复合改性活性炭的表征及其吸附模拟烟气中SO_2的研究

为了研究单一金属盐和复合金属盐改性活性炭材料对SO_2吸附性能的影响,以活性炭(activated carbon,AC)为载体,通过水热法制备ZnO/AC复合材料、Fe_2O_3/AC复合材料、ZnFe_2O_4/AC复合材料以及空白AC材料。采用场发射扫描电镜(SEM)、X射线能谱仪(EDS)、X射线衍射仪(XRD)、傅立叶变换红外光谱仪(FTIR)、物理吸附仪(BET)及X射线光电子能谱分析仪(XPS)对复合材料结构及化学组分进行表征,并且在常温条件下考察活性炭复合改性前后对模拟烟气中SO_2的吸附性能。结果表明,复合改性后活性炭材料成功负载金属氧化物活性组分,比表面积孔容减小,孔径增大并且对SO_2的去除效率显著提高。通过AC、ZnFe_2O_4以及4种复合材料脱硫效率的比较发现,负载ZnFe_2O_4的活性炭材料的脱硫效率最高,其比表面积和孔容分别为435.9m~2/g、0.37cm~3/g,脱硫性能试验中样品的击穿时间为136.0min,硫容达到168.3mg/g。     

CeO2-TiO2复合氧化物的制备及其表征

本文以廉价的无机盐为原料,采用sol－gel法制备了Ce：Ti（摩尔比）为0．05～0．4：1之间的一系列CeO₂－TiO₂复合氧化物．利用物理吸附仪,XRD,TEM等手段对复合氧化物的织构和结构性质进行了表征．结果发现：采用无机盐－超临界流体干燥法可制备大孔、高比表面积的CeO₂－TiO₂复合氧化物,随着CeO₂含量从5％增加到40％,复合氧化物的比表面积由67．3m²·g^－1增加到219．4m²·g^－1;物相由锐钛矿转变为无定形;粒体的粒径、形貌也随之变化,由颗粒状逐渐变为网络结构．而与超临界流体干燥得到的气凝胶相比;采用普通干燥法制备得到的复合氧化物具有较低的孔体积和比表面积,颗粒间团聚较严重,但无“孤岛”状大颗粒,晶相为无定型结构．     

纳米TiO2-Cu2O可见光下光催化降解活性艳红及其机理研究

采用钛酸丁酯水解和肼还原醋酸铜的方法制备出TiO2-Cu2O复合氧化物,研究了TiO2-Cu2O复合光催化剂在可见光照射下光催化降解活性艳红X-3B的性能,考察了催化剂组成、催化剂投加量、溶解氧、H2O2等对光催化反应的影响,探讨了Cu2O及TiO2-Cu2O光催化降解有机污染物的机理。结果表明,由于TiO2和Cu2O之间存在协同作用,使得复合氧化物的活性比单一的Cu2O高。Cu2O光催化的氧化物种为·OH和光生空穴。光生电子(e-)还原吸附在Cu2O表面上的氧,产生超氧阴离子,然后再进一步生成·OH,光生空穴(h+)无法直接将吸附在Cu2O表面的OH-氧化成·OH。     

Ni-Mo-Al_2O_3催化剂覆碳改性对其加氢脱硫性能的影响

在催化剂制备的不同阶段引入碳物质,制备3种覆碳改性的NiMo-Al_2O_3加氢脱硫催化剂,采用低温氮静态容量吸附-脱附法、X射线衍射、H_2程序升温还原和高分辨透射电子显微镜对3种催化剂进行表征,并考察催化剂的加氢脱硫性能。结果表明:引入碳物质能够提高催化剂的加氢脱硫活性;采用前覆碳法即在载体上负载活性组分前引入碳前躯物,或采用共浸渍法即将活性组分与碳前躯物共同浸渍到载体上制得的催化剂,都能够增加八面体Mo物种的数量;采用共浸渍法制得催化剂活性组分分散性良好,MoS_2纳米颗粒堆垛层数多,其脱硫率比未覆碳改性催化剂的高6.8%;采用前覆碳法制得催化剂的金属分散性良好,其脱硫率比未覆碳改性催化剂的高5.1%;与未覆碳改性的催化剂相比,采用后覆碳法即在已负载活性组分的Ni-Mo-Al_2O_3催化剂上引入碳前躯物制得催化剂的脱硫率提高程度不大。     

MgAlZnFeCe类水滑石水热合成、表征及其FCC硫转移性能的研究

分别以MgO为镁源,拟薄水铝石为铝源,以Zn、Fe、Ce的氯化盐为助剂,水热法合成了MgAlZnFeCe类水滑石前驱体,经过700℃焙烧6h后,制得新型FCC硫转移剂MgAlZnFeCe复合氧化物.运用XRD、TG-DTA等对硫转移剂及其前驱体的结构和物化性能进行了表征;在模拟FCC反应再生条件下,采用改装的WRP-3热重天平评价了硫转移剂的氧化吸硫和还原脱硫的性能.结果表明,采用水热法合成的前驱体材料具有典型的类水滑石结构,但MgO不能完全进入水滑石相,以Mg(OH)2的形式存在;类水滑石材料经过焙烧后得到复合氧化物MgAlZnFeCe-LDOs,在FCC再生烟气硫转移中具有良好的饱和吸附硫容量和氧化吸硫速率,10min可达到1.16g/g的饱和吸附能力,同时具有较强的还原脱硫能力.     

掺杂不同量Nd2O3对CeO2-ZrO2-Al2O3材料性能的影响

采用共沉淀法制备了一系列Nd2O3含量为0～13wt%的CeO2-ZrO2-A12O3(CZA)复合氧化物,并通过X射线衍射(XRD)、低温N2吸附–脱附、氧脉冲吸附(OSC)、H2–程序升温还原(H2-TPR)及扫描电子显微镜(SEM)等方法对所制备的材料进行了表征.研究结果表明,Nd2O3在CZA固溶体中的溶解限约为10wt%,过量Nd的添加会出现分相形成Nd0.5Ce0.5O1.75氧化物.掺杂适量Nd能有效抑制氧化物晶粒的长大,提高材料的热稳定性和氧化还原性能.Nd2O3的掺杂量为10wt%时,样品的织构稳定性最好,1000℃老化5 h后,比表面积和孔容分别达97.14 m2/g和0.44 mL/g.Nd2O3的掺杂量为7wt%时,样品有高的储氧量,经600℃和1000℃焙烧后储氧量分别为938.01μmol/g和821.72μmol/g;体相氧的移动能力最强,还原性能最佳,老化后还原峰温由465℃升高到483℃.SEM结果表明,所制备的材料均为球形颗粒,Nd2O3的添加可以有效阻止高温焙烧过程中粒子的团聚.     

改性纳米SiO_2/PVA复合纤维的制备及重金属离子吸附性能

通过静电纺丝技术制备酰肟化功能改性的纳米SiO_2/聚乙烯醇(SiO_2/PVA)复合纤维膜。采用SEM、FTIR、DSC和TGA进行表征分析;考察了在水溶液中随pH值和接触时间的变化纤维膜对金属离子吸附效果的影响。研究表明,在pH=6的条件下,纳米纤维对金属离子的吸附最佳,对Cu2+、Ni 2+金属离子的最大吸附量分别为143.7mg/g和125.1mg/g,平衡吸附时间为240min。在纤维膜吸附的前50min内,SiO_2/PVA纤维膜对Cu2+和Ni 2+金属离子的吸附量为126.8mg/g和109.8mg/g,吸附率分别为90.18%和89.92%。通过吸附等温线和吸附方程考察SiO_2/PVA纤维对Cu2+和Ni 2+金属离子的吸附行为。结果显示,复合纤维对两种金属离子的吸附满足拟二级动力学方程,热力学分析表明,吸附过程符合Langmuir单层吸附。使用酸处理纤维膜进行再生吸附试验,发现循环4次试验后,吸附效率达到53%,结果说明复合纤维膜可作为可再生金属离子吸附材料。     

CeO2-TiO2复合氧化物的制备及其表征

本文以廉价的无机盐为原料,采用sol－gel法制备了Ce：Ti（摩尔比）为0．05～0．4：1之间的一系列CeO2－TiO2复合氧化物．利用物理吸附仪,XRD,TEM等手段对复合氧化物的织构和结构性质进行了表征．结果发现：采用无机盐－超临界流体干燥法可制备大孔、高比表面积的CeO2－TiO2复合氧化物,随着CeO2含量从5％增加到40％,复合氧化物的比表面积由67．3m2·g－1增加到219．4m2·g－1;物相由锐钛矿转变为无定形;粒体的粒径、形貌也随之变化,由颗粒状逐渐变为网络结构．而与超临界流体干燥得到的气凝胶相比;采用普通干燥法制备得到的复合氧化物具有较低的孔体积和比表面积,颗粒间团聚较严重,但无“孤岛”状大颗粒,晶相为无定型结构．     

油品脱硫技术研究进展

目前油品的脱硫技术主要分为加氢脱硫技术和非加氢脱硫技术。本文主要介绍了加氢脱硫技术和萃取脱硫技术、络合脱硫技术、生物脱硫技术、氧化脱硫技术、吸附脱硫技术等几种非加氢脱硫技术的原理和最新的研究情况,并简单介绍了各种技术的优缺点。     

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。     

Fe2O3/EPDM新型吸油材料的制备及其吸油性

以三元乙丙橡胶(EPDM)作为基体, Fe₂O₃和焙烧过的Fe₂O₃粉末分别作为填料, 利用熔融共混的方法, 制备出一种新型吸油复合材料, 这类材料可以直接漂浮于含油废水表面使用。研究了填料和交联剂的用量对材料吸油率的影响。结果表明: 交联剂过氧化二异丙苯(DCP)为3wt％, Fe₂O₃为25wt％时, Fe₂O₃/EPDM吸油率达到最大; DCP为2wt%, Fe₂O₃(焙烧)为30wt%时, Fe₂O₃(焙烧)/EPDM吸油率达到最大。选择2组样品中吸油率最高的样品, 对比它们对机油的吸油速率。实验表明, Fe₂O₃(焙烧)/EPDM的吸油速率大于Fe₂O₃/EPDM的吸油速率。Fe₂O₃/EPDM的吸油率比交联EPDM的吸油率提高了227%; Fe₂O₃(焙烧)/EPDM的吸油率比Fe₂O₃/EPDM的吸油率最大可提高64%。分析认为, Fe₂O₃粒子破坏掉一部分高分子链段间的作用力, 并对网络起支撑作用, 为油分子提供了更多的进入通道和空间, 故吸油性得到提高。Fe₂O₃(焙烧)/EPDM的吸油特性要优于Fe₂O₃/EPDM。      

3D Bi12TiO20/TiO2 hierarchical heterostructure: synthesis and enhanced visible-light photocatalytic activities

A three-dimensional (3D) multicomponent oxide, Bi(12)TiO(20)/TiO(2) hierarchical heterostructure was successfully synthesized via a one-step and template-free hydrothermal route. X-ray diffraction and X-ray photoelectron spectroscopy measurements confirm that the composition of the as-fabricated sample is Bi(12)TiO(20)/TiO(2) composite. Scanning and transmission electron microscopy observation reveals that the as-synthesized sample is microsized flower-like hierarchical networks consisted of Bi(12)TiO(20) nanorods decorated with the primary TiO(2) nanoparticles. Extension of the light absorption from the ultraviolet region to the visible-light region was confirmed by UV-vis absorption spectra. Due to the structure-property relationships, the 3D Bi(12)TiO(20)/TiO(2) heterostructure exhibited enhanced visible photocatalytic activity over that of Bi(12)TiO(20) and TiO(2) samples in the decomposition of Rhodamine B in water which is a typical model pollutant. The enhanced photocatalytic activity can be attributed to the extended absorption in the visible light region resulting from the 3D Bi(12)TiO(20)/TiO(2) heterostructures, and the effective separation of photogenerated carriers driven by the photoinduced potential difference generated at the Bi(12)TiO(20)/TiO(2) junction interface, demonstrating that the Bi(12)TiO(20)/TiO(2) heterostructure is a promising candidate as a visible light photocatalyst.     

VO2(B)/ZnO异质复合纳米棒结构的室温NH3敏感性能研究

以VO₂(B)纳米棒为内核, 利用液相生长法制备了VO₂(B)/ZnO异质复合纳米棒, 研究了ZnO生长溶液浓度对复合结构微观形貌和气敏性能的影响规律。采用扫描电子显微镜和X射线衍射仪对复合结构样品的微观形貌和结晶取向进行表征, 并测试了复合结构对NH₃的敏感性能。实验结果表明, 随着ZnO种子液浓度的增大, ZnO逐渐由纳米颗粒生长为纳米棒结构, 当ZnO种子液浓度为0.01 mol/L时, ZnO呈棒状沿径向发散生长在VO₂(B)纳米棒表面, 形成树枝状VO₂(B)/ZnO异质复合纳米棒结构, 这一结构在室温下表现出对NH₃的高灵敏度和突出的选择性, 其灵敏度最大可达5.6, 对NH₃的响应时间最短仅为2 s。在室温下表现出的优良NH₃敏感性能, 主要与高密度的VO₂(B)/ZnO异质结和树枝状结构有关。研究结果为低功耗高灵敏度NH₃气敏传感器的研制提供了重要依据。     

Preparation of Co-Ni Oxide/Vertically Aligned Carbon Nanotube and Their Electrochemical Performance in Supercapacitors

A Co-Ni oxide/vertically aligned carbon nanotube (VACNT) composite was prepared by thermal decomposition of cobalt-nickel nitrate precursor on the surface of VACNT electrode. VACNTs were used as 3D nanoporous substrate and were grown by plasma-enhanced chemical vapor deposition from a mixture of H₂ and C₂H₂. The specific capacitance of Co-Ni oxide (5:5)/VACNT (with equal Co⁺²/Ni⁺² mole ratio) was measured to be 1050 Fg^?1, which is about 1.9- and 3-fold that of Ni oxide/VACNT (540 Fg^?1) and Co oxide/VACNT (341 Fg^?1), respectively. The results show Co-Ni oxide (5:5)/VACNT composite electrode has excellent specific capacitance because of porous network structure, good electrical conduction pathways, high access for the electrolyte solution, and consequently increased composite/solution interfacial contact area. The capacitance property of the Co-Ni oxide/VACNT composite electrode with different Co⁺²/Ni⁺² mole ratios was also investigated and the highest specific capacitance is achieved at equal Co⁺²/Ni⁺² mole ratio.     

Facile synthesis of monodisperse superparamagnetic Fe3O4/PMMA composite nanospheres with high magnetization

Monodisperse superparamagnetic Fe(3)O(4)/polymethyl methacrylate (PMMA) composite nanospheres with high saturation magnetization were successfully prepared by a facile novel miniemulsion polymerization method. The ferrofluid, MMA monomer and surfactants were co-sonicated and emulsified to form stable miniemulsion for polymerization. The samples were characterized by DLS, TEM, FTIR, XRD, TGA and VSM. The diameter of the Fe(3)O(4)/PMMA composite nanospheres by DLS was close to 90 nm with corresponding polydispersity index (PDI) as small as 0.099, which indicated that the nanospheres have excellent homogeneity in aqueous medium. The TEM results implied that the Fe(3)O(4)/PMMA composite nanospheres had a perfect core-shell structure with about 3 nm thin PMMA shells, and the core was composed of many homogeneous and closely packed Fe(3)O(4) nanoparticles. VSM and TGA showed that the Fe(3)O(4)/PMMA composite nanospheres with at least 65% high magnetite content were superparamagnetic, and the saturation magnetization was as high as around 39 emu g(-1) (total mass), which was only decreased by 17% compared with the initial bare Fe(3)O(4) nanoparticles.     

Influence of Surface-functionalized Graphene Oxide on the Cell Morphology of Poly(methyl methacrylate) Composite

The surface chemistry of filler is closely related to the structure and morphology of nanocomposite foams.Changing the property of filler is widely used to control the cell structures and functionalize the composite foams.Surface-functionalized graphene oxide(GO-ODA) was prepared by grafting octadecylamine(ODA) on the surface of graphene oxide(GO) to make the filler disperse better in the nanocomposites and have a strong interfacial interaction with polymer matrix.Poly(methyl methacrylate)(PMMA)/GO-ODA nanocomposite foams were obtained by solution blending and foamed using supercritical carbon dioxide(scCO_2).Compared to neat PMMA and PMMA/GO samples,the PMMA/GO-ODA nanocomposite foams showed improved cell structures with smaller size,higher cell density and more homogeneous distribution,which should be attributed to the heterogeneous nucleation caused by well-dispersed GO-ODA nanosheets.This work not only improved the compatibility and interfacial interaction of GO with polymer matrix but also indicated that the modified GO sheets can act as ideal filler to control the cell density,size and size distribution efficiently.     

TiB_2含量对AlMgB_(14)基复合材料抗高温氧化性能的影响

为了揭示纳米TiB_2对AlMgB_(14)基复合材料抗高温氧化性能的影响机理,对不同TiB_2含量(质量分数分别为0、10%和30%)的AlMgB_(14)基复合材料的抗高温氧化性能进行了研究和讨论,试验温度800℃,氧化时间10h。试样氧化前后的表面和截面形貌采用扫描电子显微镜(SEM)进行观察,氧化产物采用X射线衍射仪(XRD)进行分析。结果表明:随着TiB_2含量的增加,氧化膜厚度逐渐减小,氧化速率逐渐变缓,氧化层主要物相由Al_2O_3逐渐变化为TiO和TiO_2,说明添加的纳米TiB_2能显著阻止复合材料内部组织的氧化,提高复合材料的抗高温氧化性能。     

Synthesis and dye-sensitized solar cell performance of nanorods/nanoparticles TiO2 from high surface area nanosheet TiO2

High surface area nanosheet TiO2 with mesoporous structure were synthesized by hydrothermal method at 130 degrees C for 12 h. The samples characterized by XRD, SEM, TEM, SAED, and BET surface area. The nanosheet structure was slightly curved and approximately 50-100 nm in width and several nanometers in thickness. The as-synthesized nanosheet TiO2 had average pore diameter about 3-4 nm. The BET surface area and pore volume of the sample were about 642 m(2)/g and 0.774 cm(3)/g, respectively. The nanosheet structure after calcinations were changed into nanorods/nanoparticles composite with anatase TiO2 structure at 300-500 degrees C (10-15 nm in rods diameter and about 5-10 nm in particles diameter). The solar energy conversion efficiency (eta) of the cell using nanorods/nanoparticles TiO2 (from the nanosheet calcined at 450 degrees C for 2 h) with mesoporous structure was about 7.08% with Jsc of 16.35 mA/cm(2), Voc of 0.703 V and ff of 0.627; while eta of the cell using P-25 reached 5.82% with Jsc of 12.74 mA/cm(2), Voc of 0.704 V, and ff of 0.649.     

聚吡咯/氧化石墨复合材料的制备及其电容性能

以氧化石墨为载体,采用木质素磺酸钠作为掺杂剂,氯化铁作为氧化剂,引发吡咯单体在氧化石墨层发生化学原位聚合反应,制备了聚吡咯(PPy)/氧化石墨复合材料。通过XRD、FTIR和SEM分析分别对复合材料的物相组成、结构和微观形貌进行了表征,通过TGA分析研究了复合材料的热稳定性,采用恒电流充放电、循环伏安和电化学阻抗谱等方法测试分析其电化学性能。研究表明:采用化学原位聚合的方法合成的PPy/氧化石墨复合材料具有"层-球"状的"三明治"型微观结构,以便形成良好的导电网络,其结晶度高、排列规整、缺陷少,复合材料中吡咯单体通过N-H键与氧化石墨的含氧官能团发生键合。PPy/氧化石墨复合材料新颖的微观结构和良好的化学键合状态使其表现出优异的电容性能。在电流密度分别为0.5、1.0、2.0和5.0 A/g时的比电容分别为500、460、427和396 F/g;经过1000次恒电流(2.0 A/g)充放电循环后, PPy/氧化石墨复合材料的比电容保持率为97.2%。      

Facile Preparation of SiO(2)/TiO(2) Composite Monolithic Capillary Column and Its Application in Enrichment of Phosphopeptides

A novel SiO(2)/TiO(2) composite monolithic capillary column was prepared by sol-gel technology and successfully applied to enrich phosphopeptides as a metal oxide affinity chromatography (MOAC) material. For the monolith preparation, tetramethoxysilane (TMOS) and tetrabutoxytitanium (TBOT) were used as silica and titania source, respectively, and glycerol was introduced to attenuate the activity of titanium precursor, which provided a mild synthetic condition. The prepared monolith was characterized by energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). The results revealed an approximate 1/2 molar ratio of titanium to silica as well as an atom-scale homogeneity in the framework. The scanning electron microscopy (SEM) results demonstrated an excellent anchorage between the column and the inner capillary wall, and nitrogen adsorption-desorption experiments showed a bimodal porosity with a narrow mesopore distribution around 3.6 nm. The prepared monolith was then applied for selective enrichment of phosphopeptides from the digestion mixture of phosphoproteins and bovine serum albumin (BSA) as well as human blood serum, nonfat milk, and egg white using an in-tube solid phase microextraction (SPME) system. Our results showed that SiO(2)/TiO(2) composite monolithic capillary column could efficiently enrich the phosphopeptides from complex matrixes. To the best of our knowledge, this is the first attempt for preparing the silica-metal composite monolithic capillary column, which offers the promising application of the monolith on phosphoproteomics study.