钒离子指示电极在石煤焙烧料浸出动力学研究中的应用

以湘西吉首某地石煤矿为原料,在850℃焙烧6 h后,采用酸浸法从焙烧料提取钒,用钒离子指示电极在线跟踪石煤浸出过程中五价钒浓度的变化,研究浸出过程中的动力学;考察矿石粒径、pH值和浸出温度对浸出过程E--t曲线的影响.研究结果表明:钒离子指示电极电势测定结果受杂质Fe3+的影响很小,可以用于跟踪石煤焙烧料浸出过程中钒离子浓度的变化;硫酸浸出后,矿石粒度越小,溶液的酸度越大,浸出温度越高,五价钒离子越容易浸出.采用等高线法求算出石煤焙烧料浸出过程在高温段区的表观活化能Ea为1.56 kJ/mol,受扩散步骤控制;在低温段区的表观活化能Ea为3.99 kJ/mol,受化学反应步骤控制.     

采用氧化焙烧-酸浸法从高碳石煤中提钒试验研究

针对广西某难浸高碳石煤,比较相同焙烧和酸浸条件下静态焙烧矿和流态化焙烧矿钒的浸出率,优化流态化焙烧矿的酸浸条件。研究结果表明:流态化焙烧矿酸浸钒的浸出率比静态焙烧矿酸浸钒的浸出率平均高24%,所以,在相同焙烧温度、时间下流态化焙烧较静态焙烧更利于钒的浸出;在液固质量比为0.8:1.0,二氧化锰添加量为3%和氢氟酸添加量为2%的条件下,得最佳酸浸条件,即酸矿质量比为0.4:1.0,浸出温度为150℃,浸出时间为6 h,在此最佳酸浸条件下,钒浸出率可达88.26%。     

响应曲面法优化钒渣微波钙化焙烧提钒工艺

采用相应曲面法,建立钙化添加剂用量、焙烧温度、焙烧时间与钒浸出率关系的数学模型,对钒渣微波钙化焙烧提钒工艺进行优化,并对试验结果的可靠性进行分析与验证。研究结果表明,采用响应曲面法优化钒渣微波钙化焙烧提钒工艺参数是可行的;微波钙化焙烧工艺参数对钒浸出率的影响从大到小依次为钙化添加剂用量、焙烧温度、焙烧时间;最佳焙烧参数为焙烧温度861.69℃、钙化添加剂用量1.02、焙烧时间106.31 min,此时钒的浸出率可达93.82%。     

石煤氧化焙烧-酸溶液浸出提钒工艺

针对某地石煤原料组成特点,为提高石煤中钒的浸出率本试验采用氧化焙烧-酸溶液浸出提钒的工艺,研究了焙烧温度,添加剂氯化钠的用量,焙烧时间,酸浸出液用量及浸出温度时间对钒浸出率的影响.结果表明:,焙烧水浸后渣再用稀酸浸出的方法,钒的浸出率可提高10 %左右,钒的浸出率可达到75 %~80 %.     

碱法浸出石煤中的钒和硅

在石煤提钒工艺中,为了充分利用石煤中的有价元素硅,采用碱浸提钒工艺提取石煤中的钒和硅.经过预焙烧后,可以有效地破坏石煤结构,提高钒硅浸出率.在焙烧温度850℃、焙烧时间2h、浸出温度95℃、浸出时间4h、固液比(g∶mL)1∶1.4、矿碱质量比1.2∶1的条件下,钒的浸出率为86.6%,硅的浸出率为61.4%.     

强化氧化对石煤钙化焙烧提钒的影响

研究石煤钙化焙烧参数对提钒效果的影响,确定合理的焙烧参数:当焙烧温度为950℃,焙烧时间3 h,碳酸钙添加量为质量分数6%时,石煤焙烧料中钒的浸出率为63%。在此基础上研究增强氧化对提钒效果的影响,比较通空气和添加MnO2这2种情况下提钒的效果。用化学物相分析和钒价态分析等技术探讨加强氧化提高钒浸出率的原因。空气通入速度为0.48 L/h时,钒的浸出率为69%;MnO2添加量(质量分数)为3%时,钒浸出率为68%。研究结果表明,加强氧化后矿石的结构被破坏,V5+含量提高,生成更多易溶于酸的钒酸钙类物质。     

无盐焙烧法提取石煤钒矿中V2O5新工艺研究

本实验主要采用无盐焙烧法对暮石煤钒矿石进行焙烧和浸出研究。在700-900℃高温下焙烧．然后用硫酸做浸出分解试羽，在80-90℃条件下从舍钒石煤矿石中钢得硫酸钒酰溶液（浸出液），得到最佳焙烧和浸出工艺参数。     

酸浸对钙化焙烧提钒工艺钒浸出率的影响

采用稀硫酸浸出法提取钙化焙烧后钒渣中的钒,考察了浸出参数:物料粒度、体系pH值、浸出温度和时间、液固比(L/S)、搅拌速度对钒及杂质元素浸出率的影响.结果表明:物料粒度小于75μm时对提高钒浸出率影响较小;液固比从2∶1增加到7∶1,搅拌速度由100增加到500r/min时,钒浸出率增长幅度均低于3%;钒浸出率在浸出前15min内迅速升高,之后增长变缓;浸出体系pH值对钒及杂质浸出率影响显著,pH值为2~3时钒浸出率达90%,杂质元素Ca,Mn,Mg,Al,Si,P浸出率为10%~30%;在较佳浸出条件下:粒度96～75μm,pH值为25,温度55℃,时间30min,L/S为3,搅拌速度500r/min,钒浸出率超过91%.     

不同钙化剂对高钒渣酸浸提钒的影响

针对传统钒渣钠化焙烧-水浸提钒工艺的不足,确定对钒渣钙化焙烧-酸浸提钒进行研究。在理论分析的基础上,本研究以高钒渣为原料,研究了钙化焙烧-酸浸提钒过程中3种钙化剂(CaSO4、CaCO3、CaO)的焙烧机理以及对提钒效果的影响。研究结果表明:钒浸出率随焙烧温度的升高先增大后减小,且在1 450K时达到最大值;钙化剂配比为100%CaSO4时提钒率最大;在目前实验室研究条件下,钒的浸出率最大可达93.53%。     

石煤中影响钒转浸率的主要因素研究

通过对石煤提钒焙烧阶段焙烧温度和添加剂作用、配比的研究，得出了焙烧阶段最适宜的焙烧温度、入炉温度和添加剂配比范围。实验结果表明，采用焙砂水浸后渣再用稀酸浸出的方法，钒的转浸率平均可提高１０％左右。     

Roasting and leaching behaviors of vanadium and chromium in calcification roasting–acid leaching of high-chromium vanadium slag

Calcification roasting–acid leaching of high-chromium vanadium slag (HCVS) was conducted to elucidate the roasting and leaching behaviors of vanadium and chromium. The effects of the purity of CaO, molar ratio between CaO and V₂O₅ (n(CaO)/n(V₂O₅)), roasting temperature, holding time, and the heating rate used in the oxidation–calcification processes were investigated. The roasting process and mechanism were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), and thermogravimetry–differential scanning calorimetry (TG–DSC). The results show that most of vanadium reacted with CaO to generate calcium vanadates and transferred into the leaching liquid, whereas almost all of the chromium remained in the leaching residue in the form of (Fe_0.6Cr_0.4)₂O₃. Variation trends of the vanadium and chromium leaching ratios were always opposite because of the competitive reactions of oxidation and calcification between vanadium and chromium with CaO. Moreover, CaO was more likely to combine with vanadium, as further confirmed by thermodynamic analysis. When the HCVS with CaO added in an n(CaO)/n(V₂O₅) ratio of 0.5 was roasted in an air atmosphere at a heating rate of 10℃/min from room temperature to 950℃ and maintained at this temperature for 60 min, the leaching ratios of vanadium and chromium reached 91.14% and 0.49%, respectively; thus, efficient extraction of vanadium from HCVS was achieved and the leaching residue could be used as a new raw material for the extraction of chromium. Furthermore, the oxidation and calcification reactions of the spinel phases occurred at 592 and 630℃ for n(CaO)/n(V₂O₅) ratios of 0.5 and 5, respectively.     

氯化铵焙烧生石灰提取可溶性钙

为实现生石灰的高附加值利用,采用水浸氯化铵与生石灰的焙烧熟料提取氧化钙,考察了焙烧温度、焙烧时间及铵矿物质量的比对生石灰中氧化钙提取率的影响.通过正交试验,确定了最佳提取氧化钙焙烧条件.研究结果表明:最佳的焙烧工艺为焙烧温度250℃,焙烧时间90min,铵矿物质的量比2.2∶1,此时,氧化钙的提取率可达97.26%.利用差热法进行了机理分析,结果表明氯化铵焙烧生石灰过程总体分三个化学反应步骤.     

高钙含钒煤灰渣提钒的工艺研究

本文阐述了高钙含钒煤灰渣提钒中,影响稀盐酸脱钙、焙烧、浸取、萃取,反萃取、沉钒的有关因素,并确定了最佳工艺条件。     

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.     

炒制裸燕麦淀粉的提取及理化特性研究

通过单因素实验及正交试验,确定碱法提取炒制裸燕麦淀粉的最佳工艺,并测定其理化特性.结果表明,炒制裸燕麦淀粉较佳提取条件是料液比为1:18,pH值为9.5,提取温度为50℃,提取时间为60min.在此条件下,炒制裸燕麦淀粉提取率可达57.54%.理化特性研究表明,炒制裸燕麦淀粉中直链淀粉含量、蓝值及糊化温度均低于未炒制裸燕麦淀粉.     

利用二元钠盐体系处理钒渣的清洁焙烧工艺

试验研究了利用二元钠盐(NaOH-Na₂CO₃)对钒渣进行焙烧,并分析了相关动力学参数对焙烧效果的影响.结果表明:在二元钠盐焙烧过程中,焙烧温度、焙烧时间及NaOH与Na₂CO₃质量比对渣中钒、铬的浸出率影响重大;焙烧过程中,Fe₃O₄被氧化为Fe₂O₃,V₂O₅和Cr₂O₃分别被氧化为β钒酸钠型结构的Na₃VO₄与正交晶系结构的Na₂CrO₄;最佳焙烧条件下,NaOH与 Na₂CO₃质量比为1.5∶1,焙烧温度为600℃,焙烧时间为60min,此时钒与铬的浸出率分别为98.66%与83.57%;浸出尾渣的主要金属元素为Fe.     

茶叶中提取咖啡碱实验的改进

针对＂茶叶中提取咖啡碱实验＂中存在的问题进行改进,采用沙浴对咖啡碱的分离和提纯过程进行控温,焙炒的温度控制在120～140℃,升华温度220～235℃,获得白色针状的咖啡碱,改进后产物的纯度提高,取得了良好的教学效果。     

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%.