不同浓度的尾砂胶结充填体破坏过程 声发射特性试验研究*

制备了3种不同质量浓度的充填体试件，进行了单轴压缩声发射试验，分析了不同浓度的充填体力学特性，重点研究了试件破坏过程中的声发射振铃计数、声发射累计撞击数与声发射累计能量的比值(r值)、主频及其相对高频信号激增响应系数特征。研究表明：随着浓度的增加，充填体的峰值强度与弹性模量呈增大趋势，充填体中出现的声发射累计振铃计数越多；r值先升高再持续减小到一个较低值，随着外载荷的增加，进入缓慢升高阶段，峰值前均保持在该阶段。充填体破裂前兆信息在声发射信号主频分布中呈现主频段增多现象，表现为由加载初期的1~2个主频段，在临界主破裂时增多到3~5个主频段；且随着浓度的增加，声发射信号主频频段分布越宽，声发射相对高频信号(160~180 kHz)的激增响应系数呈递减趋势。以上特征可为不同浓度的尾砂胶结充填体稳定性监测、预测提供依据。     

Investigating the kinetics of liquid-free,OSDA-free ZSM-5 zeolite synthesis from iron ore tailings

In this study, ZSM-5, which is a Mobil-type five-type zeolite with well-defined crystal morphology, is successfully synthesized via a seed-assisted, liquid-free method that uses iron ore tailings as a silica source. The ZSM-5 crystallization kinetics at 423, 433, and 443 K and different synthesis times are investigated to identify the nucleation and crystallization mechanisms of the synthesized ZSM-5 zeolites, and results suggest that the crystallization kinetics follow a Kolmogorov-Johnson-Mehl-Avrami-type behavior. The activation energies for the induction and transition periods are 112.38 and 58.35 kJ mol⁻¹, respectively. Furthermore, the Avrami exponent indicates three-dimensional crystal growth from both sporadic and instantaneous nucleation mechanisms. A comparison of our results with previous reports of the ZSM-5 crystallization mechanism demonstrates that the seed crystals play a significant role in nucleation and crystal growth. Finally, seed surface crystallization and new nuclei crystallization dual mechanism has been proposed to describe the crystallization process of ZSM-5.     

X射线荧光光谱法测定萤石中CaF2、CaCO3、S、Fe及SiO2

X射线荧光光谱法分析是目前快速分析方法之一,精密度受基体效应、均匀性、元素间干扰等影响。采用粉末压片法制备样品,用X射线荧光光谱法直接测定F、Ca元素,得出CaF_2及CaCO_3含量,并同时分析萤石中S、Fe、SiO_2的含量。精密度实验表明,待测元素的相对标准偏差均低于0.66%(RSD,n=10),能满足萤石中各元素的检测要求。     

The Effect of Oleic Acid Emulsification using SPE on Fluorite and Dolomite Flotation**

Collector OA, oleic acid, is widely used industrially for fluorite flotation. Low selectivity, dispersibility and collecting capability of the OA collector are always observed. In this study, compared with flotation of dolomite, a collector mixture of OA and SPE (styrylphenol polyoxyethylene ether) demonstrated significantly better performances for the fluorite. An optimal mass ratio 4 : 1 OA : SPE was found, and the recovery of fluorite was increased from over 85 % to more than 94 % compared with pure OA. Furthermore, the dosage of the collector agent was reduced from 50 mg mL⁻¹ to 20 mg mL⁻¹, which did not negatively impact the recovery of dolomite. The results from the contact angle tests indicated that SPE selectively increased the surface hydrophobicity of fluorite but had little effect on dolomite. Besides, zeta potential measurements and IR analyses revealed that the addition of SPE led to strong chemical adsorption on the surface of fluorite, resulting in a significant difference in the flotation performances of the two minerals. Therefore, SPE-emulsified OA is corroborated to prompt more selectivity and collecting capability on flotation of fluorite over dolomite.     

气基磁化焙烧回收包头稀土尾矿中铁的研究

试验采用磁化焙烧-磁选的方法来回收包头稀土尾矿中的Fe。考察了还原球团的粒径、焙烧温度、还原气体的成分、还原气气体流量、焙烧时间对于磁化焙烧回收Fe的影响。在焙烧温度为580℃,CO与CO2的浓度比为40∶60,还原气体气流量为1.2 L·min-1,焙烧时间为60 min的条件下对球团进行磁化焙烧,并将焙烧后的球团进行磨矿,使得-200目的物料占物料总重量的95%。将磨矿后的物料置于磁场强度为233 k A·m-1的磁选管中进行磁选,可以得到品位为60%左右的铁精矿,其铁回收率达到70%左右。     

粉末压片-X射线荧光光谱法与红外吸收光谱法联合测定萤石中各组分

采用粉末直接压片法,用X-射线荧光光谱法[1]测得萤石中Ca总量,Fe2O3,P,SiO2,K2O的含量,再用红外吸收光谱法测得样品中碳含量,换算得到CaCO3中的钙含量,进一步求得萤石中CaF2含量。此方法简便、准确。用9个标准物质制定了工作曲线,并进行了自测,另用该系列中5号样品(GBW07254)进行准确度和精密度测试,结果令人满意。     

赣南新塘萤石矿区地下水元素钙氟变化及其成矿意义

对新塘脉状矿床及其附近地下水的钙、氟元素进行了系统检测,发现钙、氟含量存在明显的空间分布差异.采矿矿床及其附近地下水的钙、氟含量偏高,而2 km远的地下水钙、氟含量低且接近流域平均值,两处平均含量相差近10倍.钙、氟的相关性分析显示,水体中钙、氟含量具有很好的相关性,揭示该区萤石矿成矿受沉积物钙氟控制,并与地下水运动密切相关,通过热液循环不断淋滤溶蚀围岩获取钙氟形成萤石矿.由此,矿区的钙氟异常变化可以作为找矿的重要指标.     

矿山尾矿中微量银元素快速检测方法的研究

针对矿山尾矿中微量银元素测定的技术难题,提出了一种基于超短光路原理的能量色散X荧光能谱快速检测的方法。提高元素测量分辨率,提高样品分析效率,降低光管功率,延长仪器使用寿命。能谱系统优化了滤片以及探测器屏蔽物等设计,准直器采用对X射线基本无散射的聚四氟乙烯,达到微量银元素的检测要求。实际尾矿测试中,银的检出限达到0.1mg·kg~(-1),RSD在0.1%~2.6%之间,准确度在87%~115%之间。对比尾矿、原矿及精矿的检测实验,证明了在能量色散X荧光能谱中引入超短光路设计方法,能够提升系统峰/本底比,满足微量银元素的检测要求。     

Sulphur removal of iron ore tailings by flotation

Iron ore tailings have become one kind of the most hazardous solid waste. Beneficiation of iron ore tailings is a significant issue in the world steel industries, from the point of view of both pollution control and secondary resources. This investigation addressed the processing of tailings with high sulphur content from an iron ore concentrator to produce pellet feed fines and to prevent acid mine drainage. This study was the lab-scale testing of an integrated method consisting of froth flotation combined with gravity and magnetic separation. Reverse flotation located at the end of the primary treatment circuit (high- and low-intensity magnetic separation) will lower a large amount of the sulphur from magnetic separator concentrate. The effects of various operating parameters such as concentrations of collector, frother, depressant and activator, pH, solid-in-pulp concentration have been studied on the sulphur removal using reverse flotation. According to the data presented in this study, the maximum recovery of total sulphur was obtained when the operational parameters were set to the PAX dosage160?gr/t, MIBC dosage 140?gr/t, CuSo₄ 100?gr/t, air flow rate 10?l/min, pH 8.5, and pulp density 30%. With these optimum parameters, final concentrate with the grade of 63.7% Fe and 0.085% S was obtained. The results of this study indicated that, with this method, a great amount of iron concentrate is produced and, simultaneously, the sulphidic fraction is separated that can later be managed more easily owing to the reduced volume.     

原子荧光光谱法测定萤石中的微量铅

以铁氰化钾–盐酸羟胺体系代替铁氰化钾–草酸体系,建立原子荧光法测定萤石中铅含量的方法。对实验条件进行了优化,在负高压280 V,灯电流65 m A,原子化高度8 mm,还原剂3%硼氢化钾溶液(含0.5%Na OH),载流4%盐酸的工作条件下,铁氰化钾–盐酸羟胺体系有明显的增感作用。样品中Ca~(2+)含量在4 g/L之内不影响铅的测定,溶解阶段通过高氯酸冒烟赶尽HF排除氟离子的干扰,并加入硫氰酸钠–邻菲罗啉消除铁和铜等离子的干扰。测定铅的线性范围为0~80 ng/L,相关系数r=0.999 6,方法检出限为0.187μg/L,测定结果的相对标准偏差为0.25%~1.40%(n=12),加标回收率为97.8%~104.5%。该方法测定结果与电感耦合等离子体原子发射光谱法测定结果相符。原子荧光光谱法快速准确,基体干扰少,灵敏度高。