植物纤维/ABS木塑复合材料的制备、结构与性能研究
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摘要
木塑复合材料（Wood Plastic Composites---WPC）是近年来国际上兴起的一种新型环保材料，它是由木粉、竹粉、稻糠、秸秆等植物纤维与热塑性塑料配以特殊功能改性剂及其他助剂，经塑料成型加工工艺制成的性能优良的复合材料。木塑复合材料综合了植物纤维和高分子材料的诸多优点，能大量替代木材，可有效缓解我国森林资源贫乏、木材供应紧缺的现状，同时它也解决了塑料、木材行业废弃资源的再生利用问题，是一种极具发展前途的低碳、绿色、可循环、可再生的材料。近年来，国内外对于木塑复合材料的研究开发较多，但主要集中在聚氯乙烯、聚乙烯、聚丙烯基体的木塑复合材料，而对ABS基木塑复合材料的相关研究则较少。选用ABS树脂作为基体，制备新型性能优良的ABS基木塑复合材料，对于提高木塑复合材料的性能，拓宽木塑复合材料应用领域具有重要的实际意义。
本论文首先研究了竹粉、桉木粉、柏木粉、松木粉和樟木粉五种植物纤维的基本物化性能，并采用薄层毛细渗透技术测定了五种植物纤维的表面接触角和表面自由能及其分量。在此基础上，选择表面自由能较低的竹粉作为研究对象，通过熔融共混法与ABS复合制备木塑复合材料，系统地研究了竹粉/ABS复合材料的结构与性能，探讨了竹粉用于制备木塑复合材料的改性方法。同时，将噁唑啉官能化的ABS(ABSm)作为界面改性剂用于改性ABS基木塑复合材料，并对其界面改性机理进行探讨。研究结果表明：
五种植物纤维均含有大量羟基，亲水性强，但热稳定性较差。由薄层毛细渗透技术测得五种植物纤维中桉木粉的表面自由能及其非极性分量最高，竹粉表面自由能及其非极性分量较低；与ABS复合时，桉木粉有比其他几种植物纤维更好的界面相容性，由其制备的木塑复合材料的力学性能优于其它四种植物纤维/ABS复合材料的力学性能。
含有大量极性羟基的竹粉与ABS树脂两相间相容性不佳，随着竹粉添加量的增大，竹粉/ABS复合材料的拉伸强度、弯曲强度和冲击强度降低，但其弯曲模量提高。同时，随着竹粉在ABS中用量的增加，复合材料的维卡软化温度逐渐提高，在一定程度上提高了复合材料的使用温度范围，但复合材料的热稳定性和加工性能有所降低，吸水率有所增加。在80目~180目的粒径范围内，除冲击强度外，竹粉/ABS复合材料的各项力学性能随着竹粉粒径的增大呈上升的趋势。但当竹粉粒径增至40目时，复合材料的力学性能反而有所降低。
噁唑啉官能化的ABS(ABSm)对竹粉/ABS复合材料体系有良好的增容作用，可明显提高复合材料的力学性能，改善复合材料的界面相容性。腈基转化率在30%左右的ABSm2用量为7phr时，复合材料的拉伸强度和弯曲强度分别为52MPa和91.4MPa，相比未改性试样分别提高了17.6%和35.2%，已经达到甚至超过了纯ABS的拉伸强度(50MPa)和弯曲强度(82.5MPa)。三种市售的界面改性剂苯乙烯-马来酸酐共聚物(SMA)、聚苯乙烯接枝马来酸酐(PS-g-MAH)、乙烯-醋酸乙烯酯共聚物接枝马来酸酐(EVA-g-MAH)中SMA的界面改性效果较好，但均不如ABSm。
研究了在常温和高温蒸煮条件下，碱液浓度和碱处理时间对竹粉的化学组成、结晶性能、热稳定性及形态结构的影响，得到常温碱处理的优化条件为4%NaOH溶液，处理时间为1h。经常温和高温蒸煮碱处理后可以除去竹粉表面的半纤维素、木质素和抽提物，提高竹粉的热稳定性。在两种条件下，当NaOH溶液浓度大于10%后，都会导致竹粉纤维素的晶型由纤维素Ⅰ向纤维素Ⅱ转变，使得竹粉的结晶度下降，热稳定性降低，纤维束状结构发生分离，纤维卷曲。
本论文将经乙酰化处理、常温碱处理和高温蒸煮处理的三种竹粉用于制备ABS基木塑复合材料，研究结果表明，预处理后的竹粉对ABS基木塑复合材料的力学性能都有不同程度的提高，其中高温蒸煮处理对复合材料力学性能的提高幅度最大，常温碱处理次之，而乙酰化处理对复合材料力学性能的影响不明显。进一步的研究表明，两种碱处理和界面改性剂SMA并用对竹粉/ABS复合材料均存在协同效应，能较大幅度的提高复合材料的力学性能，而两种碱处理和ABSm并用以及乙酰化处理和SMA并用则无协同效应。
Wood-plastic composite (WPC) is a new type of environmental material, which ismanufactured from blends of thermoplastics and plant fibers with a special functionalmodified agent and other additives using plastic molding process. The plant fibers includewood flour, bamboo fiber, rice husk and straw. WPC synthesizes the advantages of plant fiberand polymers. It is a low carbon, green, renewable materials with a great developable future.Itcan substitute plenty of wood and efficiently mitigate the status of our country's poor forestresources and demand. It will solve the problems in the recycling of waste plastics and woodresources. In recent years, research and development of WPC have been very popular inliterature, most of which were carried out using PVC, PE, and PP as matrix, but ABS asmatrix is very rare. The preparation of the WPC with ABS matrix has important practicalsignificance for improving its properties and broadening its application area.
The characteristics of five kinds of plant fibers were explored in this thesis firstly. Theywere bamboo fiber (BF), eucalypt fiber, cypress fiber, pine fiber and camphor fiber. Thecontact angle, surface free energy and its components of plant fibers were determined by theWashburn equation with the thin-layer wicking technique. Then the bamboo fiber wasselected for further investigation because of its lower surface free energy. BF/ABS compositeswere prepared by melt compounding. Then the structure and performance of the compositeswere systematically investigated. The modification methods of bamboo fiber that strengthenthe bonding between bamboo fiber and ABS matrix were also studied. Furthermore, ainterfacial modifier was synthesized from ABS. The influence of the interfacial modifier onthe performance of BF/ABS composites was investigated. The interfacial modificationmechanisms were also discussed.
The five kinds of plant fibers all contain a large number of hydroxyl groups, but theirthermal stability is not pretty well. Based on Washburn equation and the thin-layer wickingtechnique, the surface free energies of the plant fibers were calculated. Results demonstratethat eucalypt fiber has the highest surface free energy and non polar part; while bamboo fiberhas the lowest. As combined with the same plastics, the interfacial adhesion between eucalyptfiber and matrix is better than that of the others, so the mechanical properties of eucalyptfiber/ABS composites outperforms the other four.
The poor compatibility between bamboo fiber and ABS matrix limited the performanceof BF/ABS composites. The mechanical properties of BF/ABS composites, including tensilestrength, flexural strength and impact strength, decreased with the increasing bamboo fiber loading, but its flexural modulus increased. The Vicat temperature of BF/ABS compositesincreased with the increasing bamboo fiber loading, suggesting that the incorporation ofbamboo fiber could extend the operating temperature range of composites. Besides, theaddition of bamboo fiber had negative influence on the thermal stability， processingperformance and water absorptivity of BF/ABS composites. As the bamboo particle sizeswere between80and180meshes, the mechanical properties of the samples, besides impactstrength, exhibited a creasing tendency. However, the mechanical properties showed adecreasing tendency when the particle size was40meshes.
Oxazoline modified ABS(ABSm) improved the interactions between bamboo fiber andABS matrix and promoted better mechanical properties of the composites. The tensilestrength and flexural strength of BF/ABS composites were52MPa and91.4MPa whenABSm2was added, about17.6%and35.2%up. The conversion of the nitrile groups intooxazoline of ABSm2is about30%, the optimum dosage was7phr. Among three commerciallyavailable interface modifiers(SMA, PS-g-MAH, EVA-g-MAH), SMA has the best interfacemodified effect, but none of them is better than ABSm.
Alkali treated of bamboo fiber at room temperature and high temperature cooking werestudied. The effects of time and concentration of NaOH on the chemical composition,crystallizing structure, thermal characteristic and surface morphology of bamboo fiber werediscussed. And the optimum processing of alkali treatments at room temperature,concentration of NaOH4%,1h, were obtained. The alkali treatment of the bamboo fiberspromoted the partial removal of the hemicelluloses, extractives, and lignin which present onthe surface of the fiber, and improved its thermal stability. The crystalline structuretransformation of cellulose I into cellulose II was observed by X-ray diffraction for bamboofiber, when NaOH concentration exceeded10%. This would decrease the crystallinity andthermal stability of the bamboo fiber, while the fiber bundles partially break down and appearshrinkage.
The bamboo fibers after acetylation, alkali treated and high temperature alkali cookingwas used to prepare BF/ABS composite. Experiment result showed that different treatmentincreased the dynamic property of the composite by different degree.The two kinds of alkalitreatment had better effect on the BF/ABS composites, while the effect of acetylationtreatment was insignificant. Further studies showed that two kinds of alkali treatment usedtogether with SMA had synergistic effect, while they used together with ABSm andacetylation treatment used together with SMA had no synergistic effect.
本论文首先研究了竹粉、桉木粉、柏木粉、松木粉和樟木粉五种植物纤维的基本物化性能，并采用薄层毛细渗透技术测定了五种植物纤维的表面接触角和表面自由能及其分量。在此基础上，选择表面自由能较低的竹粉作为研究对象，通过熔融共混法与ABS复合制备木塑复合材料，系统地研究了竹粉/ABS复合材料的结构与性能，探讨了竹粉用于制备木塑复合材料的改性方法。同时，将噁唑啉官能化的ABS(ABSm)作为界面改性剂用于改性ABS基木塑复合材料，并对其界面改性机理进行探讨。研究结果表明：
五种植物纤维均含有大量羟基，亲水性强，但热稳定性较差。由薄层毛细渗透技术测得五种植物纤维中桉木粉的表面自由能及其非极性分量最高，竹粉表面自由能及其非极性分量较低；与ABS复合时，桉木粉有比其他几种植物纤维更好的界面相容性，由其制备的木塑复合材料的力学性能优于其它四种植物纤维/ABS复合材料的力学性能。
含有大量极性羟基的竹粉与ABS树脂两相间相容性不佳，随着竹粉添加量的增大，竹粉/ABS复合材料的拉伸强度、弯曲强度和冲击强度降低，但其弯曲模量提高。同时，随着竹粉在ABS中用量的增加，复合材料的维卡软化温度逐渐提高，在一定程度上提高了复合材料的使用温度范围，但复合材料的热稳定性和加工性能有所降低，吸水率有所增加。在80目~180目的粒径范围内，除冲击强度外，竹粉/ABS复合材料的各项力学性能随着竹粉粒径的增大呈上升的趋势。但当竹粉粒径增至40目时，复合材料的力学性能反而有所降低。
噁唑啉官能化的ABS(ABSm)对竹粉/ABS复合材料体系有良好的增容作用，可明显提高复合材料的力学性能，改善复合材料的界面相容性。腈基转化率在30%左右的ABSm2用量为7phr时，复合材料的拉伸强度和弯曲强度分别为52MPa和91.4MPa，相比未改性试样分别提高了17.6%和35.2%，已经达到甚至超过了纯ABS的拉伸强度(50MPa)和弯曲强度(82.5MPa)。三种市售的界面改性剂苯乙烯-马来酸酐共聚物(SMA)、聚苯乙烯接枝马来酸酐(PS-g-MAH)、乙烯-醋酸乙烯酯共聚物接枝马来酸酐(EVA-g-MAH)中SMA的界面改性效果较好，但均不如ABSm。
研究了在常温和高温蒸煮条件下，碱液浓度和碱处理时间对竹粉的化学组成、结晶性能、热稳定性及形态结构的影响，得到常温碱处理的优化条件为4%NaOH溶液，处理时间为1h。经常温和高温蒸煮碱处理后可以除去竹粉表面的半纤维素、木质素和抽提物，提高竹粉的热稳定性。在两种条件下，当NaOH溶液浓度大于10%后，都会导致竹粉纤维素的晶型由纤维素Ⅰ向纤维素Ⅱ转变，使得竹粉的结晶度下降，热稳定性降低，纤维束状结构发生分离，纤维卷曲。
本论文将经乙酰化处理、常温碱处理和高温蒸煮处理的三种竹粉用于制备ABS基木塑复合材料，研究结果表明，预处理后的竹粉对ABS基木塑复合材料的力学性能都有不同程度的提高，其中高温蒸煮处理对复合材料力学性能的提高幅度最大，常温碱处理次之，而乙酰化处理对复合材料力学性能的影响不明显。进一步的研究表明，两种碱处理和界面改性剂SMA并用对竹粉/ABS复合材料均存在协同效应，能较大幅度的提高复合材料的力学性能，而两种碱处理和ABSm并用以及乙酰化处理和SMA并用则无协同效应。
Wood-plastic composite (WPC) is a new type of environmental material, which ismanufactured from blends of thermoplastics and plant fibers with a special functionalmodified agent and other additives using plastic molding process. The plant fibers includewood flour, bamboo fiber, rice husk and straw. WPC synthesizes the advantages of plant fiberand polymers. It is a low carbon, green, renewable materials with a great developable future.Itcan substitute plenty of wood and efficiently mitigate the status of our country's poor forestresources and demand. It will solve the problems in the recycling of waste plastics and woodresources. In recent years, research and development of WPC have been very popular inliterature, most of which were carried out using PVC, PE, and PP as matrix, but ABS asmatrix is very rare. The preparation of the WPC with ABS matrix has important practicalsignificance for improving its properties and broadening its application area.
The characteristics of five kinds of plant fibers were explored in this thesis firstly. Theywere bamboo fiber (BF), eucalypt fiber, cypress fiber, pine fiber and camphor fiber. Thecontact angle, surface free energy and its components of plant fibers were determined by theWashburn equation with the thin-layer wicking technique. Then the bamboo fiber wasselected for further investigation because of its lower surface free energy. BF/ABS compositeswere prepared by melt compounding. Then the structure and performance of the compositeswere systematically investigated. The modification methods of bamboo fiber that strengthenthe bonding between bamboo fiber and ABS matrix were also studied. Furthermore, ainterfacial modifier was synthesized from ABS. The influence of the interfacial modifier onthe performance of BF/ABS composites was investigated. The interfacial modificationmechanisms were also discussed.
The five kinds of plant fibers all contain a large number of hydroxyl groups, but theirthermal stability is not pretty well. Based on Washburn equation and the thin-layer wickingtechnique, the surface free energies of the plant fibers were calculated. Results demonstratethat eucalypt fiber has the highest surface free energy and non polar part; while bamboo fiberhas the lowest. As combined with the same plastics, the interfacial adhesion between eucalyptfiber and matrix is better than that of the others, so the mechanical properties of eucalyptfiber/ABS composites outperforms the other four.
The poor compatibility between bamboo fiber and ABS matrix limited the performanceof BF/ABS composites. The mechanical properties of BF/ABS composites, including tensilestrength, flexural strength and impact strength, decreased with the increasing bamboo fiber loading, but its flexural modulus increased. The Vicat temperature of BF/ABS compositesincreased with the increasing bamboo fiber loading, suggesting that the incorporation ofbamboo fiber could extend the operating temperature range of composites. Besides, theaddition of bamboo fiber had negative influence on the thermal stability， processingperformance and water absorptivity of BF/ABS composites. As the bamboo particle sizeswere between80and180meshes, the mechanical properties of the samples, besides impactstrength, exhibited a creasing tendency. However, the mechanical properties showed adecreasing tendency when the particle size was40meshes.
Oxazoline modified ABS(ABSm) improved the interactions between bamboo fiber andABS matrix and promoted better mechanical properties of the composites. The tensilestrength and flexural strength of BF/ABS composites were52MPa and91.4MPa whenABSm2was added, about17.6%and35.2%up. The conversion of the nitrile groups intooxazoline of ABSm2is about30%, the optimum dosage was7phr. Among three commerciallyavailable interface modifiers(SMA, PS-g-MAH, EVA-g-MAH), SMA has the best interfacemodified effect, but none of them is better than ABSm.
Alkali treated of bamboo fiber at room temperature and high temperature cooking werestudied. The effects of time and concentration of NaOH on the chemical composition,crystallizing structure, thermal characteristic and surface morphology of bamboo fiber werediscussed. And the optimum processing of alkali treatments at room temperature,concentration of NaOH4%,1h, were obtained. The alkali treatment of the bamboo fiberspromoted the partial removal of the hemicelluloses, extractives, and lignin which present onthe surface of the fiber, and improved its thermal stability. The crystalline structuretransformation of cellulose I into cellulose II was observed by X-ray diffraction for bamboofiber, when NaOH concentration exceeded10%. This would decrease the crystallinity andthermal stability of the bamboo fiber, while the fiber bundles partially break down and appearshrinkage.
The bamboo fibers after acetylation, alkali treated and high temperature alkali cookingwas used to prepare BF/ABS composite. Experiment result showed that different treatmentincreased the dynamic property of the composite by different degree.The two kinds of alkalitreatment had better effect on the BF/ABS composites, while the effect of acetylationtreatment was insignificant. Further studies showed that two kinds of alkali treatment usedtogether with SMA had synergistic effect, while they used together with ABSm andacetylation treatment used together with SMA had no synergistic effect.
引文
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