高铼酸的制备研究

以高铼酸铵为原料,分别采用50%TBP+50%260#溶剂油萃取法和C160树脂离子交换—真空旋转蒸发二步法制备高铼酸。结果表明,采用上述两种方法均可制得符合行业标准YS/T 836—2012要求的Ⅰ级高铼酸产品,其中萃取法铼回收率为97.47%,NH4+去除率高达99.993%;离子交换法铼损失率为0.035%,C160阳离子树脂对NH4+的穿透吸附容量为33.6g/L。     

AAS法测定纯铼中痕量元素K试验研究

用AAS法测定纯铼中的痕量元素K。通过优化原子吸收测量条件,研究了硝酸用量以及基体铼对测定K含量的影响,建立了AAS法测定纯铼中痕量元素K的分析方法。结果表明,AAS法测量K的相对标准偏差不大于9.04%,测定范围为0.0001%~0.001%,方法检出限为0.0035 μg/mL。本检测方法不仅准确可靠,而且简便快速。     

微量Re对93W-4.9Ni-2.1Fe合金性能及微观组织的影响

采用经高能球磨的超细93W-4.9Ni-2.1Fe预合金粉末，并添加少量的Re，经压制，烧结制取试样。研究Re对93W-4.9Ni-2.1Fe合金性能和微观组织的影响。用机械式拉力试验机测量试样拉伸强度，用扫描电镜观察试样拉伸断1：3的形貌，用金相显微镜对试样显微组织进行测试分析。结果表明：当添加0％-0．8％Re（质量分数，下同）时，随着Re添加量的增加，合金的相对密度稳定在99．43％～99．49％，烧结样品延伸率从不加Re时的26．47％降至0．8％Re时的14．71％，合金的抗拉强度由不加Re时的1025MPa增加到0．8％Re时的1142MPa，合金拉伸断口收缩率由不加Re时的20．45％降至0．8％Re时的10．91％；随着Re含量的增加，合金中W晶粒的穿晶解理断裂的比例增加，而粘结相延性断裂的比例减少；随着Re含量的增加，合金中W晶粒尺寸明显减小，由不加Re时的40μm-45μm减小到添加0．8％Re时的20μm-25μm。     

川北某黑色页岩型铼矿工艺矿物学研究

通过矿相显微镜、扫描电镜、电子探针、X射线能谱元素面分析等多种手段综合研究了川北某黑色页岩型铼矿中铼的赋存状态。样品为黑色页岩,有机碳含量较高。粘土矿物总量为14.6%,黄铁矿含量16.2%,石英含量37.7%。样品具典型的粘土结构,矿物粒度微细。铼有两种赋存状态,一种呈类质同象形式赋存于黄铁矿内,另一种则以分散形式存在。典型黄铁矿测点Re平均含量为0.024%。黄铁矿是Re的重要载体矿物。建议通过浮选分离黄铁矿,从而实现Re的富集。     

The Effect of Sintering on the Properties of Ultrafine

研究了一种化学气相沉积(CVD)制备超细铼粉的新方法,即以NH4ReO7为原料,通过将其分解为Re2O7后气相输运至还原区,经氢气还原生成超细铼粉。对不同还原温度下制备的超细铼粉样品,采用XRD、SEM、激光粒度分析进行表征,实验揭示了烧结作用对晶粒尺寸、形貌、表面状态及粒度等粉末性能的影响规律。结果表明,随还原温度升高,烧结作用增强,制备的超细铼粉晶粒尺寸增大,具有更好的球形度,表面趋于光洁,平均粒径增大。     

Oxorhenium-mediated assembly of noncyclic selective integrin antagonists: a combinatorial approach

The parallel oxorhenium-mediated assembly of 288 noncyclic RGD analogues is reported. All complexes contain a NS(2) +S chelating motif that enables the unambiguous coordination of the oxorhenium and oxotechnetium cores. In this study, "modules S" contain a variety of pending guanidinium groups whereas the "NS(2) modules" are made of a series of N-acylated amino acids. Combination of sets of "NS(2) " and "S modules" together with tetrabutylammonium tetrachlorooxorhenate gave the corresponding oxorhenium complexes in good yields and satisfactory purities. Evaluation of these metalloconstructs towards integrins α(V) β(3) , α(IIb) β(3) , and α(V) β(5) led to the identification of micromolar and submicromolar antagonists of theses integrins. These compounds exhibit interesting selectivities and promise attractive applications for the molecular imaging of integrin-dependent pathologies.     

铬黑T-溴酸钠催化动力学分光光度法测定铼

基于在硫酸介质中,铼催化溴酸钠氧化铬黑T的褪色反应,建立了测定铼的光度分析新方法。确定了催化体系的动力学条件,计算得出催化反应的表观活化能Ea=39.12KJ/mol,反应速率常数为K=1.248×10-3/s。在选定的试验优条件下,铼的浓度在0~10.02mg/L范围内与相对吸光度呈良好的线性关系,检出限为2.7675mg/L。方法所用仪器简单,操作简便。     

Dehydrogenation of Light Alkanes Over Rhenium Catalysts on Conventional and Mesoporous MFI Supports

Recently, Re/HZSM-5 (Si/Al = 15) was shown to be an efficient catalyst for ethane dehydrogenation and aromatization at 823 K and atmospheric pressure. In this reaction, the major initial products were benzene, toluene and xylene (BTX), but increasing amounts of ethene were produced with time on stream due to deactivation of the catalyst. We show that by use of rhenium impregnated MFI supports with very few or no acidic sites (Si/Al > 500), highly selective ethane dehydrogenation catalysts are obtained with ethene selectivities of 98%. By use of mesoporous MFI supports (Si/Al >500) the lifetime of the catalyst appears to be slightly improved compared to conventional MFI crystals. The beneficial effect of a mesoporous MFI support is convincingly demonstrated in propane dehydrogenation, where both conversion and selectivities on the mesoporous MFI (Si/Al > 500) impregnated with Re are significantly higher than on Re supported on a comparable conventional MFI support.     

The Effect of Water on the Activity and Selectivity for γ-Alumina Supported Cobalt Fischer–Tropsch Catalysts with Different Pore Sizes

The effect of water on the activity and selectivity for a series of γ-Al₂O₃ supported cobalt Fischer–Tropsch catalysts has been studied in an isothermal fixed-bed reactor at T = 483 K, P = 20 bar, and H₂/CO = 2.1. The catalysts were produced applying incipient wetness impregnation and consisted of 20 wt.% cobalt and 0.5 wt.% rhenium deposited on γ-Al₂O₃ supports with different pore characteristics. For the narrow-pore catalysts, addition of water corresponding to an inlet partial pressure ratio of P_H2O/P_H2 = 0.4 reduced the reaction rates. In contrast, for a catalyst with larger pores the same water pressure increased the reaction rates. For all catalysts, water amounts equal to P_H2O/P_H2 = 0.7 at the reactor inlet suppressed the reaction rates and led to permanent deactivation. The addition of water increased the C₅₊ selectivity and decreased the CH₄ selectivity for all catalysts. The pore characteristics seem to determine the effect of water on the rates.