铜镍尾矿砂微波加热硫酸溶解实验研究

通过尾矿砂微波加热硫酸溶解新方法的实验,研究了硫酸浓度、液固比及反应时间等因素对尾矿砂酸蚀率的影响。结果显示,在无需搅拌的情况下,微波加热实验的最佳条件酸浓度5mol/L、液固比5.0mL/g都较传统水热法有优势,在反应时间上,微波加热15min就能达到传统水热法2～3h的效果。在酸蚀率相同的情况下,微波加热所用时间仅为传统水热法的1/6,而所用的酸浓度、液固比都较传统水热法小很多。先对尾矿砂直接微波辐照一段时间,然后再加入硫酸进行微波辐照加热溶解,能够促进尾矿砂的溶解,提高尾矿砂的酸蚀率。微波加热条件下,尾矿砂在硫酸浓度8mol/L、液固比5.0mL/g条件下无需搅拌,反应1h后,除透闪石没有完全溶解外,绝大部分的矿物被溶解。与传统加热方式相比,微波加热可显著提高尾矿砂酸溶解速率。     

Preparation of chemical manganese dioxide from low-grade rhodochrosite ore

The preparation of chemical manganese dioxide(CMD) from low-grade rhodochrosite ore(LGRO) in Xiushan,Chongqing,was studied and improved,including leaching with sulfuric acid,purifying,crystallizing and decomposing of MnCO3,and refining of primary MnO2.The product was characterized by X-ray diffraction.The results showed that the extraction ratio,the manganese recovery ratio of purifying,crystallization and refining reached 96.8%,93.9%,97.7%and 85.4%,respectively.The optimum conditions of refining were described as follows:liquid(H2SO4)/solid(primary MnO2) ratio was 3 L/g,the concentrations of NaClO exceeded 20%,and reaction time was 3 hours.Under the above conditions,the contents of MnO2and Mn in the obtained manganese dioxide were respectively 85.1%and 53.9%.The refined MnO2can be used as the super grade manganese dioxide mine powder in chemical industry.The XRD indicated that the structure of the product wasγ-MnO2.     

蛇纹石微波辐照硫酸浸出的实验研究

通过蛇纹石微波辐照硫酸浸出新方法的实验，研究了微波辐照强度、辐照时间、硫酸浓度、液固比及矿石粒度等因素对蛇纹石中氧化镁浸出率的影响，结果表明：与传统加热方式相比，微波辐照加热可显著提高蛇纹石酸浸速率；在最佳工艺条件下，氧化镁浸出率可达97％以上；蛇纹石酸浸渣的主要成分为无定形SiO2，化学成分与沉淀白炭黑相同。     

Leaching of manganese residue for the preparation of trimanganese tetroxide with a high surface area

The accumulation of electrolytic manganese residue (EMR) has become a serious problem and its recycling will be of great benefit to protect the environment and assist sustainable development. The reusing method was conducted by leaching EMR with sulfuric acid and the optimal leaching condition was 1:3 (g/g) as the ratio of solid to liquid with 20% (g/g) H2SO4 , heating at 90 ℃ for 3 hours, which aims at extracting Mn in a sulfuric acid medium. The produced MnSO4 solution was precipitated by adding alkali and oxidized in aqueous phase. The oxidized products were characterized by various techniques, including X-ray powder diffraction (XRD), Fourier transform infrared (IR) spectrometry, vibrating sample magnetometry (VSM), with Brunauer-Emmett-Teller (BET) specific surface area instrument and laser particle size analyzer. The final products were confirmed to be a single-phase Mn3O4 .     

New Process for Preparation Alumina and Silica White from Coal Fly Ash

Fly ash was used to prepare alumina and silica white, The 3 stages of the process are as follows: ammonium sulfate calcining, acid leaching and alkali dissolution. The optimum conditions for the experiments to determine are as follows: molar ratio of (NH4)2SO4/Al2O3 is 6, the calcining time is 2h, he H2SO4 concentration is 20%, the leaching temperature is 80℃ and dissolution duration is 2h, the ratio of solution and solid reaction material is 6 for ammonium sulfate calcining and acid leaching stage, reaction time 30min, ratio of liquid to ore 5∶1, alkali concentration 45% and reaction temperature 95 ℃for the alkali dissolution stage. Under these conditions, the total leaching efficiencies of Al2O3 and SiO2 are 78.86% and 95%, respectively. The quality of the main products alumina and silica white can meet the national standards of GB/T24487-2009 and GB10517-89, respectively.     

Dephosphorization of phosphorus-rich manganese ores by selective leaching with dilute hydrochloric acid

Leaching of three high-phosphorus manganese ore samples from central India with dilute hydrochloric acid (0.1–0.6 M) has been found to reduce their phosphorus contents below the specified limit of 0.12%. Various process parameters, such as concentration of acid, liquid/solid ratio, temperature and period of leaching, particle size of ore etc., have been investigated in detail and optimum values have been worked out on the laboratory scale. Both liquid/solid ratio (slurry concentration) and temperature of leaching appear to be critical process parameters. While the increase in liquid/solid ratio above 3–4 has no beneficial effect, leaching temperature above 50°C has an adverse effect on the extent of dephosphorization. Grain size of ore finer than 100 mesh (B.S.) in general gives satisfactory dephosphorization. Laboratory-scale results have been, in general, supported by bench-scale work which shows that phosphorus can be effectively removed from high-phosphorus manganese ores of central India by leaching in dilute hydrochloric acid at ambient temperature. Comparative performance of the dilute solutions of all the three mineral acids as leaching agents has been discussed.     

Calcified roasting-acid leaching process of vanadium from low-grade vanadium-containing stone coal

The low-grade vanadium-containing stone coal used in this experiment was collected from Wuxi Coun- try, Chongqing City, China. The experiment focused on the vanadium recovery from roasted residue through opti- mizing the process conditions of an effective and environmentally-friendly technology, named calcified roast- ing-sulfuric acid leaching technology. By single-factor experiments and orthogonal experiments, the effects of roast- ing temperature, roasting time, sulfuric acid concentration and leaching time on the leaching ratio of vanadium were analyzed. The results showed that the leaching ratio of vanadium reached 85.5% under the proper technological con- ditions of roasting temperature=950℃, roasting time=4 h, 40% concentration of sulfuric acid and leaching time=6 h.     

用Lix984萃取分离水钴矿浸出液中的铜钴

采用Lix984作为萃取剂、硫酸作为反萃剂,从低品位水钴矿还原酸浸液中萃取分离铜、钴。研究了平衡pH值、萃取剂浓度、相比（有机相与水相的体积比）、混合时间、反萃剂浓度、反萃相比等因素对萃取分离的影响,确定了Lix984萃取分离铜、钴的优化条件。结果表明,萃取剂Lix984萃取铜的优化工艺条件：p（Lix984）为40％;平衡pH为1．83;相比为1：1;混合时间为4rain;反萃剂为4．0mol／L的H2SO4。;反萃相比为1：1。在优化条件下,料液经三级逆流萃取和二级反萃,萃取率和反萃率分别达99．O％和99．5％。     

Recovery of some valuable elements from lamprophyre dykes in the Abu Rusheid area, Southeastern Desert, Egypt

In the Abu Rusheid area, Southeastern Desert of Egypt, polymineralized (HREEs, U, Zn and Pb) lam-prophyre dykes are recently recorded. The lamprophyre dykes cut cataclastic rocks along share zones in NNW-SSE trends. The secondary U-minerals are essentially represented by uranophane, kasolite, torbernite and autunite. Ex-perimental work was carried out on the lamprophyre dykes for the recovery of uranium and other valuable elements (e.g. Zn, Pb and Al) from 50 kg of technological sample. The optimum conditions were: 100 g/L sulfuric acid con-centration, 1:5 S/L (solid/liquid) and soaking for 15 days at room temperature. The leaching efficiencies for the re-covery of uranium and other elements like Al, Zn and Pb were 40, 33.6, 98.8 and 78, respectively.     

准格尔地区粉煤灰中镓的浸出率影响因素研究

为了粉煤灰的高附加值综合利用,采用酸浸法对准格尔地区循环流化床粉煤灰进行了镓的浸出实验研究,考察了多种因素对镓的浸出率的影响,包括粉煤灰粒度,酸的种类与浓度、酸浸温度与时间、固液比等。结果表明,提高镓的浸出率的适宜条件为:粉煤灰粒度200目,盐酸的浓度6 mol/L,酸浸温度应大于160℃,酸浸时间6 h,液固比在5∶1~6∶1之间为宜。在优选的工艺条件下,镓的浸出率可达80%以上。从粉煤灰中提取镓,使其作为一种资源加以利用,是提高粉煤灰综合利用价值的有效途径。     

水热活化法提取粉煤灰中的氧化铝

采用高压水热活化法对预先烧制的粉煤灰进行碱溶实验,探讨钙硅摩尔比、碱液浓度、液固比、苛性比、反应温度、反应时间等影响因素对于氧化铝溶出率的影响。考虑到氧化铝溶出率及反应成本等各方面因素,得出氧化铝溶出的适宜条件。结果表明:碱溶条件下,钙硅摩尔比为1.0,溶液碱浓度为350 g/L,液固比为10∶1,苛性比为14,反应温度280℃,活化时间为2 h。通过氧化铝溶出工艺条件的优化,可使氧化铝提取率达到95%以上。     

基于二苯乙醇酸体系快速测定区域地质矿产调查样品中的钨钼

本文建立了一种快速分析区域地质矿产调查样品中钨钼的方法。试样经高温焙烧、碱熔分解,钨、钼与其它杂质元素所形成的氢氧化物沉淀分离;在二苯乙醇酸体系(0.25mol/L硫酸-0.04g/L二苯乙醇酸-0.10g/L二苯胍-20g/L氯酸钠)中,钼、钨分别于约-0.25V、-0.85V产生灵敏的平行催化波,根据极限扩散电流的大小同时测定这两种元素。该方法的测定下限(X0+3S)<0.10×10-6;准确度(|Δlog|)≤0.05;精密度(RSD)≤7.72%。国家标准物质测定值与标准值相符;实际样品测定值优于电感耦合等离子体发射质谱法。方法扩大了催化极谱法的适应性,提高了实际应用价值。     

氧化亚铁硫杆菌浸取黄铜矿石影响因素的试验研究

本文通过对氧化亚铁硫杆菌浸出青海某地区低品位黄铜矿石的试验,探讨了接种量、矿石粒度、矿浆含量对黄铜矿石摇瓶浸出过程的影响。结果表明：在无菌硫酸浸出过程中,黄铜矿可以自发氧化分解,最终浸出率为15.98%;在有菌浸出过程中,氧化亚铁硫杆菌接种量为5/100（mL/mL）时铜浸出率最高可达31.16%。氧化亚铁硫杆菌浸出黄铜矿在接种量为5/100（mL/mL）,矿石粒径为〈104μm,矿浆含量为5/100（mL/mL）时较为适宜。     

Hydrometallurgical processing and recovery of molybdenum trioxide from spent catalyst

Hydrometallurgical processing of spent hydrodesulphurisation (HDS) catalyst for the recovery of molybdenum using sodium carbonate and hydrogen peroxide mixtures was investigated. The results indicated that the recovery of molybdenum was largely dependent on the concentrations of Na₂CO₃ and H₂O₂ in the reaction medium, which controls the acidity of the leach liquor and carry over of impurities such as Al, Ni, P, Si and V. Leaching process was exothermic and leaching efficiency of molybdenum decreased with increasing solid to liquid ratio. Large scale leaching of spent catalyst, under optimum conditions: 20% pulp density, 85 g/L Na₂CO₃, 10 vol.% H₂O₂ and 1 h reaction, resulted a leaching efficiency of 84% Mo. The obtained leach liquor contained (g/L): Mo — 22.0, Ni — 0.015 and Al — 0.82, P — 1.1, Si — 0.094 and minor quantities of V — 8 mg/L, As and Co — < 1 mg/L. Recovery of Mo from leach solution as MoO₃ of 97.30% purity was achieved by ammonium molybdate precipitation method.     

碳质银精矿氯化浸出工艺的研究与应用

采用氧化焙烧工艺对碳质银精矿进行除碳、除硫预处理,试验确定焙烧温度为650℃。焙砂以3YL--NaCl无氰氯化体系浸出,研究了影响氯化浸出的因素:3YL用量、氯化钠浓度、浸出酸度、时间、温度℃及固液比等,并在试验确定的工艺条件下,进行了公斤级试验,得出Au、Ag、Cu、Pb、Zn的氯化浸出率分别为95.1%、91.6%、85.7%、95.2%、83.8%。     

钾长石粉酸浸除铁废液资源化的实验研究

钾长石粉经过硫酸或盐酸酸浸除铁后, 废液中含有大量的金属离子和游离酸.对废硫酸进行循环利用实验, 钾长石粉铁的浸出率达到88.3%.对酸浸废液进行蒸发结晶, 分别制备得到了纯度为94.1%的绿钾铁矾和74%的三氯化铁.用硫酸酸浸废液蒸发结晶后, 铁的回收率为70.0%, 钾的回收率为96.5%, 整个工艺无需高温, 无需加压, 操作简单, 具有高效、低能耗、低污染的特点, 表明用本项技术处理酸浸废液行之有效.分析认为, 废液呈强酸性、溶液中存在大量Fe2+、碱金属离子含量偏低是蒸发结晶过程中形成绿钾铁矾而不是黄钾铁矾的主要原因.      

氯化铵浸取纤蛇纹石动力学研究

较低的矿物溶解率和反应剂的不可循环利用是CO2矿物封存发展的两大难题。针对这些问题,本文提出了一种新的以可循环的NH4Cl溶液作为中间媒介的CO2矿物封存工艺,并系统地研究了蛇纹石在氯化铵溶液中的液-固两相的反应动力学。实验研究发现:(1)纤蛇纹石的浸取符合Elovich模型,浸取过程基本在1h左右完成,在100℃、5mol/L氯化铵溶液中,纤蛇纹石的浸取率达到12.67%;(2)温度对纤蛇纹石初始反应速率的影响显著,温度越高,反应速率越快;(3)当氯化铵浓度在1~5mol/L范围内变化时,它对镁离子浸取率的影响不明显,反应速率随着浓度的升高而有所增加;(4)本实验反应表现出来的活化能大小为129.56kJ/mol。      

钾长石粉酸浸除铁的实验研究

在利用钾长石粉合成沸石分子筛和制取碳酸钾技术中，铁的存在会降低沸石的白度。对北京平谷、天津蓟县、内蒙白云鄂博三地钾长石粉进行硫酸酸浸除铁实验，获得最大铁浸出率分别为88．6％、93．2％和64．6％，且前两地钾长石粉中铁的浸出行为相似，酸浸除铁效果均优于白云鄂博钾长石粉。采用正交实验法研究硫酸浓度、酸浸温度和时间对除铁效果的影响，表明三者对不同地区钾长石粉酸浸除铁效果的影响程度各不相同。钾长石酸浸除铁反应开始时，铁的溶解极快，反应速率主要由化学反应控制；其后溶解相对缓慢，反应速率则由扩散作用控制。     

硅灰石与盐酸快速反应规律及应用研究

反应体系pH≤1．5时，硅灰石与盐酸快速反应，反应后体系中Si,Ca,Fe,Mg等元素在固液两相中化学状态及分布不同，当pH值为0．3－0．6时，液相中SiO2(硅溶胶）比例最大，Ca主要存在于液相中，但固相中总有少量Ca存在。快速反应固相比表面积较大，若反应前添加PEG，反应后中和到pH=4，可制备高比表面多孔SiO2，其比表面积＞430m^2/g，孔径1－2nm，该产物在合成以二氧化硅为基质的纳米复合材料及用作催化剂载体等方面有较好的应用前景。     

二苯碳酰二肼光度法测定超基性岩石中三氧化二铬的改进

二苯碳酰二肼光度法是测定微量Cr(Ⅵ)的行业标准方法,以硫酸作为显色介质,酸度要求严格,显色稳定时间短,体系显色后需在10 min～1 h测定完毕,灵敏度较差。本文对标准方法进行改进,将显色介质由硫酸改为磷酸。结果表明,在H3PO4介质中显色剂与Cr(Ⅵ)反应生成的络合物可稳定3 h,方法相对标准偏差(RSD)≤5.25%,加标回收率为99.2%～102.0%,检出限由标准方法的13.6μg/g降至3.8μg/g。建立的方法用于超基性岩标准物质分析,相比于标准方法,稳定性、精密度和准确性均有提高。