have the potential to be used as base substrate for flexible organic light-emittingdiode displays (FOLEDs).
引文
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