从沉钨钼后液中制备高纯铼酸铵

利用沉钨钼后液首先经氯化钾沉淀反应得到铼酸钾,其次采用离子交换法将铼酸钾溶液转为高铼酸溶液,最后经氨水中和-浓缩结晶-重结晶得到高纯铼酸铵。结果表明:向沉钨钼后液中加入KCl固体再浓缩析出KReO₄白色晶体,其主要杂质Na、Ca、Fe、Cl含量均小于1.00%,特别是W、Mo含量均小于0.10%,且Re结晶率可达94.92%～98.38%。采用动态法脱K,选用C160(H⁺型)树脂,当KReO₄溶液pH为中性,料液流速控制在2BVs·h^-1时,C160树脂对K⁺穿透容量和饱和容量分别为117.87和128.39g·L^-1,且树脂利用率达到91.81%;所得纯HReO₄溶液中K、Na、Ca、Fe、W、Mo、Mg浓度均降至0.50 mg·L^-1以下。通过添加优级纯氨水中和HReO₄溶液,控制终点pH为7～8,再经浓缩结晶+1次重结晶,所得铼酸铵纯度达到99.99%以上,其SEM形貌为树枝状。     

Purolite A172树脂对铼和钼的静态分离

针对目前溶液体系中铼和钼分离困难的问题,通过树脂选型确定选用中强碱性阴离子交换树脂Purolite A172分离铼和钼,研究A172树脂对铼的吸附性能和对铼-钼的分离性能。结果表明:A172树脂吸附铼的反应为放热反应,而且吸附速率很大,吸附速率常数k_(298 K)=7.719×10~(-4) s~(-1),受内扩散控制,树脂对铼的静态饱和吸附容量达到340.13 mg/g湿树脂;当铼溶液pH=9、摇床往复震荡速率110 r/min、摇床水浴温度25℃、吸附时间1 h时,树脂对铼的吸附量最大;当以浓度为2 mol/L硫氰酸铵为解吸剂,在溶液pH=5、摇床往复震荡速率150 r/min、摇床水浴温度50℃下解吸5 h时,铼的解吸率最高,达到99.19%。大量的钼会阻碍铼的吸附,但随着吸附时间的延长,被吸附的钼逐渐被铼取代,铼和钼的分离因数最大值达到1192;解吸时,负载的钼对铼的解吸也有抑制作用,随着钼铼质量比的增加,铼的解吸率降低。     

铼酸铵提纯技术研究

采用紫外光照+离子交换组合工艺提纯铼酸铵，并在离子交换前预热铼酸铵溶液及离子交换树脂柱。采用电感耦合等离子体发射光谱仪(ICP-MS)测定杂质元素质量分数。讨论了紫外光照、紫外光照时间、预热温度、预热时间等工艺对铼酸铵中金属杂质质量分数的影响。研究表明：采用紫外光照2 h，预热温度60°C，预热时间0.5 h后进行离子交换提纯后的铼酸铵纯度最佳，Be、Mg、Al、Ca、Ti、Cr、Mn、Co、Cu、Zn、Mo、Pb、W、Sn、Ni、Sb、Bi、Tl等元素杂质质量分数均在1×10^-6以下，铼酸铵纯度>99.99%。     

银离子在斛壳丹宁酸树脂表面的吸附和解吸(英文)

将斛壳丹宁酸与甲醛聚合来形成的凝胶作为吸附剂能有效地移去水溶液中的银离子。研究了不同银离子初始浓度、溶液温度、pH值条件下斛壳丹宁酸树脂的附和解吸行为。研究了有关经验动力学模型的适应性。伪二级动力学模型表明银离子的吸附是很快的。用FTIR和SEM对吸附和解吸银离子后的斛壳彤宁酸和斛壳丹宁酸树脂进行表征。银离子在斛壳宁酸树脂上的吸附随着银离子初始浓度的增加而增加,随着溶液温度的升高而减少。在低pH值的H2SO4、HNO3和HCl溶液中进行解吸实验。斛壳丹宁酸树脂在pH2.0~7.0溶液中对银离子表现出高的吸附容量,在银离子初始浓度100.0mg/L、温度296K和pH5.0的条件下达到最大的吸附量97.08mg/g。在1mol/LHCl+1%硫脲溶液中银离子的脱吸率达99.6%。     

血液灌流抢救超大剂量地高辛中毒

目的: 观察1例血液灌流抢救超大剂量( 50mg)地高辛中毒的效果。方法: 使用HA 330 ml 灌流器和YT-160 灌流器, 血管通路为股静脉单针双腔导管。入院后共进行了4 次血液灌流( HP) 治疗。结果: 第1 次HP 前后检测地高辛血药浓度均16 μg·L^-1。第2 次HP 血药浓度9. 22 μg·L^-1。第3 次HP 前血药浓度12. 4 μg·L^-1, HP 后为10. 45 μg·L^-1。第4 次HP 前3. 22 μg·L^-1, HP 后为2. 84 μg·L^-1。结论: 采用间隔一定的时间HP, 多次进行, 可阶梯式降低药物浓度。     

离子交换树脂法吸附、解吸钯工艺研究

用9335型阴离子交换树脂吸附经王水溶解的含钯物料,可以选择性吸附钯,铜、镍等杂质不被吸附。用8%氨水、40 g/L氯化铵解吸,98%以上的钯被解吸。吸附操作简单,解吸后的树脂可重复使用。     

季铵功能化NH2-MIL-101(Fe)吸附氰化钯性能

制备了一种新型季铵功能化金属有机框架(MOFs)材料Et-N-NH₂-MIL-101(Fe),用于氰化钯的吸附，采用红外光谱、扫描电镜等对其吸附Pd(CN)₄^2-特性进行了表征。吸附热力学表明吸附为放热反应，且能自发进行。Et-N-NH₂-MIL-101(Fe)对Pd(CN)₄^2-的吸附过程符合准二级动力学和Langmuir模型，采用2.0 mol·L^-1KI溶液洗脱Et-N-NH₂-MIL-101(Fe)上吸附的Pd(CN)₄^2-,洗脱率大于97.0%。5次循环后Pd(CN)₄^2-的回收率大于91.0%。研究表明，Et-N-NH₂-MIL-101(Fe)在中性介质中稳定性良好，对Pd(CN)₄^2-具有快速优良的吸附能力。     

盐酸特比萘芬溶液的透皮吸收

目的: 观察1 %盐酸特比萘芬溶液经皮肤给药后药物在体内的吸收性和蓄积性。方法: 6 只新西兰大白兔, 每兔皮肤单次涂药液8 ml·d^-1, 收集24 h 内药时血样。随后连续涂药液7 d, 收集每日峰、谷浓度血样, 用高效液相色谱(HPLC) 测定兔血清特比萘芬血药浓度。结果: 药物透皮吸收3 h C_max 8. 3 ±3. 7 μg·L^-1, 随着血药浓度下降维持一个较低水平。连续7 d, 药峰浓度在d 3 达10. 5 ± 3. 0 μg·L^-1, 随后数日峰浓度维持于一平台水平, 谷浓度无明显变化。结论: 1 %盐酸特比萘芬溶液没有体内累积现象。     

LC-MS 法测定Beagle 犬血浆中苦参碱及其药代动力学

目的: 建立Beagle 犬血浆中苦参碱的LC-MS测定法, 测定其药物动力学及绝对生物利用度。方法: 采用Lichrospher C18 柱, 250 mm×4.6 mm(ID),5 μm, 柱温:25 ℃;流动相:10 mmol·L^-1醋酸胺水溶液∶甲醇(25 ∶75), 流速:1 ml·min^-1 。电喷雾离子化(ESI) 方式, 采用选择性离子检测, 检测离子为正离子, 苦参碱的离子是[M+H] +, m/z 249.2 。结果: 苦参碱在2～5 000 μg·L^-1的范围内呈良好的线性关系(r=0.9975), 最低检出限达0.3 μg·L^-1。日内和日间误差均小于4.5 %, 方法回收率大于96.6 %;药-时数据符合二室模型, C_max 为3821±705 μg·L^-1, T_max为0.4±0.1 h, T_1/2β为11.2±2.1 h,AUC_0→∞为7446±1456 μg·h·L^-1, 绝对生物利用度为(60.1±19.0) %。结论: 该法灵敏、快速、简单, 专属性强, 苦参碱在Beagle 犬体内有较高的绝对生物利用度。     

HPLC-MS法测定Beagle犬血浆中氧化苦参碱及其药代动力学

目的: 建立Beagle犬血浆中氧化苦参碱的LC-MS测定法,测定它的绝对生物利用度。方法: Beagle犬6只,随机分为2组,采用单剂量双周期自身交叉设计,分别给犬单剂量静脉注射或灌胃氧化苦参碱,用LC-MS法测定给药后的血浆中药物浓度。结果: 氧化苦参碱在2～5000μg·L^-1的范围内呈良好的线性关系(r=0.9990),最低检出限达0.6μg·L^-1,日内和日间误差均小于4.2 %,方法回收率大于96.7 %;氧化苦参碱的药-时数据符合二室模型,C_max为2.42±0.97μg·L^-1,T_max为1.0±0.3 h,T_1/2β为5.54±1.58h,AUC_0→∝为6.12±1.08μg·L^-1·h^-1,绝对生物利用度为(19.4±9.01)%。结论: 该法灵敏、简单,专属性强;氧化苦参碱在Beagle犬体内绝对生物利用度较低。     

Recovery of V<Subscript>2</Subscript>O<Subscript>5</Subscript> from Bayer liquor by ion exchange

A new technology was developed to recover V2O5 from Bayer spent liquor by ion exchange.The experimental results show that in the conditions of 105°C and 0.20-0.25 mass ratios between CaO in lime and Al2O3 in spent liquor, the precipitation rate of vanadium in Bayer liquor is more than 85%.The vanadium-bearing precipitation is leached by NaHCO3 solution.The leaching rate of vanadium can reach 85% in the conditions of 95°C, 40 g·L-1 of NaHCO3 concentration, and ventilating of CO2.The 201 × 7 type of resin has...     

Recovery of rhenium from tungsten‑rhenium wire by alkali fusion in KOH-K2CO3 binary molten salt

Tungsten‑rhenium wire is used in thermocouple and lamp filament manufacturing due to its good thermal sensitivity and high temperature plasticity, and many waste wires are generated in processing and after use. This work focuses on the efficient recovery of high value rhenium from tungsten‑rhenium wire waste with a mass composition represented by W95Re5. The main steps for recovery include alkali fusion, recrystallization, hydrogen reducing and washing. First, WRe wire was decomposed by KOH-K₂CO₃ molten salt to produce potassium perrhenate, where the decomposition ratios of W and Re reached 99.36% and 99.80% using a mass ratio of salt to wire of 3:1, m(KOH) of 80% (m representing the mass fraction of KOH in binary salt), a temperature of 800 °C and a reaction time of 60 min. Then, the decomposed product was leached by water, and from the resulting lixivium high purity KReO₄ crystals were obtained by segregation, which had a perfect rhombic dipyramid morphology and average size of 73.26 μm. Last, the material was reduced to Re powder at 350 °C with a H₂ flow rate of 10 L/min. Re powder, with a purity of higher than 99.5% and fine grain size of 19.37 μm, was obtained after washing with acid and water. This method provided a potential economic process for the recovery of waste WRe wire.     

Selectivity recovery of molybdenum(VI) from rhenium(VII) by amine-modified persimmon waste

Amine functional group was grafted to obtain modified persimmon waste gel(NH_2–CPT) with the focus of development of selective recovery of molybdenum from rhenium. The adsorption behavior of the NH_2–CPT gel for various metal ions at varying hydrochloric acid concentrations was studied. It is found that the NH_2–CPT exhibits high affinity for Mo(VI) and no affinity for Re(VII), Cu(II),Fe(III), Mn(VII), and Zn(II) under the operating conditions. The maximum adsorption capacity for Mo(VI) is 172 mgág-1, and the adsorption behavior obeys the Langmuir model. Owing to Mo(VI) as poly-anions, the adsorption mechanism of molybdenum anions could be explained as the anion exchange reactions at weak acid concentration, while neutral molecules could be explained as the complexation reactions at strong acid concentration,respectively. In addition, its excellent adsorption characteristics for Mo(VI) are confirmed by separation of Mo(VI)from Mo to Re containing industrial effluent.     

Sb(V) removal from copper electrorefining electrolyte: Comparative study by different sorbents

Removal of Sb(V) from copper electrolyte by different sorbents such as activated carbon, bentonite, kaolin, resin, zeolite and white sand was investigated. Adsorption capacity of Sb(V) removal from copper electrolyte was as follows: white sand < anionic resin < zeolite < kaolin < activated carbon < bentonite. Bentonite was characterized using FTIR, XRF, XRD, SEM and BET methods. The results show specific surface area of 95 m²/g and particles size of 175 nm for bentonite. The optimum conditions for the maximum removal of Sb are contact time 10 min, 4 g bentonite and temperature of 40 °C. The adsorption of Sb(V) on bentonite is followed by pseudo-second-order kinetic (R²=0.996 and k=9×10^?5 g/(mg·min)). Thermodynamic results reveal that the adsorption of Sb(V) onto bentonite from copper electrolyte is endothermic and spontaneous process (ΔG^Θ=–4806 kJ/(mol·K). The adsorption data fit both the Freundlich and Langmuir isotherm models. Bentonite has the maximum adsorption capacity of 10000 mg/g for adsorption of Sb(V) in copper electrolyte. The adsorption of Zn, Co, Cu and Bi that present in the copper electrolyte is very low and insignificant.     

酒石酸对电解法制备树枝状超细银粉的影响研究

采用电解法制备树枝状银粉,研究了酒石酸对银粒子电化学沉积过程的形貌演变和生长机制的影响。通过SEM、TEM和XRD分析了酒石酸对沉积过程银粉的形貌和结构的影响。此外,利用阴极极化(LSV)、循环伏安(CV)和计时电流(CA)探究了酒石酸对电解法制备树枝状银粉的电化学行为影响规律。结果表明：当溶液中添加0 g/L酒石酸时,银离子在850A/m2电流密度下形成类球状结构,而当溶液中添加0.05g/L酒石酸时,银离子在相同电流密度下形成棒状结构,随着酒石酸添加量的增加,阴极极化程度增加,过电位增大。而当酒石酸增加到0.5 g/L时,成功制备出粒径3～4μm,松装密度1.1 g/cm³,振实密度0.6 g/cm³、结晶性好的树枝状银粉。计时电流结果表明溶液体系均遵循瞬时成核过程,但添加酒石酸影响了银的成核和生长动力学,并抑制了阴极极化。     

Preparation of pure SbCl3 from lead anode slime bearing high antimony and low silver

A novel treatment process of lead anode slime bearing high antimony and low silver was developed by a potential-controlled chloridization leaching and continuous distillation.The experimental results show a high Sb 3+ concentration,489.2 g/L,in the leaching solution for two-stage countercurrent leaching process,and the leaching rates of Sb,Cu,Bi more than 99% when the potential is controlled at 450 mV.When the leaching solution is distillated and concentrated at 120°C,almost all the silicon compound is evaporated into the concentration distillate and exists as amorphous hydrated silica.By the continuous distillation,high pure SbCl3 could be prepared,and AsCl3 is enriched in the distillate while metals Bi,Cu are enriched in the continuous distillation residue.As a result,the recovery rate of Sb is more than 95%.     

Removal of vanadium from ammonium molybdate solution by ion exchange

The separation techniques of vanadium and molybdenum were summarized, and a new method of removal V(Ⅴ) from Mo(Ⅵ) by adsorption with chelate resin was presented. Nine kinds of chelate resins were used to investigate the adsorbent capability of V(Ⅴ) in ammonium molybdate solution with static method. The test results show that DDAS, CUW and CW-2 resins can easily adsorb V(Ⅴ) in ammonium molybdate solution, but hardly adsorb Mo(Ⅵ). The dynamic experimental results show more than 99.5% of V(Ⅴ) can be adsorbed, and the adsorption rate of Mo(Ⅵ) is less than 0.27% at 294-296 K for 60 min at pH 7.42-8.02. The mass ratio of V to Mo decreases to l/5 0000 in the effluent from 1/255 in the initial solution. The loaded resin can be desorbed by 5% NH3·H2O solution, and the vanadium desorption rate can reach 99.6%. The max concentration of vanadium in desorbed solution can reach 20 g/L, while the concentration of molybdenum is less than 0.8 g/L.     

Adsorption behavior and mechanism of amino methylene phosphonic acid resin for Ag（ Ⅰ ）

1 Introduction Many efforts have been made on using ion exchange resin to separate and concentrate certain metal cations [1?11]. However, less research for using it to adsorb noble metal Ag(Ⅰ), and much less research for commercializa- tion has been don…     

Recycling of rhenium-containing wire scrap

Rhenium is a refractory metal and is one of the rarest elements. Due to its high cost, recycling of rhenium-containing scraps is of economic interest. This paper pertains to the recycling of rhenium from tungsten–rhenium wire scrap generated in the manufacturing of W₉₇Re₃ wire. Rhenium from wire scrap, which contained 3.1–3.4% Re, was volatilized at 900 °C in the presence of air at 2 L/min in a tube furnace according to the following equation: 4Re + 7O₂ → 2Re₂O₇ (g). Volatilized Re was solidified on the inner surface of the tube and was recovered as ammonium perrhenate (NH₄ReO₄) solution after washing the tube with dilute ammonium hydroxide solution (Re₂O₇ + 2NH₄OH → 2NH₄ReO₄ + H₂O). Ammonium perrhenate solution was crystallized to obtain ammonium perrhenate crystals which were free of tungsten and other metal impurities. First pass yield of rhenium recovery was 65.1%. Ammonium perrhenate crystals were reduced in hydrogen at 400–700 °C to obtain Re-metal powder: (2NH₄ReO₄ + 7H₂ = 2Re + 8H₂O + 2NH₃₎. Rhenium metal powder obtained from the W–Re wire scrap was blended with non-sag tungsten powder to make a 6 kg W₉₇Re₃-alloy ingot which was rolled to make tungsten–rhenium wire. Results presented in this paper were intended for developing a commercial process for the recycling of a large inventory of W–Re wire scrap.