Fe掺杂SUZ-4催化剂制备及其SCR反应活性

在添加晶种和有机模板剂条件下,采用两步溶胶-凝胶法,酸环境下共水解正硅酸乙酯和金属盐,合成得到骨架Fe-SUZ-4分子筛。通过紫外可见漫反射表征证明Fe成功嵌入分子筛的四配位骨架上。Fe-SUZ-4分子筛催化剂在NH_3-SCR脱硝反应中表现出优异的催化性能,其催化活性显著高于离子交换法和浸渍法制备的含Fe分子筛催化剂。结果表明,凝胶配比为n(TEAOH)∶n(KOH)∶n(Al_2O_3)∶n(SiO_2)∶n(H2O)=1.0∶10∶1∶22.5∶500,晶种质量分数为1%,n(Fe)∶n(Si)=0.005~0.02,随着Fe含量的增加,Fe-SUZ-4分子筛晶化时间略有延长,且结晶度略降。NH_3-SCR脱硝反应中,Fe-SUZ-4分子筛催化剂最适宜的金属含量为n(Fe)∶n(Si)=物质的量比0.01,反应温度约350℃时,NO转化率达到100%。而通过离子交换法和浸渍法合成得到的含Fe分子筛催化剂用于SCR反应,NO转化率达到100%时,反应温度均有提高。     

Synthesis of sub-micrometer lithium iron phosphate particles for lithium ion battery by using supercritical hydrothermal method简

A supercritical hydrothermal method was employed to prepare sub-micrometer LiFePO4 particles with high purity and crystallinity. The structure and morphology of LiFePO4 particles were characterized by X-ray diffraction and scanning electron microscope. The electrochemical tests were carried out to determine the reversible capacity, rate and cycling performance of the LiFePO4 particles as cathode material for lithium ion battery. Experimental results show that solvent and calcining time have significant effects on purity, size and morphology of LiFePO4 particles. Mixed solvent contained deionized water and ethanol is conducive to synthesize smaller and more uniform particles. The size of LiFePO4 particles as-prepared is about 100-300 nm. The specific discharge capacities of the LiFePO4 particles are 151.3 and 128.0 mA. h. g-1 after first cycle at the rates of 0.1 and 1.0 C, respectively. It retains 95.0% of the initial capacity after 100 cycles at 1.0 C.     

Synthesis of Pd（C4H2O4）（C4H8N2）0.5 Complex and the Catalytic Activity for Oxidative Carbonylation of Phenol

A novel complex Pd（C4H2O4）（C4H8N2）0.5 has been synthesized by solvent thermal synthesis and used as a heterogeneous catalyst for direct synthesis of diphenyl carbonate （DPC） by oxidative carbonylation of phenol. In the reaction system of Pd（C4H2O4）（C4H8N2）0.5/Cu（OAc）2/ tetrabutylammonium bromide/ hydroquinone/ 4A molecular sieves, the effect of reaction temperature, time and CO pressure on catalytic activity were investigated, and the results revealed that the catalyst could catalyze oxidative carbonylation of phenol effectively. Under suitable reaction conditions of T=90℃, t=4 h, p（O2）=0.3 MPa, p（CO）=3.9 MPa and CH2Cl2 as solvent, the turnover number （TON） of diphenyl carbonate can reach about 13.50 （mol-DPC/mol-Pd）, which is higher than the TON for oure PdCl2 under the same reaction conditions.     

Synthesis of magnetic core-shell structure Fe3O4@MCM-41 nanoparticle by vesicles in aqueous solutions☆

In this study, magnetic core–shel structure Fe3O4@MCM-41 nanoparticles were synthesized with vesicles as soft templates. In the preparation, FeCl2 and tetraethy orthosilicate (TEOS) were selected as Fe processor and Si pre-cursor, respectively. Stable vesicles first formed in 0.03 mol·L?1 1:2 mixture of anionic surfactant sodium dode-cyl sulfate and cationic surfactant cetyltrimethyl ammonium bromide. Then, TEOS was added in the vesicle aqueous solution, leading to a highly dispersed solution. After high-temperature calcination, Fe3O4@MCM-41 nanoparticles were obtained. Their structure and morphology were characterized by Saturn Digisizer, transmis-sion electron microscope and vibrating sample magneto-meter. The results indicate that the vesicles are spherical and their size could be tuned between 20 and 50 nm. The average grain diameter of synthesize magnetic core–shel Fe3O4@MCM-41 particles is 100–150 nm and most of them are in el iptical shape. The dispersion of magnet-ic particles is very good and magnetization values are up to 33.44 emu·g?1, which are superior to that of other Fe3O4 materials reported.     

Synthesis of 4-ethyl-α-methylbenzenemethanol and α,α'-dimethyl-1,4-benzenedimethanol

研究了一种以对二乙苯为原料,经四苯基氯化钴卟啉催化氧气氧化、硼氢化钠还原、水解合成标题化合物的新方法,并采用熔点测定、红外及核磁共振对目标产物的结构进行了表征,产品分离总收率较高,分别达57.B％和52.3％,纯度均达到了99.5％.该合成方法反应条件相对温和,简便易行.     

Synthesis of hierarchical dendritic micro–nano structure ZnFe_2O_4 and photocatalytic activities for water splitting

Hierarchical dendritic micro–nano structure Zn Fe_2O_4 have been prepared by electrochemical reduction and thermal oxidation method in this work. X-ray diffractometry, Raman spectra and field-emission scanning electron microscopy were used to characterize the crystal structure, size and morphology. The results show that the sample(S-2) is composed of pure ZnFe_2O_4 when the molar ratio of Zn~(2+)/Fe~(2+)in the electrolyte is 0.35. Decreasing the molar ratio of Zn~(2+)/Fe~(2+), the sample(S-1) is composed of ZnFe_2O_4 and α-Fe_2O_3, whereas increasing the molar ratio of Zn~(2+)/Fe~(2+), the sample(S-3) is composed of ZnFe_2O_4 and Zn O. The lattice parameters of ZnFe_2O_4 are influenced by the molar ratio of Zn~(2+)/Fe: Zn at excess decreases the cell volume whereas Fe at excess increases the cell volume of Zn Fe_2O_4. All the samples have the dendritic structure, of which S-2 has micron-sized lush branches with nano-sized leaves. UV–Vis diffuse reflectance spectra were acquired by a spectrophotometer. The absorption edges gradually blue shift with the increase of the molar ratio of Zn~(2+)/Fe~(2+). Photocatalytic activities for water splitting were investigated under Xe light irradiation in an aqueous olution containing 0.1 mol·L~(-1)Na_2S/0.02 mol·L~(-1)Na_2SO_3 in a glass reactor. The relatively highest photocatalytic activity with 1.41 μmol·h-1· 0.02 g~(-1)was achieved by pure ZnFe_2O_4sample(S-2). The photocatalytic activity of the mixture phase of Zn Fe_2O_4 and α-Fe_2O_3(S-1) is better than ZnF e_2O_4 and ZnO(S-3).     

Influence of MgF2 Coating on Water Resistance of SrAl2O4：Eu^2＋,Dy^3＋

采用液相沉积法在发光粉 SrAl2O4：Eu2＋,Dy3＋表面包覆了 MgF2膜。借助酸度仪、X 射线衍射仪、扫描电子显微镜和荧光分光光度计等分析手段对粉体包覆前后的物相组成、表面形貌和能谱、耐水性能、激发和发射光谱及余辉性能进行了表征。结果表明：包覆 MgF2后样品的物相未发生改变,粉体表面变得粗糙,耐水性能显著提高;包覆样品的发射光谱和激发光谱峰的位置未发生改变,但相对强度随包覆量的增加而降低;初始亮度和余辉时间随包覆量的增加亦呈减小的趋势。综合考虑耐水性能、光谱性能和余辉性能的要求,选取 MgF2最佳包覆量为 25%     

Direct synthesis of single-phase α-CaSO4·0.5H2O whiskers from waste nitrate solution

Single-phase α-CaSO₄·0.5H₂O whiskers were directly synthesized from waste Ca(NO₃)₂ solution using a hydrothermal method, and HNO₃ was synchronously regenerated. The effects of reaction temperature and Ca²⁺ concentration on the phase composition and morphology of products were determined by X-ray diffraction and optical microscopy. On the basis of the experimental results, the formation diagram of α-CaSO₄·0.5H₂O was plotted within the range of 5-35 g·L^-1 Ca²⁺ and 115℃-150℃. In addition, the conditions of the direct synthesis of α-CaSO₄·0.5H₂O were determined. Well-crystallized, single-phase α-CaSO₄·0.5H₂O whiskers with high aspect ratios (length, 1785 μm; diameter, 10.63 μm; aspect ratio, 168) and HNO₃ (70.25 g·L^-1) were obtained at the optimal conditions of 25 g·L^-1 Ca²⁺ and 125℃.     

碳酸锶原料对合成SrAl2O4:Eu,Dy发光材料的影响

通过TG-DSC和XRD分析,对合成SrAl2 O4:Eu,Dy发光材料所用碳酸锶原料形貌及合成过程中的变化特征展开研究.研究结果表明,碳酸锶原料影响SrAl2 O4:Eu,Dy余辉发光性能的主要因素是原料的颗粒粒度和形貌.由于原料微观结构的不同,导致加热到900℃以上发生热分解的过程不同,合成过程中与氧化铝的反应表面面积和活性也不同,从而影响合成过程中锶离子和其他稀土掺杂离子的扩散,导致发光材料的结构和性能的差异.研究的几种碳酸锶原料中,采用平均粒径0.8μm的原料制得的产物发光性能最好.     

Synthesis and Luminescence Properties of Red Long Afterglow Phosphor Y2O2S：Eu3＋,Mg2＋,Ti4＋by Sol-Gel Process

以金属硝酸盐和钛酸丁酯为原料,乙酰丙酮为螯合剂,采用溶胶–凝胶法制备了 Y2O2S：Eu3＋,Mg2＋,Ti4＋红色长余辉发光粉体。采用 X 射线衍射仪、扫描电子显微镜和荧光分光光度计对不同温度合成的样品性能进行测试与表征。结果表明：干凝胶在 600 ℃保温 2 h 生成了立方相的前驱体Y2O3：Eu3＋,Mg2＋,Ti4＋。前驱体在 1050～1150 ℃硫化后的产物为 Y2O3与 Y2O2S 的混合相,在 1 200 ℃时,硫化生成纯相的 Y2O2S：Eu3＋,Mg2＋,Ti4＋,产物平均粒径约为 150nm,1300 ℃时再次出现 Y2O3相。与高温固相法相比,溶胶–凝胶法制备的样品主激发峰出现蓝移,主发射峰位于 616nm 和 626nm处,对应于 Eu3＋的5D0→7F2跃迁;硫化温度为 1200 ℃时,样品的余辉时间为 40min。