High-efficiency trace Na extraction from crystal quartz ore used for fused silica-——A pretreatment technology

Trace Na sources, extraction dynamics of trace Na, and influences of calcination temperature on quartz lattice, fluid inclusions, and muscovite were studied in detail herein for trace Na extraction from the quartz ore with water leaching at 90℃. Experimental results suggested that the trace Na sources included quartz lattice, fluid inclusions, and muscovite. The extraction rate of the trace Na in quartz ores can reach 31.0wt% after calcination at 900℃ for 5 h and water leaching at 90℃ for 24 h. The extraction process consisting of the dissolution of unfree Na and diffusion of free Na was dominated by calcination temperature. Calcination at 900℃ for 5 h was effective for extraction of the trace Na in fluid inclusions and muscovite. The extraction of the trace Na was mainly affected by the decrepitation of fluid inclusions when the calcination temperature ranged from 400 to 600℃ and by the damage of muscovite when the calcination temperature ranged from 600 to 900℃. Based on the extraction rates at different calcination temperatures, approximately 20.1wt% of the trace Na occurred in fluid inclusions, approximately 10.9wt% existed in muscovite, and 69.0wt% mainly occurred in quartz lattice.     

Comparison of the mechanisms of microwave roasting and conventional roasting and of their effects on vanadium extraction from stone coal

Experiments comparing microwave blank roasting and conventional blank roasting for typical vanadium-bearing stone coal from Hubei Province in central China, in which vanadium is present in muscovite, were conducted to investigate the effects of roasting temperature, roasting time, H₂SO₄ concentration, and leaching time on vanadium extraction. The results show that the vanadium leaching efficiency is 84% when the sample is roasted at 800℃ for 30 min by microwave irradiation and the H₂SO₄ concentration, liquid/solid ratio, leaching temperature, and leaching time are set as 20vol%, 1.5:1 mL·g-1, 95℃, and 8 h, respectively. However, the vanadium leaching efficiency achieved for the sample subjected to conventional roasting at 900℃ for 60 min is just 71% under the same leaching conditions. Scanning electron microscopy (SEM) analysis shows that the microwave roasted samples contain more cracks and that the particles are more porous compared to the conventionally roasted samples. According to the results of X-ray diffraction (XRD) and Fourier-transform infrared (FTIR) analyses, neither of these roasting methods could completely destroy the mica lattice structure under the experimental conditions; however, both methods deformed the muscovite structure and facilitated the leaching process. Comparing with conventional roasting, microwave roasting causes a greater deformation of the mineral structure at a lower temperature for a shorter roasting time.     

Characteristics and evolution of ore-forming fluids of the Chongjiang copper deposit in the Gangdise porphyry copper belt,Tibet

Petrography, microthermometry, and scanning electron microscope/energy dispersive spectrometer (SEM/EDS) studies were performed on the fluid inclusions in the ore-beating quartz veins and quartz phenocrysts in the porphyry of the Chongjiang porphyry copper deposit. The analyses of the fluid inclusions indicate that the ore-forming fluids were exsolved from magma. They are near-saturated, supercritical, rich in volatile constituents, and have the capture temperature of 362-389℃ and salinities of 17.7wt%- 18.9wt% NaC1 eq. With the decreasing of temperature and pressure, the supercritical fluids were separated into a low salinity vapor phase and a high salinity liquid phase. During quartz-sericitization, the high salinity fluid boiled and separated into a low salinity vapor phase and a high salinity liquid phase. The high salinity inclusions that formed in the boiling process had daughter mineral melting temperatures higher than the homogenization temperatures of the vapor and liquid phases. The late fluids that are responsible for argillization are of lower temperature and salinity.     

Chlorination roasting-coupled water leaching process for potash recovery from waste mica scrap using dry marble sludge powder and sodium chloride

The present paper reports the effective utilization of marble sludge powder(MSP) for the recovery of potash values from waste mica scrap using chlorination roasting–water leaching method. Characterization studies indicated the presence of dolomite as the major mineral phase in MSP, whereas muscovite and quartz were observed in the mica sample. The acid leaching studies suggest a maximum of 22% potash recovery under conditions: 4 M H_2SO_4 acid, particle size of ～100 μm, stirring speed of 600 r/min, leaching temperature of 75℃, and leaching time of 90 min. The chlorination roasting–water leaching process was adopted to achieve the lowest level of 80%–90% potash recovery. The optimum conditions for the recovery of ～93% potash from mica(～8.6 wt% K_2O) requires 900℃ roasting temperature, 30 min roasting time,and 1:1:0.75 mass ratio of mica : MSP : Na Cl. The roasting temperature and amount of Na Cl are found to be the most important factors for the recovery process. The reaction mechanism suggests the formation of different mineral phases, including sylvite(KCl), wollastonite, kyanite,and enstatite, during roasting, which were confirmed by X-ray diffraction(XRD) analyses and scanning electron microscopy(SEM) morphologies. The MSP-blended Na Cl additive is more effective for potash recovery compared with the other reported commercial roasting additives.     

Influence of acid leaching and calcination on iron removal of coal kaolin

Calcination and acid leaching of coal kaolin were studied to determine an effective and economical preparation method of calcined kaolin. Thermogravimetric-differential thermal analysis (TG-DTA) and X-ray diffraction (XRD) demonstrated that 900℃ was the suitable temperature for the calcination. Leaching tests showed that hydrochloric acid was more effective for iron dissolution from raw coal kaolin (RCK), whereas oxalic acid was more effective on iron dissolution from calcined coal kaolin (CCK). The iron dissolution from CCK was 28.78wt%, which is far less effective than the 54.86wt% of RCK under their respective optimal conditions. Through analysis by using M?ssbauer spectroscopy, it is detected that nearly all of the structural ferrous ions in RCK were removed by hydrochloric acid. However, iron sites in CCK changed slightly by oxalic acid leaching because nearly all ferrous ions were transformed into ferric species after firing at 900℃. It can be concluded that it is difficult to remove the structural ferric ions and ferric oxides evolved from the structural ferrous ions. Thus, iron removal by acids should be conducted prior to calcination.     

Effects of the mineral phase and valence of vanadium on vanadium extraction from stone coal

The influence of roasting on the leaching rate and valence of vanadium was evaluated during vanadium extraction from stone coal. Vanadium in stone coal is hard to be leached and the leaching rate is less than 10% when the raw ore is leached by 4 mol/L H₂SO₄ at 90℃ for 2 h. After the sample is roasted at 900℃ for 2 h, the leaching rate of vanadium reaches the maximum, and more than 70% of vanadium can be leached. The crystal of vanadium-bearing mica minerals decomposes and the content of V(V) increases with the rise of roasting temperature from 600 to 900℃, therefore the leaching rate of vanadium increases significantly with the decomposition of the mica minerals. Some new phases, anorthite for example, form when the roasting temperature reaches 1000℃. A part of vanadium may be enwrapped in the sintered materials and newly formed phases, which may impede the oxidation of low valent vanadium and make the leaching rate of vanadium drop dramatically. The leaching rate of vanadium is not only determined by the valence state of vanadium but also controlled by the decomposition of vanadium-bearing minerals and the existence state of vanadium to a large extent.     

Extraction and separation of nickel and cobalt from saprolite laterite ore by microwave-assisted hydrothermal leaching and chemical deposition

Extraction and separation of nickel and cobalt from saprolite laterite ore were studied by using a method of microwave-assisted hydrothermal leaching and chemical deposition. The effects of leaching temperature and time on the extraction efficiencies of Ni2+ and Co2+ were investigated in detail under microwave conditions. It is shown that the extraction efficiencies of Ni2+ and Co2+ from the ore pre-roasted at 300℃ for 5 h were 89.19% and 61.89% when the leaching temperature and time were about 70℃ and 60 min, respectively. For the separation process of Ni and Co, the separation of main chemical components was performed by adjusting the pH values of sulfuric leaching solutions using a NaOH solution based on the different pH values of precipitation for metal hydroxides. The final separation efficiencies of Ni and Co were 77.29% and 65.87%, respectively. Furthermore, the separation efficiencies of Fe of 95.36% and Mg of 92.2% were also achieved at the same time.     

Existence and release of fluid inclusions in bornite and its associated quartz and calcite

The existence and release of fluid inclusions in bornite and its associated minerals, namely, quartz and calcite were investigated and confirmed. The structures, forms, and phases of these large quantities of fluid inclusions were also studied. A mass of fluid inclusions with various sizes, distributions, shapes, and phases exist in bornite and its associated minerals. Their sizes vary from a few micrometers to tens of micrometers, and the forms appear as negative crystals, or elongated, elliptical, and irregular. At room temperature, fluid inclusions were mainly characterized as gas-liquid twophase. However, small amounts of fluid inclusions with pure gas phase and pure liquid single-phase were also observed in quartz and calcite. These fluid inclusions initially broke during the ore crushing and grinding process and then released into the flotation pulp in the flotation process. The quantitative analysis of fluid inclusions in the solution and the comparisons of mineral dissolution show that the amount of copper and iron released by fluid inclusions in the bornite sample is higher than the amount dissolved by the mineral; fluid inclusions in the associated gangue minerals, quartz, and calcite also make contribution.     

Upgradation of bauxite by molecular hydrogen and hydrogen plasma

An approach was developed to upgrade the bauxite ore by molecular hydrogen and hydrogen plasma. A gibbsite-type bauxite sample was obtained from National Aluminium Company (NALCO), Odisha, India. The obtained sample was crushed and sieved (to 100 μm) prior to the chemical analysis and grain-size distribution study. The bauxite sample was calcined in the temperature range from 500 to 700°C for different time intervals to optimize the conditions for maximum moisture removal. This process was followed by the reduction of the calcined ore by molecular hydrogen and hydrogen plasma. Extraction of alumina from the reduced ore was carried out via acid leaching in chloride media for 2 h at 60°C. X-ray diffraction, scanning electron microscopy, thermogravimetry in conjunction with differential scanning calorimetry, and Fourier transform infrared spectroscopy were used to determine the physicochemical characteristics of the material before and after extraction. Alumina extracted from the reduced ore at the optimum calcination temperature of 700°C and the optimum calcination time of 4 h is found to be 90% pure.     

Bioleaching of vanadium from barren stone coal and its effect on the transition of vanadium speciation and mineral phase

This study determined the optimal conditions required to obtain maximum vanadium extraction and examined the transition of mineral phases and vanadium speciation during the bioleaching process. Parameters including the initial pH value, initial Fe2+ concentration, solid load, and inoculum quantity were examined. The results revealed that 48.92wt% of the vanadium was extracted through bioleaching under optimal conditions. Comparatively, the chemical leaching yield (H₂SO₄, pH 2.0) showed a slower and milder increase in vanadium yield. The vanadium bioleaching yield was 35.11wt% greater than the chemical leaching yield. The Community Bureau of Reference (BCR) sequential extraction results revealed that 88.62wt% of vanadium existed in the residual fraction. The bacteria substantially changed the distribution of the vanadium speciation during the leaching process, and the residual fraction decreased to 48.44wt%. The X-ray diffraction (XRD) and Fourier transform infrared (FTIR) results provided evidence that the crystal lattice structure of muscovite was destroyed by the bacteria.     

In situ cryogenic Raman spectroscopic studies on the synthetic fluid inclusions in the systems H2O and NaCl-H2O

Fluid inclusions of the H2O-salt systems constitute the major fluid inclusion types preserved in the nature. The salts commonly present in the fluid inclusions are NaCl, KCl, CaCl2 and MgCl2[1,2]; among them NaCl is the dominant species. The most powerful…     

低品位钼精矿的钼提取研究

采用焙烧—氨浸—渣碱浸工艺对某低品位钼精矿进行钼提取的研究.结果表明,碳酸钠的加入能有效分解钼酸钙,提高钼的提取率.焙烧—氨浸阶段最优工艺条件为焙烧温度600℃,焙烧时间2 h,氨浸温度80℃,氨水过量系数1.4,碳酸钠用量467 kg/t,液固比4.浸出渣中的钼分别采用酸法(HCl)和碱法(Na2CO3+NaOH)进行提取.结果表明:酸法仅可回收渣中34.92%的钼,而且操作过程不易控制,不适合实际应用;碱法(Na2CO3+NaOH)处理工艺中碳酸钠用量533 kg/t,氢氧化钠用量433 kg/t.放大实验结果显示整个流程钼的回收率达到96.8%.     

溶胶-凝胶法制备超细Ce-Ti复合粉体的研究

采用溶胶-凝胶法制备了Ce-Ti复合超细粉体,主要研究了溶胶-凝胶法制备过程中溶胶-凝胶形成的条件及不同焙烧温度对超细粉体粒径的影响.结果表明,C2H5OH与H2O摩尔比在0.5~2.0时能形成稳定的凝胶;采用真空干燥能形成松散的结构,不易团聚,真空干燥温度60℃,真空干燥压力5 kPa左右,真空干燥时间大于24 h;超细Ce-Ti复合粉体的平均粒径随干凝胶焙烧温度的升高而增加,在600℃下焙烧1 h,能得到较好的效果,粒径可达5.9 nm.     

黑龙江鹿鸣钼矿床流体包裹体特征

鹿鸣钼矿床位于小兴安岭-张广才岭成矿带中南部.钼矿体产于二长花岗岩与花岗斑岩的接触带内,钼矿化主要载体为石英脉,呈脉状、网脉状分布于矿体的内部.研究了主要含矿石英脉体中流体包裹体的特征,结果表明:包裹体相态类型主要为气液两相,矿床的成矿温度峰值分别为400,220℃,盐度为19%~144%,成矿压力平均为18MPa,成矿深度为09~28km,成矿流体成分富含CO2,H2O,CH4等多种气态组分,以及Na+,Ca2+,SO2-4,Cl-液态组分;矿床初始流体来源于岩浆热液,成矿后期受大气降水的混入.矿床成因类型应划归为与中酸性侵入岩浆活动有关的中高温斑岩型钼矿床.     

从硼泥中提取硅、硼的新工艺

以硼泥为原料,硼泥与碳酸钠混合后在900℃下焙烧2h,采用碱浸法回收焙烧后硼泥中的SiO₂和B₂O₃.通过TG-DSC曲线分析了焙烧阶段的反应过程.通过单因素试验研究了碱浸阶段:n(NaOH)/n(SiO₂)、反应温度、反应时间、液固质量比等条件对硼泥中的SiO₂和B₂O₃提取率的影响.通过正交试验,确定了影响SiO₂提取率各因素之间的主次关系依次为:n(NaOH)/n(SiO₂)＞液固质量比＞反应时间＞反应温度,影响B₂O₃提取率各因素之间的主次关系为:反应时间＞反应温度＞n(NaOH)/n(SiO₂)＞液固质量比.最佳的回收条件:n(NaOH)/n(SiO₂)为25,反应温度为50℃,反应时间为40min,液固质量比为8,在此条件下SiO₂的提取率为83.11%,B₂O₃的提取率为75.28%.     

纳米级钇稳定氧化锆的制备与电性能表征

以共沸蒸馏过程辅助的化学方法制备了纳米级的钇稳定氧化锆（YSZ）粉体,结果表明共沸蒸馏的方法有效地实现了沉淀的完全脱水,从而阻上了颗粒间的硬团聚,X射线衍射研究指出共沉淀物转变为方立相的最低温度为600度,X射线衍射谱和高分辨透射电镜照片均显示在600度下灼烧得到的粉体的粒径为6nm,而由BET比表面积测定计算所得到的粉体粒径则为11nm,从而确定团聚为软团聚,YSZ样片在1500度下烧结5h得到相对密度为94．8％的烧结体,以交流阻抗谱技术研究在空气和氩气气氛中材料的电导率,在9000度空气气氛下测得的电导率为056S.cm^-1,而在氩气气氛下可达到0067S.cm^-1显著高于用单纯共沉淀法制备的YSZ样片的电导率（0．009S.cm^-1)以用Plaster casting法制备的电导率（0.028S.cm^-1）,而电导活化能为0．88－0．89eV,较文献报导值低。     

影响纳米锌铝复合氧化物紫外吸收性能的因素

在自制全返混液膜反应器中,采用共沉淀法,制备了粒径为30～90 nm的纳米锌铝复合氧化物.研究了Zn/Al摩尔比、锌铝复合氧化物前体的晶体结构完整性、煅烧温度及升温速率对锌铝复合氧化物紫外吸收性能的影响.结果表明,锌铝复合氧化物紫外吸收性能与其晶体结构密切相关.Zn/Al摩尔比提高、锌铝复合氧化物前体的晶体结构完整有利于增强紫外吸收性能;煅烧温度在400～600 ℃范围时,随着煅烧温度的升高锌铝复合氧化物紫外吸收性能增强,而在700～900 ℃范围时,煅烧温度升高紫外吸收性能降低;升温速率变化对锌铝复合氧化物紫外吸收性能影响不明显.     

钒渣无焙烧浸出液中钒铁萃取分离

利用本课题组提出的钛白废酸无焙烧加压浸出钒渣提钒的新技术,以P204为萃取剂从废酸浸出钒渣的浸出液中进行了提钒研究.实验结果表明:采用亚硫酸钠为浸出液预处理还原剂,将浸出液中三价铁还原成二价铁,从而防止三价铁的共萃;常温条件下,当浸出液初始p H=2.5、水相与有机相体积比为1∶3,震荡时间为4 min时,采用有机相组成为20%P204及10%TBP协同萃取体系,钒的萃取率可达98.61%以上,钒铁的分离系数可达135.3.