稻麦秸秆和淀粉制备复合材料研究
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摘要
节能和环保是当今世界的紧迫要求。开发和利用农作物废弃物等可再生且能降解的复合材料已成为当前研究的热点,是环境友好材料研究领域未来的发展方向,也是农作物废弃物利用和抑制环境污染的有效途径之一。秸秆资源丰富,具有低密度性、可再生性及洁净性；淀粉来源广泛、价格便宜,具有可生物降解、可再生等诸多优点。采用农作物秸秆和淀粉制备的复合材料,具有其它复合材料无法比拟的质轻价廉、可再生及可生物降解等优点。秸秆/淀粉复合材料的研究和应用对我国可持续发展具有重要意义。
本研究以稻、麦秸秆和玉米淀粉、木薯淀粉及马铃薯淀粉为主要原料,通过模压成型制备了秸秆/淀粉全降解复合材料,探讨秸秆纤维预处理方法(2%草酸溶液、2%氢氧化钠溶液、水热处理及未处理)、秸秆纤维尺寸、淀粉类型、阻湿剂含量、增塑剂含量及胶粘剂含量对复合材料内结合强度(IB)、弯曲强度(FS)、弯曲弹性模量(MOE)、拉伸强度(TS)、拉伸模量(MOR)、断裂伸长率(EOF)、冲击强度(IS)、2h吸水厚度膨胀率(2hTS)及吸湿率(MA)的影响。分析比较了稻、麦秸秆纤维预处理前后表面化学成分、表面形貌、吸湿性及浸润性能的变化情况。也对比分析了不同配比淀粉胶粘剂表观粘度随温度和剪切速度的变化规律。并观察了复合材料微观结构。取得的主要成果如下：
(1)秸秆拉伸性能测试表明,稻、麦秸秆预处理均能不同程度的降低其拉伸强度,其中氢氧化钠处理后秸秆纤维拉伸强度降幅最大。
(2)红外光谱(IR)和扫描电子显微镜(SEM)分析表明,稻、麦秸秆纤维预处理能不同程度的去除其表面蜡质-硅化层、木质素及半纤维素等化学成分,表面形貌发生较大变化,使细胞壁物质充分暴露,即秸秆纤维表面纤维素、半纤维素以及木质素的特征官能团暴露,红外吸收峰个数增多、峰吸收增强,使秸秆纤维持水力增加,提高其表面润湿性。其中氢氧化钠处理和水热处理效果较为显著,而草酸处理未显著影响秸秆纤维基本组织形态。
(3)秸秆纤维吸湿性能研究表明,稻、麦秸秆纤维吸湿率均随时间的增加而增大,且6h前吸湿率增加较快,10～20mm秸秆段吸湿率在整个吸湿过程中始终较小其吸湿平衡率分别为0.931%和1.071%。粉碎后,稻、麦秸秆纤维吸湿率不同程度的有所增大；其中氢氧化钠处理秸秆纤维吸湿率最大,分别为2.243%和2.411%；水热处理次之,分别为1.84%和1.714%；草酸处理后,分别为1.591%和1.514%；而未处理秸秆纤维吸湿率较小,分别为1.585%和1.449%。通过对秸秆纤维吸湿率数据进行一元非线性回归,得出吸湿率随时间的变化模型,发现所选模型能较好的描述秸秆纤维吸湿率曲线。
(4)秸秆纤维浸润性研究表明,稻、麦秸秆纤维预处理均能不同程度的降低其表面接触角,增强蒸馏水对其表面的浸润性。水热处理、氢氧化钠处理、草酸处理及未处理稻秸秆纤维6min接触角分别为71.5°、61.5°、88.5°和95.5°,麦秸秆纤维6min接触角分别为71.1°、56.5°、74.4°和73.6°。
(5)秸秆纤维热性能研究表明,稻、麦秸秆纤维预处理均能不同程度改变其玻璃化转变温度Tg,并能去除部分硅化物等无机物质。
(6)制备了淀粉与水质量比分别为1/6、1/8和1/10的玉米淀粉、木薯淀粉和马铃薯淀粉胶粘剂,研究分析了其在不同温度和不同剪切速度下表观粘度的变化情况,结果表明：3种淀粉制备的胶粘剂存在剪切稀化现象,即表观粘度随剪切速度的增大而减小,且淀粉与水质量比越小,表观粘度越低。玉米淀粉胶粘剂表观粘度随温度的升高先增大后减小,10℃有最大值。木薯淀粉胶粘剂表观粘度随温度的升高而减小,15℃前变化明显,之后趋于缓和。马铃薯淀粉胶粘剂表观粘度随温度的升高而逐渐减小。通过对不同配比的淀粉胶粘剂流变性能数据进行一元非线性回归,得出淀粉胶粘剂在不同温度下的流变模型,发现所选模型能较好的描述淀粉胶粘剂流变性能。此外,在相同条件下,3种淀粉胶粘剂表观粘度大小顺序为：马铃薯淀粉>玉米淀粉>木薯淀粉。
(7)通过正交试验方法L9(34),以弯曲强度和弯曲弹性模量为优化参数,得出制备复合材料最佳模压工艺参数为：压力4MPa、温度120℃、时间30min。
(8)在最佳工艺参数条件下,制备了不同尺寸秸秆纤维及不同淀粉复合材料：复合材料力学性能基本随秸秆纤维尺寸的减小而先增大后减小,且各项性能随秸秆纤维尺寸的变化有所不同,0.2～0.45mm时,IB较好；0.45～0.9mm时,FS、MOE、TS较好；0.9～30mm时,MOR、EOF和IS较好；<0.2mm时,力学性能较差；混合纤维时,各项力学性能也较好；10～20mm秸秆段时,仅有IS较好。2hTS和MA随秸秆纤维尺寸的减小先减小后增大,0.9～30mm时,2hTS较大；0.2～0.45mm时,2hTS较小；10～20mm秸秆段制备的复合材料在浸水0.5h左右结构变的松散,甚至分解。玉米淀粉基复合材料IB、MOE、MOR及IS较好,EOF较小；木薯淀粉基复合材料FS和TS较好；马铃薯淀粉复合材料性能较差；淀粉类型对2hTS和MA影响甚微。
(9)水热处理稻、麦秸秆纤维复合材料FS、MOE、IS、TS、MOR较高,IB较低；氢氧化钠处理时,IB较高,FS较低；草酸处理时,IB、FS、MOE、IS均有不同程度的降低。氢氧化钠处理秸秆纤维复合材料2hTS较小,而秸秆纤维预处理不同程度的降低复合材料防湿性能,MA增大。
(10)阻湿剂的加入导致稻、麦秸秆纤维复合材料各项力学性能降低,IB、FS、MOE、TS、MOR、EOF及IS最大降幅分别为：56.25%、6.68%、11.31%、40.17%、54.74%、20.4%和26.46%(稻秸秆纤维复合材料),以及36.1%、56.2%、68.5%、56.5%、58.1%、20.3%和27.4%(麦秸秆纤维复合材料)。适量阻湿剂(1%)能提高复合材料防水防湿性能。
(11)增塑剂的加入导致稻、麦秸秆纤维复合材料MOR和EOF略微降低,而其它力学性能均有不同程度的提高,同时复合材料防水防湿性能也提高。
(12)稻秸秆纤维复合材料力学性能随淀粉胶粘剂含量的增大均先增大后减小；淀粉胶粘剂含量为10%时,IB、FS、MOE、TS、IS均达最大值,淀粉胶粘剂含量9%时,EOR和EOF达最大值；麦秸秆纤维复合材料IB在淀粉胶粘剂含量为9%时有最大值,EOF和IS在10%时有最大值,而其它力学性能均随淀粉胶胶剂含量的增加而降低。稻、麦秸秆纤维复合材料2hTS随淀粉胶粘剂含量的增加而略有减小,吸湿率变化不明显。
(13)复合材料微观结构分析表明：基体和增强体两相界面结合存在明显缝隙、空洞现象,且随秸秆纤维尺寸的增大而变大,其中<0.2mm时,复合材料表面出现较多裂纹。
综上所述,秸秆纤维预处理能不同程度的去除稻、麦秸秆纤维表面有机硅-蜡质层,使细胞壁物质充分暴露,且降低秸秆粗纤维、半纤维素和木质素含量,秸秆纤维持水力增加,提高了其吸湿性能,同时降低其表面接触角,使秸秆纤维表面易被浸润,为淀粉胶粘剂和秸秆纤维的结合提供良好界面。复合材料性能随多个影响因素相互“竞争”的结果不同而有所差异。在相同条件下,不同淀粉胶粘剂表观粘度差异较大,但其制备的复合材料相关性能并未表现相似差异。秸秆纤维尺寸、预处理、阻湿剂含量、增塑剂含量及胶粘剂含量均对复合材料各项性能的影响差异较大。
Energy saving and environmental protection are the world's urgent requirements. Development and utilization of agricultural waste and other renewable and degradable composites materials have become a research focus, which is environmental-friendly materials' research direction for future development, and also an effective way of using crop waste and reducing environmental pollution. Straw and starch are both rich in resources, and their composites represented low density, light weight, low cost, renewable nature, and acceptable biodegradability, which other composites can not match. Research and applications of straw/starch composites have important significance for sustainable development, not only to ease the conflict of timber supply and demand, but also to prosper rural economy and increase farmers' income.
The main goal of this work was to use rice, wheat straw and corn starch, tapioca starch and potato starch as the main raw material to prepare environmentally sound, biodegradable composites using starch-based adhesives by a compression molding process. Effects of straw fiber pretreatments, straw fiber sizes, starch type, moisture resistance agent content, plasticizer content, and adhesive content on internal bond strength (IB), flexural strength (FS), modulus of elasticity (MOE), tensile strength (TS), modulus of rupture (MOR), elongation of fracture (EOF), impact strength (IS),2h thickness swelling (2hTS) and the moisture absorption rate (MA) of the obtained composites were investigated. Analysis and comparison of rice, wheat straw fiber morphology and properties were undertaken before and after pretreatments. The influence of temperature and shear rate variation on apparent viscosity of starch adhesive of different combinations had been also investigated. The main results obtained as follows:
(1) Testing for tensile properties indicated that:pretreatments reduced the tensile strength of rice, wheat straw, and the biggest down-range appeared after NaOH treatment.
(2) Infrared spectroscopy (IR) and scanning electron microscopy (SEM) suggested that:all pretreatments were efficient in partially changing RS surface properties, by removing wax-silicide layer on rice, wheat straw fibre surface in different levels, fully exposing the cell wall materials, as well as exposing functional groups of cellulose, hemicellulose, and lignin on the surface of straw, increasing the number of infrared absorption peak, enhancing the peak absorption, increasing water-holding capacity, improving the surface wettability. Among them, effects of NaOH treatment and hot-water treatment were more significant, while the oxalic acid treatment did not affect the basic organizational form of straw fibre significantly.
(3) Moisture absorption of straw fiber showed that:moisture absorption rate increased with time increasing, and increased rapidly within6h. Moisture absorption rate of10-20mm straw section was smaller in the whole process, and their moisture equilibrium rates were0.9314%and1.071%. After crushing, rice, wheat straw fibers' moisture absorption rate increased in different levels; after NaOH treatment, moisture absorption rate was largest, where2.243%and2.411%, respectively; hot-water treatment followed, where1.84%and1.714%, respectively; after oxalic acid treatment, where1.591%and1.514%, respectively; moisture absorption rate of untreated straw fiber was smaller, where1.585%and1.449%, respectively.
(4) Wettability of straw fiber was also investigated and showed that:pretreatments of rice, wheat straw fiber lowered surface contact angle and enhanced wettability of distilled water on the straw surface. Hot-water treatment, NaOH treatment, oxalic acid treatment and untreated rice straw fibers' contact angle at6min were71.5°,61.5°,88.5°and95.5°, and wheat straw fibers'were71.1°,56.5°,74.4°, and73.6°, respectively.
(5) Differential scanning calorimetry (DSC) suggested that:pretreatments changed the glass transition temperature (Tg) of rice, wheat straw fiber, and decreased the contents of inorganic matter such as silicide.
(6) Corn starch, tapioca starch and potato starch adhesives of starch to water mass ratio1/6,1/8and1/10were prepared. The influence of temperature and shear rate (decided by rotor speed) on apparent viscosity of starch adhesives was also investigated. Three starch adhesives showed a shear thinning phenomenon. Apparent viscosity decreased with starch/water mass ratio decreasing. The apparent viscosity of corn starch adhesive increased and then decreased with temperature increasing, and reached peak value at10℃. Apparent viscosity of cassava starch adhesive decreased with temperature increasing, changing significantly before15℃, and then easing. Apparent viscosity of potato starch adhesive decreased with temperature increasing.
(7) The optimum molding process parameters of composites were pressure of4MPa, temperature of120℃, and pressure-holding time of30min, which were obtained by orthogonal test method L9(34) and flexural strength and flexural modulus as optimization parameters.
(8) Based on the optimum molding process parameters, composites of different sizes straw fibers and different starch were prepared:(a), each property of composites changed differently with different dimensions, at0.2-0.45mm, IB was better; at0.45-0.9mm, FS, MOE were better; at0.9～30mm, TS, MOR, EOF and IS were better; at mixing straw fibres, the mechanical properties picked-up in different levels; at10-20mm section, only IS was better.2hTS and MA decreased and then increased with straw fiber size decreasing, at0.9～30mm,2hTS was bigger; at0.2～0.45mm,2hTS was smaller; composites from10～20mm section straw fibres dissolved in about0.5h.(b), IB, MOE, MOR and IS of corn starch-based composites were better, and EOF was smaller. FS and TS of cassava starch-based composites were better. Potato starch-based composites showed poor mechanical properties. The effect of starch types on2hTS and MA was slight.
(9) FS, MOE, IS, TS, and MOR of composites from hot-water treatment straw fibers were higher, IB was lower; after NaOH treatment, IB was higher, FS was lower; after oxalic acid treatment, IB, FS, MOE, IS decreased in different levels. After NaOH treatment,2hTS was smaller. Pretreatments of straw fibers decreased moisture resistance properties of composites, and MA increased.
(10) The introduction of moisture resistance agent reduced the mechanical properties in different levels, the maximum drops of IB, FS, MOE, TS, MOR, EOF, and IS were as follows:56.25%,6.68%,11.31%,40.17%,54.74%,20.4%and26.46%(rice straw fibers composites), and36.1%,56.2%,68.5%,56.5%,58.1%,20.3%and27.4%(wheat straw fibers composites).1%moisture resistance agent improved the performance of composites' waterproof and moisture resistance.
(11) The introduction of plasticizer reduced MOR and EOF slightly, but enhanced the other mechanical properties in different levels, while improved the performance of composites' waterproof and moisture resistance.
(12) The mechanical properties of rice straw fibers composites increased and then decreased with starch adhesive content increasing; IB, FS, MOE, TS, and IS reached peak value at10%adhesives content; IB and IS of wheat straw fibers composites reached peak value at9%adhesives content, while the other mechanical properties decreased with adhesives content increasing in different levels.2hTS reduced with starch adhesive content increasing slightly. The effect of adhesives content on MA was slight.
(13) Microstructure of composites was also studied:all composites surfaces were smooth, but there are apertures, and gaps obviously in interface of matrix and reinforcement, which facilitated water or moisture to infiltrate inside of the composites. This also could explain why the moisture resistance was poor. The apertures and gaps become larger with the straw fibers size increasing. Otherwise, there were many cracks at<0.2mm.
In summary, pretreatments of straw fibers changed surface properties or removed silicone-waxy layer partly, exposed the cell wall material, reduced cellulose, hemicellulose, and lignin content, increased water-holding capacity, improved surface wettability and moisture absorption, and reduced the surface contact angle, which provided a better combination interface of straw fiber and starch adhesives. Composites' properties were decided by "competitive results" among the multiple factors. Under the same conditions, the apparent viscosity of different starch adhesives was quite different, but the relevant composites did not show similar performance as adhesives did. Straw fiber sizes, pretreatments and moisture resistance agents, plasticizers, adhesives content showed greater impact on performance of composites.
本研究以稻、麦秸秆和玉米淀粉、木薯淀粉及马铃薯淀粉为主要原料,通过模压成型制备了秸秆/淀粉全降解复合材料,探讨秸秆纤维预处理方法(2%草酸溶液、2%氢氧化钠溶液、水热处理及未处理)、秸秆纤维尺寸、淀粉类型、阻湿剂含量、增塑剂含量及胶粘剂含量对复合材料内结合强度(IB)、弯曲强度(FS)、弯曲弹性模量(MOE)、拉伸强度(TS)、拉伸模量(MOR)、断裂伸长率(EOF)、冲击强度(IS)、2h吸水厚度膨胀率(2hTS)及吸湿率(MA)的影响。分析比较了稻、麦秸秆纤维预处理前后表面化学成分、表面形貌、吸湿性及浸润性能的变化情况。也对比分析了不同配比淀粉胶粘剂表观粘度随温度和剪切速度的变化规律。并观察了复合材料微观结构。取得的主要成果如下：
(1)秸秆拉伸性能测试表明,稻、麦秸秆预处理均能不同程度的降低其拉伸强度,其中氢氧化钠处理后秸秆纤维拉伸强度降幅最大。
(2)红外光谱(IR)和扫描电子显微镜(SEM)分析表明,稻、麦秸秆纤维预处理能不同程度的去除其表面蜡质-硅化层、木质素及半纤维素等化学成分,表面形貌发生较大变化,使细胞壁物质充分暴露,即秸秆纤维表面纤维素、半纤维素以及木质素的特征官能团暴露,红外吸收峰个数增多、峰吸收增强,使秸秆纤维持水力增加,提高其表面润湿性。其中氢氧化钠处理和水热处理效果较为显著,而草酸处理未显著影响秸秆纤维基本组织形态。
(3)秸秆纤维吸湿性能研究表明,稻、麦秸秆纤维吸湿率均随时间的增加而增大,且6h前吸湿率增加较快,10～20mm秸秆段吸湿率在整个吸湿过程中始终较小其吸湿平衡率分别为0.931%和1.071%。粉碎后,稻、麦秸秆纤维吸湿率不同程度的有所增大；其中氢氧化钠处理秸秆纤维吸湿率最大,分别为2.243%和2.411%；水热处理次之,分别为1.84%和1.714%；草酸处理后,分别为1.591%和1.514%；而未处理秸秆纤维吸湿率较小,分别为1.585%和1.449%。通过对秸秆纤维吸湿率数据进行一元非线性回归,得出吸湿率随时间的变化模型,发现所选模型能较好的描述秸秆纤维吸湿率曲线。
(4)秸秆纤维浸润性研究表明,稻、麦秸秆纤维预处理均能不同程度的降低其表面接触角,增强蒸馏水对其表面的浸润性。水热处理、氢氧化钠处理、草酸处理及未处理稻秸秆纤维6min接触角分别为71.5°、61.5°、88.5°和95.5°,麦秸秆纤维6min接触角分别为71.1°、56.5°、74.4°和73.6°。
(5)秸秆纤维热性能研究表明,稻、麦秸秆纤维预处理均能不同程度改变其玻璃化转变温度Tg,并能去除部分硅化物等无机物质。
(6)制备了淀粉与水质量比分别为1/6、1/8和1/10的玉米淀粉、木薯淀粉和马铃薯淀粉胶粘剂,研究分析了其在不同温度和不同剪切速度下表观粘度的变化情况,结果表明：3种淀粉制备的胶粘剂存在剪切稀化现象,即表观粘度随剪切速度的增大而减小,且淀粉与水质量比越小,表观粘度越低。玉米淀粉胶粘剂表观粘度随温度的升高先增大后减小,10℃有最大值。木薯淀粉胶粘剂表观粘度随温度的升高而减小,15℃前变化明显,之后趋于缓和。马铃薯淀粉胶粘剂表观粘度随温度的升高而逐渐减小。通过对不同配比的淀粉胶粘剂流变性能数据进行一元非线性回归,得出淀粉胶粘剂在不同温度下的流变模型,发现所选模型能较好的描述淀粉胶粘剂流变性能。此外,在相同条件下,3种淀粉胶粘剂表观粘度大小顺序为：马铃薯淀粉>玉米淀粉>木薯淀粉。
(7)通过正交试验方法L9(34),以弯曲强度和弯曲弹性模量为优化参数,得出制备复合材料最佳模压工艺参数为：压力4MPa、温度120℃、时间30min。
(8)在最佳工艺参数条件下,制备了不同尺寸秸秆纤维及不同淀粉复合材料：复合材料力学性能基本随秸秆纤维尺寸的减小而先增大后减小,且各项性能随秸秆纤维尺寸的变化有所不同,0.2～0.45mm时,IB较好；0.45～0.9mm时,FS、MOE、TS较好；0.9～30mm时,MOR、EOF和IS较好；<0.2mm时,力学性能较差；混合纤维时,各项力学性能也较好；10～20mm秸秆段时,仅有IS较好。2hTS和MA随秸秆纤维尺寸的减小先减小后增大,0.9～30mm时,2hTS较大；0.2～0.45mm时,2hTS较小；10～20mm秸秆段制备的复合材料在浸水0.5h左右结构变的松散,甚至分解。玉米淀粉基复合材料IB、MOE、MOR及IS较好,EOF较小；木薯淀粉基复合材料FS和TS较好；马铃薯淀粉复合材料性能较差；淀粉类型对2hTS和MA影响甚微。
(9)水热处理稻、麦秸秆纤维复合材料FS、MOE、IS、TS、MOR较高,IB较低；氢氧化钠处理时,IB较高,FS较低；草酸处理时,IB、FS、MOE、IS均有不同程度的降低。氢氧化钠处理秸秆纤维复合材料2hTS较小,而秸秆纤维预处理不同程度的降低复合材料防湿性能,MA增大。
(10)阻湿剂的加入导致稻、麦秸秆纤维复合材料各项力学性能降低,IB、FS、MOE、TS、MOR、EOF及IS最大降幅分别为：56.25%、6.68%、11.31%、40.17%、54.74%、20.4%和26.46%(稻秸秆纤维复合材料),以及36.1%、56.2%、68.5%、56.5%、58.1%、20.3%和27.4%(麦秸秆纤维复合材料)。适量阻湿剂(1%)能提高复合材料防水防湿性能。
(11)增塑剂的加入导致稻、麦秸秆纤维复合材料MOR和EOF略微降低,而其它力学性能均有不同程度的提高,同时复合材料防水防湿性能也提高。
(12)稻秸秆纤维复合材料力学性能随淀粉胶粘剂含量的增大均先增大后减小；淀粉胶粘剂含量为10%时,IB、FS、MOE、TS、IS均达最大值,淀粉胶粘剂含量9%时,EOR和EOF达最大值；麦秸秆纤维复合材料IB在淀粉胶粘剂含量为9%时有最大值,EOF和IS在10%时有最大值,而其它力学性能均随淀粉胶胶剂含量的增加而降低。稻、麦秸秆纤维复合材料2hTS随淀粉胶粘剂含量的增加而略有减小,吸湿率变化不明显。
(13)复合材料微观结构分析表明：基体和增强体两相界面结合存在明显缝隙、空洞现象,且随秸秆纤维尺寸的增大而变大,其中<0.2mm时,复合材料表面出现较多裂纹。
综上所述,秸秆纤维预处理能不同程度的去除稻、麦秸秆纤维表面有机硅-蜡质层,使细胞壁物质充分暴露,且降低秸秆粗纤维、半纤维素和木质素含量,秸秆纤维持水力增加,提高了其吸湿性能,同时降低其表面接触角,使秸秆纤维表面易被浸润,为淀粉胶粘剂和秸秆纤维的结合提供良好界面。复合材料性能随多个影响因素相互“竞争”的结果不同而有所差异。在相同条件下,不同淀粉胶粘剂表观粘度差异较大,但其制备的复合材料相关性能并未表现相似差异。秸秆纤维尺寸、预处理、阻湿剂含量、增塑剂含量及胶粘剂含量均对复合材料各项性能的影响差异较大。
Energy saving and environmental protection are the world's urgent requirements. Development and utilization of agricultural waste and other renewable and degradable composites materials have become a research focus, which is environmental-friendly materials' research direction for future development, and also an effective way of using crop waste and reducing environmental pollution. Straw and starch are both rich in resources, and their composites represented low density, light weight, low cost, renewable nature, and acceptable biodegradability, which other composites can not match. Research and applications of straw/starch composites have important significance for sustainable development, not only to ease the conflict of timber supply and demand, but also to prosper rural economy and increase farmers' income.
The main goal of this work was to use rice, wheat straw and corn starch, tapioca starch and potato starch as the main raw material to prepare environmentally sound, biodegradable composites using starch-based adhesives by a compression molding process. Effects of straw fiber pretreatments, straw fiber sizes, starch type, moisture resistance agent content, plasticizer content, and adhesive content on internal bond strength (IB), flexural strength (FS), modulus of elasticity (MOE), tensile strength (TS), modulus of rupture (MOR), elongation of fracture (EOF), impact strength (IS),2h thickness swelling (2hTS) and the moisture absorption rate (MA) of the obtained composites were investigated. Analysis and comparison of rice, wheat straw fiber morphology and properties were undertaken before and after pretreatments. The influence of temperature and shear rate variation on apparent viscosity of starch adhesive of different combinations had been also investigated. The main results obtained as follows:
(1) Testing for tensile properties indicated that:pretreatments reduced the tensile strength of rice, wheat straw, and the biggest down-range appeared after NaOH treatment.
(2) Infrared spectroscopy (IR) and scanning electron microscopy (SEM) suggested that:all pretreatments were efficient in partially changing RS surface properties, by removing wax-silicide layer on rice, wheat straw fibre surface in different levels, fully exposing the cell wall materials, as well as exposing functional groups of cellulose, hemicellulose, and lignin on the surface of straw, increasing the number of infrared absorption peak, enhancing the peak absorption, increasing water-holding capacity, improving the surface wettability. Among them, effects of NaOH treatment and hot-water treatment were more significant, while the oxalic acid treatment did not affect the basic organizational form of straw fibre significantly.
(3) Moisture absorption of straw fiber showed that:moisture absorption rate increased with time increasing, and increased rapidly within6h. Moisture absorption rate of10-20mm straw section was smaller in the whole process, and their moisture equilibrium rates were0.9314%and1.071%. After crushing, rice, wheat straw fibers' moisture absorption rate increased in different levels; after NaOH treatment, moisture absorption rate was largest, where2.243%and2.411%, respectively; hot-water treatment followed, where1.84%and1.714%, respectively; after oxalic acid treatment, where1.591%and1.514%, respectively; moisture absorption rate of untreated straw fiber was smaller, where1.585%and1.449%, respectively.
(4) Wettability of straw fiber was also investigated and showed that:pretreatments of rice, wheat straw fiber lowered surface contact angle and enhanced wettability of distilled water on the straw surface. Hot-water treatment, NaOH treatment, oxalic acid treatment and untreated rice straw fibers' contact angle at6min were71.5°,61.5°,88.5°and95.5°, and wheat straw fibers'were71.1°,56.5°,74.4°, and73.6°, respectively.
(5) Differential scanning calorimetry (DSC) suggested that:pretreatments changed the glass transition temperature (Tg) of rice, wheat straw fiber, and decreased the contents of inorganic matter such as silicide.
(6) Corn starch, tapioca starch and potato starch adhesives of starch to water mass ratio1/6,1/8and1/10were prepared. The influence of temperature and shear rate (decided by rotor speed) on apparent viscosity of starch adhesives was also investigated. Three starch adhesives showed a shear thinning phenomenon. Apparent viscosity decreased with starch/water mass ratio decreasing. The apparent viscosity of corn starch adhesive increased and then decreased with temperature increasing, and reached peak value at10℃. Apparent viscosity of cassava starch adhesive decreased with temperature increasing, changing significantly before15℃, and then easing. Apparent viscosity of potato starch adhesive decreased with temperature increasing.
(7) The optimum molding process parameters of composites were pressure of4MPa, temperature of120℃, and pressure-holding time of30min, which were obtained by orthogonal test method L9(34) and flexural strength and flexural modulus as optimization parameters.
(8) Based on the optimum molding process parameters, composites of different sizes straw fibers and different starch were prepared:(a), each property of composites changed differently with different dimensions, at0.2-0.45mm, IB was better; at0.45-0.9mm, FS, MOE were better; at0.9～30mm, TS, MOR, EOF and IS were better; at mixing straw fibres, the mechanical properties picked-up in different levels; at10-20mm section, only IS was better.2hTS and MA decreased and then increased with straw fiber size decreasing, at0.9～30mm,2hTS was bigger; at0.2～0.45mm,2hTS was smaller; composites from10～20mm section straw fibres dissolved in about0.5h.(b), IB, MOE, MOR and IS of corn starch-based composites were better, and EOF was smaller. FS and TS of cassava starch-based composites were better. Potato starch-based composites showed poor mechanical properties. The effect of starch types on2hTS and MA was slight.
(9) FS, MOE, IS, TS, and MOR of composites from hot-water treatment straw fibers were higher, IB was lower; after NaOH treatment, IB was higher, FS was lower; after oxalic acid treatment, IB, FS, MOE, IS decreased in different levels. After NaOH treatment,2hTS was smaller. Pretreatments of straw fibers decreased moisture resistance properties of composites, and MA increased.
(10) The introduction of moisture resistance agent reduced the mechanical properties in different levels, the maximum drops of IB, FS, MOE, TS, MOR, EOF, and IS were as follows:56.25%,6.68%,11.31%,40.17%,54.74%,20.4%and26.46%(rice straw fibers composites), and36.1%,56.2%,68.5%,56.5%,58.1%,20.3%and27.4%(wheat straw fibers composites).1%moisture resistance agent improved the performance of composites' waterproof and moisture resistance.
(11) The introduction of plasticizer reduced MOR and EOF slightly, but enhanced the other mechanical properties in different levels, while improved the performance of composites' waterproof and moisture resistance.
(12) The mechanical properties of rice straw fibers composites increased and then decreased with starch adhesive content increasing; IB, FS, MOE, TS, and IS reached peak value at10%adhesives content; IB and IS of wheat straw fibers composites reached peak value at9%adhesives content, while the other mechanical properties decreased with adhesives content increasing in different levels.2hTS reduced with starch adhesive content increasing slightly. The effect of adhesives content on MA was slight.
(13) Microstructure of composites was also studied:all composites surfaces were smooth, but there are apertures, and gaps obviously in interface of matrix and reinforcement, which facilitated water or moisture to infiltrate inside of the composites. This also could explain why the moisture resistance was poor. The apertures and gaps become larger with the straw fibers size increasing. Otherwise, there were many cracks at<0.2mm.
In summary, pretreatments of straw fibers changed surface properties or removed silicone-waxy layer partly, exposed the cell wall material, reduced cellulose, hemicellulose, and lignin content, increased water-holding capacity, improved surface wettability and moisture absorption, and reduced the surface contact angle, which provided a better combination interface of straw fiber and starch adhesives. Composites' properties were decided by "competitive results" among the multiple factors. Under the same conditions, the apparent viscosity of different starch adhesives was quite different, but the relevant composites did not show similar performance as adhesives did. Straw fiber sizes, pretreatments and moisture resistance agents, plasticizers, adhesives content showed greater impact on performance of composites.
引文
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