利用尾矿砂制备镁铁氢氧化物实验研究

以金川铜镍矿尾矿酸浸液为原料,根据矿物沉淀pH值区间的不同,分步分离Fe、Mg的沉淀物以及有价金属Al、Co、Ni、Cu的混合沉淀物,进而制备具有高附加值的Fe(OH)3和Mg(OH)2,同时富集Co、Ni、Cu等有价金属。结果表明,当溶液pH值为3.8时可沉淀分离出主要成分为施威特曼石(schwertmannite)的氢氧化铁前驱体,pH值达到9.8时沉淀富集出Al、Co、Ni、Cu的混合氢氧化物,随即得到只含有Mg离子的溶液。在60℃条件下,将施威特曼石在pH值为12的NaOH溶液中老化36h,可以得到Fe(OH)3。同时,以NaOH调节只含有Mg离子的溶液至pH值为12.4时可获得Mg(OH)2。本研究为金属矿山尾矿的资源化综合利用提供了新的思路与方法。     

New CGSP Carbonate Matrix Reference Materials for LA-ICP-MS Analysis

Four CGSP (Chinese Geological Standard Powders) carbonate matrix element reference materials were prepared by a coprecipitation method. The major and trace elements were dissolved from natural rare earth carbonate raw materials in strong acid and precipitated with ammonium bicarbonate or ammonia to form carbonate matrix phases. The carbonate reference materials were ground and pressed into tablets for microanalysis. The element homogeneity and stability in CGSP reference materials were tested by LA-ICP-MS using a calibration strategy without an internal standard element and evaluated mainly following ISO Guide 35: 2017 and JJF 1343-2012. Although the homogeneity of most of elements in the CGSP series were comparable to the repeatability obtained from homogeneous glasses, some elements (e.g., Mo, Se, Ga, Ge, Cd, Ni, Co, U) were found to have some degree of heterogeneity. All of elements passed the t-test evaluation in a 32-month stability examination except for Mo in CGSP-A, Na, Ge, Mo in CGSP-B, Ni, Cd, Sn in CGSP-C, and Al, P, Tb, Ho in CGSP-D. The certified element mass fraction values and uncertainties were determined with the characterisation of a non-operationally defined measurand using various bulk analysis methods in eight laboratories. GGSPs will provide a new carbonate calibration reference option for microanalysis.     

不同类型氢氧化镁阻燃剂填充聚丙烯（PP）复合材料力学性能研究

研究了普通氢氧化镁(MH)、六角片状MH和硬脂酸改性MH分别填充聚丙烯(PP)复合材料的性能。用FTIR、SEM和TG对上述3种类型MH及其复合材料的结构和形貌进行了分析。试验结果表明:相比普通MH,六角片状MH和硬脂酸改性后的MH有效降低了表面极性,大大降低了对复合材料的力学性能的影响,显著提高了复合材料的热稳定性;4%SA改性MH比6%SA改性MH填充PP,界面相容性好,对复合材料力学性能的影响小。硬脂酸湿法表面处理氢氧化镁改性的最佳条件为:硬脂酸用量4%,处理温度85~90℃,处理时间60 min,料浆浓度10%。     

共沉淀富集法测定海水中稀土元素含量方法研究

稀土元素已越来越多地应用于示踪各类地球化学体系的物质来源与岩石矿物形成等演化过程。但在进行海水样品的稀土元素检测时,由于样品的高盐特征和稀土元素的痕量特征又使得分析具有相当的挑战性。本研究旨在从高盐的海水基质中有效分离并富集痕量的稀土元素,同时结合电感耦合等离子体质谱（Inductively Coupled Plasma Mass Spectrometry, ICP-MS）技术对海水中的稀土进行定量分析。通过对海水样品稀土元素的定量限分析、加标回收实验和梯度加标回收实验,验证了方法的准确性,评估方法的分离富集效率。通过共沉淀过程中的pH比较、氢氧化钠与氨水作为共沉淀剂的比较,确定了富集过程中共沉淀剂用量、种类等影响因素。通过稀土元素配分曲线的绘制与类似样品结果进行比对,以及标准海水的检测结果,验证了方法在实际样品中的可行性。本研究探索了共沉淀富集法在分离富集海水中稀土元素的实验条件,实现高盐背景下痕量稀土的准确定量,并将其用于近岸海水与孔隙水的实际检测。     

Assessment of the conventional molybdenum-blue and magnesium-induced coprecipitation procedures in phosphorus measurement in various aquatic environments

Phosphorus (P) is an essential nutrient utilized by all organisms for energy transport and growth. Both the conventional molybdenum-blue method and the magnesium-induced coprecipitation (MAGIC) procedures were applied for the measurement of dissolved inorganic phosphorus (DIP) and total dissolved phosphorus (TDP) in more than 840 water samples collected between 2003 and 2005, including seawater (the Huanghai Sea, the East China Sea, and the northern South China Sea), water from rivers and estuaries (the Changjiang, the Huanghe, and the major rivers emptying into the Jiaozhou Bay), groundwater (in the drainage basin surrounding the Jiaozhou Bay), rain- water, and aquaculture water samples. The MAGIC method allows the investigation of phosphorus distributions and cycling for systems in which DIP is below the detection limits of conventional methods. Comparison between the two methods demonstrated that the concentrations obtained with both methods were signiˉcantly correlated. The di?erences of DIP and TDP concentrations measured with the two methods were higher when the concentrations of DIP and TDP were lower, implying the lower reproducibility at low concentrations. The concentration di?erences increase with the increase in the proportion of DOP in TDP, which indicates that the discrepancy of DIP concentrations measured with the two methods increases when the DOP concentration is high. The discrepancies indicated that the composition of P compounds di?ers depending on sample sources and water type; it would be useful to infer the presence of di?erent phosphorus compound pools from di?erences between the two methods. This study indicates the potential presence of a pool of alkaline-labile compounds for samples from rainwater and rivers and estuaries surrounding the Jiaozhou Bay; the potential presence of acid-labile compounds that were adsorbed by Mg(OH)2 for samples from the Changjiang Estuary, Huanghai Sea, East China Sea, and groundwater; the po- tential presence of a substantial pool of acid-labile compounds that were not adsorbed by Mg(OH)2 for samples from the Huanghe Estuary, aquaculture water, the East China Sea algal bloom water, and the northern South China Sea.     

小球藻的絮凝沉降及溶气气浮采收研究

研究了氢氧化钠对不同生长时期小球藻液的絮凝效果,比较了絮凝沉降法和溶气气浮法的采收效果,并初步优化了气浮操作参数。结果表明,在小球藻液中添加氢氧化钠能够取得很好的絮凝效果,添加700 mg/L氢氧化钠,沉降30 min即能达到90%的沉降采收率;同等氢氧化钠添加量下,溶气气浮法的采收效果要优于絮凝沉降法;确定的气浮采收最佳操作参数:指数生长期和稳定期藻液的最佳氢氧化钠添加量分别为350 mg/L和600 mg/L,溶气水进水流速为60 L/h,溶气水/藻液体积比为25%。絮凝沉降法中指数生长期和稳定期的小球藻液采收效果相差不大,而溶气气浮法中同等采收条件下指数生长期的采收率高于稳定期,其采收浓缩倍数也略高于稳定期。     

海水中超低含量活性磷酸盐的Mg(OH)2共沉淀法测定研究

活性磷(正磷酸盐)是海洋浮游植物生长所必需的物质基础[1-8],磷的生物可利用性直接影响全球的初级生产力水平.磷在特定的海洋环境中还可能限制固氮作用,成为限制海洋初级生产力的重要因素[1,3,6].海水中磷酸盐含量的测定也是海洋污染调查的重要指标之一[4,9].农业和工业废水中磷的过度排放导致河口和近岸海水富营养化,引起浮游植物异常繁殖,造成“赤潮”现象[4].因此,海水中磷的准确测定对深入理解生物地球化学过程及海洋环境保护具有重要理论和实际意义[4-6,9].磷钼蓝分光光度法是海水中活性磷的经典测定方法,检测限为324 nmo1/dm3[5],但在一些寡营养盐海域,例如在南海、地中海     

即时合成Zn-Mg-Al层状双氢氧化物处理含Zn2+废水实验研究

在模拟含Zn2 废水中加入Mg2 和Al3 ,以NaOH为沉淀剂,研究金属盐水解即时合成层状双氢氧化物(LDH)去除Zn2 的可行性。详细探讨了体系终点pH值、配料中Mg2 /Zn2 摩尔比值及反应温度和时间对Zn2 去除率的影响,结合X射线衍射分析(XRD)探讨了Zn2 去除机理,并与化学沉淀法进行了比较。结果表明,实验条件下只有pH值显著影响Zn2 去除率(p<0.05),在9.0~11.0范围内去除效果最佳,达99%以上。通过XRD分析结合即时合成法特点,废水中Zn2 主要是在晶体生成阶段以Zn-Mg-Al三元LDH化合物形式被去除的。与化学沉淀法相比,即时合成法效果更好,适用pH值范围更广,用来处理含Zn2 废水更具优势。     

水滑石对水溶性染料活性深蓝ST-2GLN脱色性能研究

研究了水滑石(LDH)及其焙烧产物(LDO)吸附脱除水溶液中活性深蓝ST-2GLN的性能。考察了pH值、吸附剂投加量、时间等因素对吸附的影响。结果表明:LDH及LDO对活性深蓝ST-2GLN染料具有良好的脱除效果,室温下,1 g/L的LDH和0.5 g/L的LDO对浓度为100 mg/L的染料的脱色率分别达到96.11%和98.58%。pH值是影响吸附能力的关键因素,吸附剂对溶液pH值有一定缓冲作用。LDH及LDO对活性深蓝ST-2GLN吸附结果均符合Langmuir吸附等温式。饱和吸附后的LDH用高温热解法再生,再生产物吸附性能良好,随再生次数增多,脱色率下降。     

物理化学条件对合成Mg／Al-LDH结晶度和结构的影响

采用共沉淀法在不同物理条件下合成了一系列镁铝层状双氢氧化物(LDH),用化学分析、XRD和红外光谱对产物的组成与结构进行了表征,并探讨了初始溶液Mg/Al比、平衡pH值、水热反应温度、干燥温度等因素对合成LDH产物的结晶度、Mg/Al比、结构以及镁铝水解率的影响。结果表明,在实验条件范围内,最佳的合成条件为:初始Mg/Al比为2∶1,pH值为10,合成温度50℃,在此条件下固体产物为单一LDH物相,合成LDH的Mg/Al比为2∶1,镁铝水解率分别为99.21%和98.97%,结晶度高,可以实现在较低的温度下水热合成LDH。由于在LDH结构中Al3 替代Mg2 的量不同,导致X衍射分析d值和晶胞参数呈规律性变化。