SiO_2@Fe_3O_4磁性纳米复合材料的制备及其对亚甲基蓝吸附性能研究

利用正硅酸四乙酯作为SiO_2的前驱体,制备了SiO_2包覆铁氧体(SiO_2@Fe_3O_4)磁性纳米复合材料。通过FT-IR、TEM、BET等表征方法,研究了不同搅拌速率、(TEOS)g/(MNPs)g、氨量及水解温度制备的SiO_2@Fe_3O_4磁性纳米复合材料对废水中亚甲基蓝吸附性能的影响。结果表明,在搅拌速率为400 r/min,(TEOS)g/(MNPs)g为2.4,氨量为2.5mL,水解反应温度为40℃时,所制备的SiO_2@Fe_3O_4磁性纳米复合材料对亚甲基蓝的吸附性能最佳。磁选和再生性能研究表明,所制备的SiO_2@Fe_3O_4磁性纳米复合材料孔径大小合适、分布均匀,其磁选性能满足日常需要,且具有良好的再生性能和优异的亚甲基蓝吸附性能。     

Fe3O4/SiO2/PS的制备及对有机染料分子的吸附性能

采用乳液聚合法在Fe_3O_4@SiO_2纳米粒子表面引发苯乙烯单体聚合,制备了聚苯乙烯修饰的Fe_3O_4@SiO_2磁性复合微球(Fe_3O_4@SiO_2@PS),研究了其对甲基橙(MO)和亚甲基蓝(MB)的吸附性能。用透射电镜和扫描电镜对所制得样品进行了形貌表征。结果表明,复合材料中的Fe_3O_4粒径分布在150～220 nm范围内,粒径分布较均匀、分散性良好;用振动样品磁强计对样品的磁性能进行表征,Fe_3O_4@SiO_2@PS复合粒子具有超顺磁性和较好的磁响应性;采用X射线衍射仪、傅里叶变换红外光谱仪、热重分析仪分析了复合粒子的结构和组成,用紫外-可见分光光度计测定有机染料分子的浓度,从而计算吸附量。Fe_3O_4@SiO_2@PS复合粒子对甲基橙和亚甲基蓝具有良好的吸附性能,在2 h达到吸附平衡,MO和MB单位平衡吸附量分别为94.5 mg/g、167.8 mg/g;该磁性吸附剂吸附染料分子后,可以用乙醇进行解吸附,在保持原始最大吸附量的81%下,可重复使用4次。     

纤维素基磁性吸附剂的制备及其吸附金属离子性能

为提高纤维素基吸附剂性能,使纳米纤维素(NCC)与乙二胺(EDA)反应制得NCC-EDA后,链接原位生成的Fe_3O_4制备了磁性吸附剂NCC-EDA/Fe_3O_4,并在结构表征的同时,考察了体系pH值、吸附时间、溶液浓度、吸附温度等对产物吸附金属离子性能的影响。结果表明,NCC-EDA/Fe_3O_4具有较大比表面积和孔隙,丰富的活性官能团及顺磁性能;最佳条件下对Pb~(2+)、Ni~(2+)及Cr~(6+)的最大吸附量为352.10,265.96和291.55mg/g;吸附过程为单分子层吸附,吸附行为符合拟二级动力学方程及Langmuir吸附等温线,具有吸附速率高及重复使用性能优等特点。     

PEI功能化的磁性四氧化三铁纳米粒子高效吸附水中刚果红

通过水热法制备了枝状聚乙烯亚胺(PEI)修饰的Fe_3O_4纳米粒子,并借助傅立叶转换红外光谱(FT-IR)、X射线衍射(XRD)、扫描电子显示镜(SEM)和透射电子显示镜(TEM)对该材料进行表征,同时考察了PEI-Fe_3O_4纳米粒子对水中刚果红的吸附性能。结果表明,PEI-Fe_3O_4纳米粒子对刚果红的吸附符合准二级动力学方程和Langmuir吸附等温模型,红外光谱分析表明刚果红吸附的主要方式是化学吸附。PEI-Fe_3O_4纳米粒子对刚果红的最大吸附容量为85.47mg/g,优于文献报道的其他磁性吸附材料,可望作为一种优良的吸附剂去除染料废水中刚果红。     

氨基化修饰介孔Fe_3O_4@SiO_2@mSiO_2磁性吸附剂的制备及吸附性能的研究

以Fe_3O_4为磁核,中间包覆一层SiO_2,再以十六烷基三甲基溴化铵(CTAB)为模板剂形成介孔二氧化硅,并以3-氨丙基三乙氧基硅烷(APTES)为表面官能团化基团,对介孔磁性材料表面进行氨基官能团化。通过XRD、TEM、FT-IR对磁性纳米粒子及核壳式磁性纳米复合粒子进行了表征分析。研究了氨基功能化介孔磁性纳米粒子对水中Cu(Ⅱ)的吸附性能。考察了接触时间、溶液的pH值、初始浓度、吸附剂用量对吸附效果的影响,并对其吸附动力学和吸附等温线进行了研究。同时考察了负载了重金属离子的吸附材料用酸溶液超声处理后循环使用的吸附效率。结果表明,二级动力学模型比一级动力学模型更适合于描述吸附剂对Cu(Ⅱ)的吸附动力学行为,说明吸附过程为化学吸附;其对Cu(Ⅱ)的吸附可用Langmuir吸附等温模型进行较好地描述,说明吸附为单分子层吸附,其对Cu(Ⅱ)的最大吸附量为120 mg/g;最大吸附发生在pH值为5.0,t=120 min时。且吸附剂解吸再生4次后,吸附率还能达到68.75%,说明所制备的氨基功能化磁性纳米材料具有较高的吸附容量,是一种潜在的能高效吸附、可再生利用的去除废水中重金属离子的吸附材料。     

Fe3O4@SiO2核壳磁性纳米材料的制备及其对Cu(Ⅱ)的吸附研究

首先通过溶剂热法制备了磁性Fe_3O_4纳米粒子,随后采用SiO_2对其进行包覆形成了Fe_3O_4@SiO_2核壳磁性纳米材料。通过XRD、SEM、TEM、磁性能分析和吸附性能分析等对Fe_3O_4@SiO_2核壳磁性纳米材料进行了表征。结果表明,合成的Fe_3O_4@SiO_2核壳磁性纳米材料具有Fe_3O_4和SiO_2两种晶型结构,SiO_2成功包覆在磁性Fe_3O_4纳米粒子上,SiO_2并没有对各组织的结构和成分产生较大影响;Fe_3O_4@SiO_2核壳磁性纳米材料的粒径在200～400 nm左右,且呈核壳式的结构,内层Fe_3O_4纳米粒子的颜色较深,外层SiO_2的颜色较浅;Fe_3O_4@SiO_2核壳磁性纳米材料在室温下的饱和磁化强度为76.31 A·m~2/kg,剩余磁化强度几乎为0;Fe_3O_4@SiO_2核壳磁性纳米材料对Cu(Ⅱ)的吸附在1 500 min时达到饱和,去除率最高为63%,最大吸附容量可达120 mg/g,其对Cu(Ⅱ)具有较好的吸附效果。     

赖氨酸修饰磁性Fe3O4纳米粒子的制备及其对Cu（Ⅱ）的吸附性能

采用化学共沉淀法制备磁性Fe3O4纳米粒子,通过在磁性Fe3O4纳米粒子表面接枝赖氨酸,制备一种新型磁性纳米吸附剂。通过TEM、FT-IR、XRD、VSM对其进行表征,着重研究了其对Cu(Ⅱ)离子的吸附性能。结果表明,溶液pH值能显著影响吸附剂对Cu(Ⅱ)的吸附效果,pH为5时其效果最佳。等温吸附数据符合Langmuir模型,T=298K、pH=5、V=5mL时,吸附剂的饱和吸附容量qm=22.42mg/g,吸附常数为0.0346L/mg。     

煅烧工艺对α-Fe_2O_3磁性纳米纤维形貌及性能的影响研究

结合静电纺丝和水热合成技术制备PVA/Fe_3O_4磁性纳米纤维,空气气氛中在不同煅烧温度下制备出一系列α-Fe_2O_3纳米纤维。采用扫描电子显微镜(SEM),X射线衍射仪和超导量子干涉仪对不同煅烧温度下制得的α-Fe_2O_3磁性纳米纤维进行形貌与性能表征。结果表明,PVA/Fe_3O_4复合磁性纳米纤维在600~800℃的煅烧温度区间内可获得稳定的α-Fe_2O_3磁性纳米纤维,纤维形貌从中空管状结构逐渐转变为沟槽状结构,纤维中的α-Fe_2O_3粒子具有不同的晶粒尺寸,结晶随温度升高而变好,且具有不同的磁性能。制备的α-Fe_2O_3磁性纳米纤维在水处理等方面具有潜在应用。     

端氨基超支聚合物功能化磁性复合材料对Cu~(2+)和甲基橙的吸附研究

合成端氨基超支聚合物(HBPA)后与"一锅法"合成的氨基修饰磁性纳米微球通过戊二醛交联得到多氨基功能化磁性纳米吸附剂。通过傅里叶红外光谱、XRD光谱和热重分析表明端氨基修饰磁性纳米吸附剂(Fe_3O_4@HBPA)成功制备。探讨了Fe_3O_4@HBPA吸附剂对模拟废水中Cu~(2+)和甲基橙的吸附性能。Fe_3O_4@HBPA对Cu~(2+)和甲基橙的吸附时间为120min,温度30℃,吸附剂用量为10.0mg,pH=5.0时对Cu~(2+)的吸附效果最佳,pH大于5,对甲基橙吸附效果都较佳。Fe_3O_4@HBPA吸附剂对Cu~(2+)和甲基橙吸附速率较快,在10min左右就基本达到吸附平衡,温度对Cu~(2+)和甲基橙的吸附影响不大。结果表明端氨基超支聚合物修饰的磁性纳米吸附剂对Cu~(2+)和甲基橙具有较好的吸附能力。     

3D石墨烯增效的磁性功能材料的制备及其吸附性能研究

用共沉淀法制备Fe_3O_4纳米粒子,将3D石墨烯包裹在Fe_3O_4纳米粒子表面,先后分别用正硅酸乙酯(TEOS)和乙烯基三甲氧基硅烷(VTMO)对其表面进行乙烯基硅烷化改性,最后通过"巯基-烯"点击化学将功能单体3-巯基-1-丙磺酸钠(MPS)聚合在粒子表面制备了一种磁性功能材料Fe_3O_4@3DG@VTMO@MPS。分别采用扫描电镜(SEM)、能谱分析(EDS)、粒径分析(DLS)、红外光谱(FT-IR)及热重分析(TGA)对功能材料的结构、形貌及热稳定性等进行表征,再通过静态吸附实验研究了此功能材料对溶菌酶的吸附性能。结果表明,制备的磁性功能材料具有较高的吸附性能(最大吸附量达162.1 mg/g)和较快的吸附动力学(150 min可达吸附平衡)。拟二级动力学模型适用于描述功能材料对溶菌酶的吸附动力学行为,且功能材料对溶菌酶的吸附过程更符合Langmuir吸附模型,表明功能材料对溶菌酶的吸附为单分子层吸附。以Fe_3O_4@3DG@VTMO@MPS作为固相萃取材料,分离富集蜂蜜中的溶菌酶,并结合高效液相色谱对实际样品进行检测。     

Enhanced removal of Cr(VI) from aqueous solution using polypyrrole/Fe3O4 magnetic nanocomposite

Fe(3)O(4) coated polypyrrole (PPy) magnetic nanocomposite was prepared via in situ polymerization of pyrrole monomer for the removal of highly toxic Cr(VI). Structure and morphology of the prepared nanocomposite were characterized by attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), X-ray diffraction pattern, Field emission scanning electron microscopy (FE-SEM) and high resolution transmission electron microscopy (HR-TEM). Electron spin resonance (ESR) studies confirmed that the nanocomposite is magnetic in nature. Up to 100% adsorption was found with 200mg/L Cr(VI) aqueous solution at pH 2. Adsorption of Cr(VI) on the surface of the adsorbent was confirmed by the ATR-FTIR and X-ray photoelectron spectroscopy (XPS). XPS studies also suggested that ion exchange and reduction on the surface of the nanocomposite may be the possible mechanism for Cr(VI) removal by the PPy/Fe(3)O(4) nanocomposite. Adsorption results showed that Cr(VI) removal efficiency by the nanocomposite decreased with an increase in pH. Adsorption kinetics was best described by the pseudo-second-order rate model. Isotherm data fitted well to the Langmuir isotherm model. Thermodynamic study revealed that the adsorption process is endothermic and spontaneous in nature. Desorption experiment showed that in spite of the very poor recovery of the adsorbed Cr(VI); the regenerated adsorbent can be reused successfully for two successive adsorption-desorption cycles without appreciable loss of its original capacity.     

Removal of fluoride from aqueous solution by polypyrrole/Fe3O4 magnetic nanocomposite

Polypyrrole (PPy)/Fe₃O₄ magnetic nanocomposite as a novel adsorbent was prepared via in-situ polymerization of pyrrole (Py) monomer using FeCl₃ oxidant in aqueous medium in which Fe₃O₄ nanoparticles were suspended. The adsorbent was characterized by Attenuated Total Reflectance Fourier transform infrared spectroscope (ATR-FTIR), Brunauer–Emmet–Teller (BET) method, field emission scanning electron microscope (FE-SEM), high resolution transmission electron microscope (HR-TEM), X-ray photoelectron spectroscope (XPS) and X-ray diffraction (XRD). Magnetic property of the adsorbent was measured by electron spin resonance (ESR). Subsequently, the ability of the adsorbent to remove fluoride ions from aqueous solution was demonstrated in a batch sorption mode. Results reveal that the adsorption is rapid and that the adsorbent has high affinity for fluoride, which depends on temperature, solution pH and adsorbent dose. From equilibrium modelling, the equilibrium data is well described by Freundlich and Langmuir–Freundlich isotherms while the adsorption kinetics is described by the pseudo-second-order model. Thermodynamic parameters confirm the spontaneity and endothermic nature of the fluoride adsorption. Meanwhile, the fluoride adsorption proceeds by an ion exchange mechanism.     

涂层结构设计对等离子喷涂陶瓷层结合强度及其应力的影响

用等离子在45#碳钢上喷涂了不同涂层设计的Al2O3以及Al2O3+130mg·g-1TiO2陶瓷层.用X-射线衍射法和拉伸实验测量了涂层表面层中的残余应力及结合强度.增加粘结层和过渡层能大大地克服陶瓷涂层与基材机械的以及热的不匹配性,使涂层的应力和结合强度都得到明显改善.此外,SiO2能改善ZrO2陶瓷层与基材以及陶瓷层内部的结合程度,使涂层内应力松弛并使其结合强度提高.然而SiO2添加剂只有在高熔点陶瓷层中(如ZrO2),"液相烧结"作用才明显,而在熔点较低的陶瓷层中(如Al2O3),这种作用并不明显.在用等离子喷涂低熔点Al2O3陶瓷时,添加适量的低熔点TiO2陶瓷是必要的.     

微乳液法制备掺杂铁的纳米二氧化钛及其表征

为了研究掺杂铁的纳米二氧化钛的性质,以TiCl4为原料,在CTAB/正丁醇/环己烷/水组成的微乳液体系中制备了掺杂铁的TiO2纳米粉末。采用热分析仪(TG-DTA)、X射线衍射分析(XRD)、透射电子显微镜(TEM)和比表面分析仪(BET)等对粉体的结构、粒径大小、物相、形貌和比表面积等进行了表征。经600℃焙烧2h后,0.04%Fe3+-TiO2粉末为单一的锐钛型结构,其平均晶粒度约为16nm,比表面积达120.4m2.g-1,D101为16.1nm。由于在XRD图谱上未发现有新相的生成,因此,Fe3+经过焙烧渗入到了二氧化钛的晶格中,掺杂所引起的变化主要是由于Fe3+渗入TiO2晶格所引起的。     

改性油菜秸秆对水溶液中碱性品红的吸附性能研究

采用傅里叶红外光谱仪(FTIR)对天然和改性油菜秸秆进行表征,探究了溶液初始pH值、吸附剂投加量、碱性品红初始质量浓度、吸附时间等因素对天然和改性油菜秸秆吸附碱性品红的影响。实验表明:经酒石酸改性的油菜秸秆对碱性品红的吸附容量较天然油菜秸秆提升了近1倍,最大吸附量由改性前的70.922mg·g~(-1)增加至138.889mg·g~(-1)。298K时,在不调节染料溶液初始pH值,投加量为0.04g,吸附60min条件下,改性油菜秸秆对100mg·L~(-1)碱性品红的去除率达到了95.85%。实验结果符合Langmuir等温吸附模型,相关系数R2值在0.99以上。改性油菜秸秆对碱性品红的吸附符合准二级动力学方程。     

Fe3O4复合材料对Cd2+的吸附性能研究

在碱性条件下,以共沉淀法合成Fe₃O₄,再以正硅酸乙酯和二乙烯三胺为原料,制备出Fe₃O₄复合材料(Fe₃O₄-SiO₂-NH₂)。采用FT-IR、VSM和SEM对其结构进行表征,并研究了复合材料对Cd2+的吸附性能。实验结果表明,在T=55℃、t=60 min、Cd2+溶液的初始浓度为100 mg·L-1、Fe₃O₄-SiO₂-NH₂的添加量为0.1 g时,该材料对Cd2+的吸附容量为71.4 mg·g-1。其吸附动力学行为更符合准二级动力学,热力学更适合用Langmuir等温吸附模型描述。Fe₃O₄-SiO₂-NH₂吸附Cd2+后洗脱再生,经过5次循环使用后,其对Cd2+的去除率仍然大于70%。      

Magnetic chitosan nanoparticles for removal of Cr(VI) from aqueous solution

A simple method was introduced to prepare magnetic chitosan nanoparticles by co-precipitation via epichlorohydrin cross-linking reaction. The average size of magnetic chitosan nanoparticles is estimated at ca. 30 nm. It was found that the adsorption of Cr(VI) was highly pH-dependent and its kinetics follows the pseudo-second-order model. Maximum adsorption capacity (at pH 3, room temperature) was calculated as 55.80 mg·g^? 1, according to Langmuir isotherm model. The nanoparticles were thoroughly characterized before and after Cr(VI) adsorption. From this result, it can be suggested that magnetic chitosan nanoparticles could serve as a promising adsorbent for Cr(VI) in wastewater treatment technology.     

TiO2-聚吡咯纳米复合材料的电化学制备及其在锂硫电池中的应用

采用电化学沉积的方法,以阳极氧化法制备的二氧化钛纳米管阵列为基底,制备出高度有序的TiO_2-聚吡咯(PPy)纳米阵列,再通过共热法,将单质硫颗粒负载到基底阵列中,得到S/PPy/TiO_2纳米阵列结构复合材料。扫描电镜(SEM)、透射电镜(TEM)、能谱(EDX)、傅里叶变换红外光谱(FT-IR)和热重分析(TGA)表征结果表明,TiO_2纳米管高度有序平行排列,管径约120nm,聚吡咯均匀沉积在纳米管壁上,复合材料中硫的质量分数约为61.9%。电化学测试结果表明,在0.1C电流密度下,S/PPy/TiO_2纳米复合材料首次循环比容量达1155mAh·g-1,100次循环后比容量为648.4mAh·g-1,库伦效率保持在96.8%。高容量下良好的循环稳定性能显示出S/TiO_2/PPy纳米阵列结构复合材料作为锂硫电池正极材料的优势。     

Fabrication of magnetic activated carbon by carbothermal functionalization of agriculture waste via microwave-assisted technique for cationic dye adsorption

The agriculture shell wastes were carbothermally converted to magnetic activated carbon by a microwave-assisted decoration of iron oxide nanoparticles onto the shell surface. The influence of ternary catalytic mixtures, including zinc, iron II and III chlorides on the cationic dye adsorption efficiency was addressed by the composite impregnations onto the almond or walnut shell powders, explored to the carbonization. The efficiency was maximized by determination the proportions of used salts. The best results were obtained with loading FeCl₃ onto the walnut shell in which the proportion of salt was 50%. Although the load of magnetic particles onto the adsorbent normally lead to decrease in efficiency, the prepared powder exhibited the appropriate performance above 99%. It should be point out that the dye adsorption efficiency of magnetic activated carbons fabricated by carbothermal functionalization was 7–10% higher than those produced in the nitrogen atmosphere. The adsorbent displayed the nano-porous structure with average pore diameter about 2 nm, providing a surface area around 1000 m²·g⁻¹ for the removal of dye in a dynamic system. The maximum adsorption capacity was determined to be 130 mg·g⁻¹ in the neutral condition.