TiO2/Fe2O3纳米复合材料的制备及光催化性能

分别以Fe(NO₃)₃·9H₂O和钛酸四丁酯为铁源和钛源,以HF、HAc、NH₄F、NH₃·H₂O、H₂O₂为形貌控制剂,通过沉淀分离法联合溶胶-凝胶法制备了不同形貌的TiO₂/Fe₂O₃纳米复合材料。用X-射线粉末衍射仪(XRD)和场发射扫描电子显微镜(FESEM)对TiO₂/Fe₂O₃样品的结构和形貌进行了分析,并探究了所合成的TiO₂/Fe₂O₃纳米复合材料在紫外光照射条件下对亚甲基蓝(MB)的降解性能。结果表明,当以NH₃·H₂O为形貌控制剂时,制备的NH₃·H₂O-TiO₂/Fe₂     

Fenton氧化法处理双唑杂环废水

以含双唑杂环类化合物的模拟废水为对象,采用Fenton氧化和高效液相色谱法研究了pH、反应时间和Fenton试剂用量等影响因子对双吡唑模拟废水处理效果的影响,通过高效液相色谱测试探究了Fenton处理双唑杂环类结构的降解机理。结果表明,最佳处理条件为:初始pH=3、反应时间为30 min、 m（Fe²⁺）∶V（H₂O₂）=1∶20、FeSO₄·7H₂O投加量2.5 g/L、H₂O₂投加量50 mL/L,双吡唑去除率可达97.5%,COD去除率可达82.1%。Fenton氧化过程中依次产生更为亲水的中间物质,亲水性越强的物质更难被破坏。     

In2O3/ZnIn2S4复合光催化剂的制备及其降解甲基橙性能

采用二次水热法构建了In₂O₃/ZnIn₂S₄异质结光催化剂,通过XRD、SEM、DRS、电化学等表征研究此异质结光催化剂的晶体结构、形貌、光学性质及光生载流子的分离效率。在模拟可见光下,以甲基橙作为目标污染物,通过考察光催化降解甲基橙的效率来评价其性能。研究表明,In₂O₃/ZnIn₂S₄复合光催化剂的光催化性能明显优于In₂O₃、ZnIn₂S₄,In₂O₃与ZnIn₂S₄摩尔比为0.3∶1的复合光催化剂在90 min内降解效率可以达到96.33%,3次循环后降解效果仍能达到78.26%,具有较好的稳定性。     

Fe3O4/CuCo2S4复合物活化过硫酸一氢盐对有机染料的去除作用

采用水热法制备了Fe₃O₄/CuCo₂S₄复合催化剂,利用SEM、XRD、EDS对0.25-Fe₃O₄/CuCo₂S₄复合材料的表面形貌和结构进行表征,研究了复合催化剂活化PMS降解染料废水的效能。实验结果显示,在室温条件下,加入200 mg/L PMS、125 mg/L催化剂,20 mg/L RhB在40 min内去除率达到99.5%。自由基淬灭实验表明,Fe₃O₄/CuCo₂S₄活化PMS产生的羟基自由基、硫酸根自由基和单线态氧等活性物质均参与了RhB降解过程。回收实验表明,4次循环使用后RhB的降解率仍能达到94.2%,表明Fe₃O₄/CuCo₂S₄复合催化剂具有良好的可重复利用性和优异的催化活性,易于回收。Fe₃     

Fe/硅藻土、Fe/ZSM-5非均相Fenton处理垃圾渗滤液的研究

以硅藻土、ZSM-5分子筛为载体，以Fe(NO₃)₃·9H₂O为Fe源，制备了Fe/硅藻土、Fe/ZSM-5两种催化剂，分别与H₂O₂组成非均相Fenton体系处理垃圾渗滤液。研究了溶液pH值、温度、H₂O₂用量、催化剂加入量和反应时间对垃圾渗滤液COD去除效果的影响。实验结果表明：利用该非均相Fenton体系处理COD浓度为1 110mg/L的垃圾渗滤液，在溶液体系pH值为3.0,反应温度30℃,催化剂投加量折合浓度为1.6 g/L,H₂O₂加入量折合浓度为0.2 mol/L,反应时间60 min的条件下，Fe/硅藻土、Fe/ZSM-5两种催化剂处理垃圾渗滤液COD去除率可分别达到88.78%和92.58%。     

混凝-Fenton联合工艺处理垃圾渗滤液膜滤浓缩液

为了去除垃圾渗滤液膜滤浓缩液中的污染物,文中通过混凝实验选择了混凝剂,寻找出了最优混凝剂的最佳运行pH值和投加量;同时通过Fenton试验确定了FeSO₄·7H₂SO₄和H₂O₂的投加量,最终形成了混凝与Fenton氧化联合的工艺。研究结果表明：文中工艺可以有效去除浓缩液中的COD和色度,最佳混凝剂为FeCl₃,当初始pH为4,FeCl₃的量为400 mg·L^-1,FeSO₄·7H₂SO₄量为250 mg·L^-1,H₂O₂量为1 mL·L^-1时,可以得到最优的去除效果,两种污染物的去除率分别为76.75%和85.18%。结论可为相近水质的垃圾渗滤液膜滤浓缩液的处理提供理论依据。     

Fe3O4/SnS2的制备及其催化性能研究

为提高Fe₃O₄的类芬顿效果,基于光助类芬顿催化氧化技术,在共沉淀法制备Fe₃O₄的基础上采用醇热法制备能高效降解亚甲基蓝的Fe₃O₄/SnS₂催化剂。建立了以Fe₃O₄/SnS₂为催化剂的光助类芬顿催化氧化体系,分析不同制备及降解条下Fe₃O₄/SnS₂的类芬顿活性,并通过X射线衍射(XRD)、扫描电子显微镜(SEM)等对Fe₃O₄/SnS₂材料进行表征。结果表明：当Fe₃O₄和SnS₂物质的量比为1∶1时,Fe₃O₄/SnS₂的催化效果最好;亚甲基蓝溶液pH为3.0、Fe₃O_...     

等离子体辅助制备的Co3O4光催化甲苯净化性能研究

等离子体改性是提高催化材料性能的有效途径。利用水热法合成了Co₂(OH)₂CO₃前驱体，通过氧气低温等离子体技术，制备了表面改性的Co₃O₄催化剂(Co₃O₄-P)，并对其进行了XRD、O₂-TPD、H₂-TPR、SEM、TEM、XPS、FTIR、Raman和UV-Vis等表征。结果表明，等离子体处理可以降低Co₃O₄中Co元素的平均价态，在其表面形成更多的缺陷点位，降低Co₃O₄的Co-O键能，增强其低温还原性能；在全太阳光谱的光强为776 mW/cm²、反应空速为30 000 mL/(g·h)、甲苯质量分数为500μg/g的测试条件下，Co₃O₄-P的甲苯降解率为100.0%,其值约为通过焙烧法制备的Co₃O     

低碱比H2O2的电化学合成

采用线性扫描伏安法和恒电流电解技术探讨了分隔式电解槽中以自制的石墨/聚四乙烯气体扩散电极（GDE）合成低碱比H₂O₂溶液的方法,着重考察了pH值、催化剂（2-乙基蒽醌）载量、电流密度及电解液温度等对H₂O₂电合成效率的影响.结果表明:当温度低于35℃时,在分隔式电解槽中以pH=12的2.5%Na₂SO₄溶液为阴极液、2-乙基蒽醌载量为1 mg/cm²的GDE为阴极,控制电流密度为750 A/m²条件下,经8 h电解可以制得低碱比（0.23）的H₂O₂溶液,其中H₂O₂浓度达0.45 mol/L.18 d的连续电解试验初步表明该体系具有较高的电流效率（约83%）和良好的稳定性,从而为电Fenton和光电Fenton法在废水处理领域的实用应用奠定了良好的基础.     

PMo12/TiO2光催化降解工业DNBP废水的研究

采用溶胶-凝胶法和水热合成法制备H₃PMo₁₂O₄₀(PMo₁₂)/TiO₂复合光催化剂并应用于工业废水的降解。利用红外光谱仪(IR),X射线衍射仪(XRD),X射线光电子能谱(XPS)和扫描电子显微镜(SEM)进行测定，并在紫外光照射下分析光催化剂对DNBP废水的光催化降解性能。考察了废水的初始pH值、催化剂用量及重复利用率等对DNBP废水降解的影响。结果表明，在光照时间为5 h, pH值为5.10,用量为1.00 g/L的条件下，复合光催化剂较单纯TiO₂催化剂的光催化性能有明显提高，降解率达到98.36%,COD去除率达到53.18%,且POM/TiO₂复合催化剂回收利用3次仍具有较高活性。     

Synthesis of γ-Al2O3 nanoparticles by chemical precipitation method

Highly pure active γ-Al₂O₃ nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studied. The properties of γ-Al₂O₃ nanoparticles were characterized by DTA, XRD, BET, TEM, laser granularity analysis and impurity content analysis. The results show that the amorphous precursor Al(OH)₃ sols are produced by using 0.1 mol/L Al(NO₃)₃ · 9H₂O and 0.16 mol/L (NH₄)₂CO₃ · H₂O reaction solutions, according to the volume ratio 1.33, adding 0.024% (volume fraction) surfactant PEG600, and reacting at 40 °C, 1 000 r/min stirring rate for 15 min. Then, after stabilizing for 24 h, the precursors were extracted and filtrated by vacuum, washed thoroughly with deionized water and dehydrated ethanol, dried in vacuum at 80°C for 8 h, final calcined at 800 °C for 1 h in the air, and high purity active γ-Al₂O₃ nanoparticles can be prepared with cubic in crystal system, O _H ⁷ -FD3M in space group, about 9 nm in crystal grain size, about 20 nm in particle size and uniform size distribution, 131. 35 m²/g in BET specific surface area, 7 – 11 nm in pore diameter, and not lower than 99.93% in purity. Foundation item: Project(03JJY3015) supported by the Natural Science Foundation of Hunan Province     

Decoioration and mineralization of yeast wastewater by using Ce-Fe/Al2O3 as heterogeneous photo-Fenton catalyst

Decoloration and mineralization of yeast wastewater were investigated by using Ce-Fe/Al2O3 as a heterogeneous photo-Fenton catalyst in fluidized bed reactor in order to solve the problem of yeast wastewater discharge. The experimental results were assessed in terms of total organic carbon（TOC） reduction. The operational and reaction conditions affecting the efficiencies of TOC removal such as initial pH value, H2O2 concentration, catalyst loading and UV power were studied. The results show that TOC is reduced from 347.6 mg/L to 10.8 mg/L, color is changed from 500 units to 0 under the conditions as follows： initial pH value 6. 0, H2O2 concentration of 1. 000 g/L, catalyst loading of 5 g/L, reaction duration of 120 rain and reaction temperature of 30 ℃. The irradiated Ce-Fe/Al2O3 catalyst was complexed with 1,10-phenanthroline and then it was subjected to Fourier transform infrared spectroscopy and diffuse reflectance spectroscopy to confirm the formation of Fe（Ⅱ） in the solid state. Heterogeneous photo-Fenton reaction proves to be effective for the treatment of yeast wastewater.     

Kinetics of Fe3O4 formation by air oxidation

The kinetics of Fe₃O₄ formation by air oxidation of slightly acidic suspension of Fe(OH)₂ was studied. The effects of initial concentration of Fe(II), temperature, partial pressure of oxygen, air flow rate and stirring rate on the oxidation rate were investigated. The results show that Fe₃O₄ formation is composed of two-step reaction, the first step is the formation of Fe(OH) ₂ ⁺ by oxidation of Fe(OH)⁺ complex ions, the second step is the formation of magnetite by dehydration and deprotonation of Fe(OH)⁺ and Fe(OH) ₂ ⁺ . The oxidation reaction is zero-order with respect to the concentration of Fe(II) and around 0.5-order with respect to partial pressure of oxygen, and oxygen transfer process is rate-limiting step of oxidation reaction with apparent activation energy of 2.74 kJ · mol⁻¹.     

Preparation of TiO2 photocatalyst loaded with V2O5 for O2 evolution

TiO₂ photocatalysts loaded with V₂O₅ were prepared via a modified hydrolysis process, and characterized by X-ray diffraction, transmission electron microscopy, Raman spectra and diffuse reflectance UV-Vis spectra measurements. The photocatalytic activity of V₂O₅/TiO₂ was investigated by employing splitting of water for O₂ evolution. The results indicate that V₂O₅ loading can pronouncedly improve the photocatalytic activity of TiO₂ with Fe³⁺ as an electron acceptor under UV or visible light irradiation. The optimum mass fraction of the loaded V₂O₅ is 8%, and the largest speed of O₂ evolution for 8%V₂O₅ (mass fraction) loaded TiO₂ catalyst is 118.2 μmol/(L·h) under UV irradiation, and 83.7 μmol/(L·h) under visible light irradiation.     

Effect of CaCO3 on hydration characteristics of C3A

Hydration products and morphology characteristics of C₃A (tricalcium aluminate)-CaCO₃-H₂O system were studied by means of XRD, DSC, FTIR spectrum analysis and SEM. The results indicate that, the new phases, i.e., C₃A·0.5CaCO₃·0.5Ca(OH)₂·11.5H₂O and C₃A·CaCO₃·11H₂O are found in this system due to the activity of CaCO₃; the formation of C₄AH₁₃ and C₂AH₈ is prohibited and the generation of C₃AH₆ is delayed in the early hydration process. C₃A·0.5CaCO₃·0.5Ca(OH)₂·11.5H₂O is not stable and will be totally transferred within 24 h; C₃A·CaCO₃·11H₂O exists stably once formation, and its flake-like crystalline phases in the early hydration transform to long rod shape, and to finally fine-needle at 28 d.     

三维电Fenton深度处理煤化工废水的催化反应机理

为进一步去除煤化工废水生化出水中残留的有机污染物,采用以剩余污泥和铁泥为原材料制备的SAC-Fe作为催化粒子电极构建三维电Fenton体系深度处理煤化工废水,对过程参数进行优化,并探讨催化反应机理.结果表明:制备的SAC-Fe对煤化工废水生化出水中的污染物具有较高吸附性能,单位COD吸附容量为101.1 mg/g;采用RSM优化的三维电Fenton过程参数为电流密度16.78 m A/cm2、Fe浓度14.75 mmol/L、p H 3.92,此时TOC去除率为67.12%;通过体系内H2O2和·OH生成量分析,结合吸附作用探讨三维电Fenton深度处理煤化工废水的催化反应机理,SAC-Fe表现出较高的(电)催化活性,显著提升三维电Fenton体系内H2O2和·OH的生成量和生成速率,吸附作用提高·OH利用率和污染物降解率,进而提升三维电Fenton深度处理煤化工废水的效能.     

Preparation, characterization and photocatalytic behavior of WO3-TiO2/Nb2O5 catalysts

TiO2/Nb2O5 photocatalyst loaded with WO3 (WO3-TiO2/Nb2O5) was prepared by a modified hydrolysis process, and characterized by X-ray diffractometry, transmission electron microscopy, Raman spectra and UV-Vis diffuse refraction spectroscopy. The photocatalytic activity of WO3-TiO2/Nb2O5 was investigated by employing splitting of water for O2 evolution. The results indicate that WO3 loading can pronouncedly improve the photocatalytic activity of TiO2/Nb2O5 by using Fe3 as an electron acceptor under UV irradiation. The optimum molar fraction of the loaded WO3 is 2%, and the largest speed of O2 evolution for 2% WO3-TiO2/Nb2O5 catalyst is 151.8 μmol/(L·h).     

Modification of nano-TiO2 by Al2O3 in-situ coating

A novel technology of in-situ coating Al₂O₃ on the surface of H₄TiO₄ was developed to prevent the aggregation of nano-TiO₂ powders and improve the dispersibility and thermal stability in the way of forming a uniform coating layer. The heterogeneous nucleation was conducted to prepare the precursor of nano-TiO₂ and then Al₂O₃ was coated on the surface of precursor. The effects of Al₂O₃ in-situ coating on the properties of nano-TiO₂ were investigated. The results show that H₄TiO₄ can be dispersed well under alkaline condition (pH 8.5) and the heterogeneous nucleation can be controlled easily. The optimized uniform coating layer is obtained by adding 5% (mass fraction) and 10% of Al₂O₃ and the aggregation of nano-TiO₂ powders is effectively inhibited and the dispersibility is obviously improved. The crystal sizes of TiO₂ powders are 12.3, 11.4 and 8.7 nm after coating 0,5% and 10% of Al₂O₃ respectively. Al₂O₃ on the surface of particulates in amorphous phase could increase the thermal stability of nano-particles after calcined at 550 °C. Foundation item: Project(04GK2007) supported by Hunan Industrial Key Project of Science and Technology     

Hydrothermal Synthesis and Characterization of a Novel Organic Inorganic Hybrid Compound [Co（dien）2]（dienH3）（H3O）7[P2Mo5O23]2·14H2O

A new compound,[Co（dien）2]（dienH3）（H3O）7[P2Mo5O23]2·14H2O, has been hydrothermallly synthesized by using Na2MoO4,CoCl2, H3PO4 and dien, and structurally characterized by elemental analysis, X-ray powder diffraction analysis, SEM, IR and TG analysis. The results show that the compound is composed of a polyanion [P2Mo5O23]2^12, complex [Co（dien）2]^2＋ cation, protonated [dienH3]^3＋ , and forteen crystallization water molecule.     

New technique of comprehensive utilization of spent Al2O3 -based catalyst

A new technology was developed to recover multiple valuable elements from the spent Al2O3-based catalyst by X-ray phase analysis and exploratory experiments. The experimental results show that in the condition of roasting temperature of 750 ℃ and roasting time of 30 min, molar ratio of Na2O to Al2O3 of 1.2, the leaching rates of alumina, vanadium and molybdenum in the spent catalyst are 97.2%, 95.8% and 98.9%, respectively. Vanadium and molybdenum in sodium aluminate solution can be recovered by precipitators A and B, and the precipitation rates of vanadium and molybdenum are 94. 8% and 92. 6%. Al（OH）3 was prepared from sodium aluminate solution in the carbonation decomposition process, and the purity of Al2O3 is 99. 9% after calcination, the recovery of alumina reaches 90. 6% in the whole process; the Ni-Co concentrate was leached by sulfuric acid, a nickel recovery of 98. 2% and cobalt recovery over 98.5% can be obtained under the experimental condition of 30% H2SO4, 80 ℃, reaction time 4 h, mass ratio of liquid to solid 8, stirring rate 800 r/min.