低碱度共沉淀法制备苯选择加氢Ru-Zn催化剂

在低碱度下采用共沉淀法成功制备了非负载型Ru-Zn催化剂,用于苯选择加氢制环己烯反应.固定氢氧化钠沉淀剂的量,考察了不同氯化锌加入量对催化剂结构和催化性能的影响,采用N2吸附、X射线衍射和程序升温还原等手段对催化剂进行了表征.同时考察了选用具有最佳锌含量的Ru-Zn催化剂时搅拌速度和硫酸锌添加剂等对催化反应性能的影响,最后考察了催化剂多次使用时的反应性能.研究表明, Zn含量16.7%(质量分数)的Ru-Zn催化剂具有最佳的催化性能;在ZnSO4水溶液(0.45 mol/L)中,优化反应条件(哈氏合金釜,1200 r/min,150oC, H2压5 MPa)下反应45 min,苯转化率57%时环己烯选择性可达80%(收率超过45%).钌催化剂中ZnO晶体对于环己烯选择性达到80%非常重要.催化剂回收循环反应5次时反应性能基本不变,表明低碱度下制备的催化剂具有良好的稳定性,显示了工业化应用前景.     

Coprecipitation‐assisted coacervative extraction coupled to high‐performance liquid chromatography: An approach for determining organophosphorus pesticides in water samples

An analytical methodology based on coprecipitation‐assisted coacervative extraction coupled to HPLC‐UV was developed for determination of five organophosphorus pesticides (OPPs), including fenitrothion, guthion, parathion, methidathion, and chlorpyrifos, in water samples. It involves a green technique leading to an efficient and simple analytical methodology suitable for high‐throughput analysis. Relevant physicochemical variables were studied and optimized on the analytical response of each OPP. Under optimized conditions, the resulting methodology was as follows: an aliquot of 9 mL of water sample was placed into a centrifuge tube and 0.5 mL sodium citrate 0.1 M, pH 4; 0.08 mL Al₂(SO₄)₃ 0.1 M; and 0.7 mL SDS 0.1 M were added and homogenized. After centrifugation the supernatant was discarded. A 700 μL aliquot of the coacervate‐rich phase obtained was dissolved with 300 μL of methanol and 20 μL of the resulting solution was analyzed by HPLC‐UV. The resulting LODs ranged within 0.7–2.5 ng/mL and the achieved RSD and recovery values were <8% (n = 3) and >81%, respectively. The proposed analytical methodology was successfully applied for the analysis of five OPPs in water samples for human consumption of different locations of Mendoza.     

自组装硫化铜微米管的制备及可见光催化性能

以二水合氯化铜为铜源,硫代乙酰胺为硫源,通过共沉淀法成功合成了自组装CuS微米管,该合成方法简单、反应条件温和,是合成纳米材料的一种有效方法。通过扫描电子显微镜（SEM）考察反应时间对产物形貌的影响,并初步研究其形成过程。X射线衍射（XRD）表征产物是CuS。通过改变光催化实验的条件,如催化剂的量、溶液pH值、活性橙的浓度,研究了样品在可见光下对活性橙的光催化性能。     

Coprecipitation Synthesis of a Superconductor via Multi‐Precipitants

A precipitation process has been developed to prepare precursor powders, which can be calcined and sintered to form high‐Tc superconductors such as YBa₂Cu₃O_y. Precursor powders are prepared using a mixed‐precipitants system in which a solution contains precipitating anions such as hydroxide, oxinate and oxalate ions. A theoretical study on the conditions of mixed‐precipitants coprecipitation is performed. The solution pH of complete precipitation of the title system is extended and is maintained between 4.46 and 12.0. A series of experiments were conducted to confirm the as‐derived optimal condition. Finally, characterization of the properties of the YBa₂Cu₃O_y obtained after high temperature treatment is reported.     

Inductively coupled plasma atomic emission spectrometric determination of 27 trace elements in table salts after coprecipitation with indium phosphate

The coprecipitation method using indium phosphate as a new coprecipitant has been developed for the separation of trace elements in table salts prior to their determination using inductively coupled plasma atomic emission spectrometry (ICP-AES). Indium phosphate could quantitatively coprecipitate 27 trace elements, namely, Be, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, Cd, Pb, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu, in a table salt solution at pH 10. The rapid coprecipitation technique, in which complete recovery of the precipitate was not required in the precipitate-separation process, was completely applicable, and, therefore, the operation for the coprecipitation was quite simple. The coprecipitated elements could be determined accurately and precisely by ICP-AES using indium as an internal standard element after dissolution of the precipitate with 5 mL of 1 mol L⁻¹ nitric acid. The detection limits (three times the standard deviation of the blank values, n = 10) ranged from 0.001 μg (Lu) to 0.11 μg (Zn) in 300 mL of a 10% (w/v) table salt solution. The method proposed here could be applied to the analyses of commercially available table salts.     

表面活性剂辅助共沉淀法制备Ni-Mg-Al固体碱催化剂用于CH_4-CO_2重整反应

采用表面活性剂辅助共沉淀法制备了Ni-Mg-Al固体碱催化剂并用于CH4-CO2重整反应,探讨了表面活性剂对Ni(111),Ni(200)晶面的择优取向作用,在800℃下比较了不同表面活性剂制备的催化剂的催化性能,详细考察了CTAB制备的催化剂CB-LDO在不同反应温度下的催化活性和稳定性.采用红外光谱、X射线衍射、程序升温还原、X射线光电子能谱、高分辨透射电镜和程序升温氧化等表征手段分析了催化剂的活性、稳定性和失活原因.结果表明,四丙基氢氧化铵(TPAOH)促进Ni(200)的生长,而聚氧乙烯-聚氧丙烯-聚氧乙烯(P123)、聚乙烯吡咯烷酮(PVP)和十六烷基三甲基溴化铵(CTAB)抑制Ni(200)晶面的生长;Ni(200)的结晶程度对CH4的活化起到关键的作用,催化剂CB-LDO在高温下反应会发生晶型的转化,Ni(200)晶面由于反应过程中生成NiAl2O4尖晶石而得到缓慢释放,使催化剂的活性得以维持较高的水平.     

碳酸钙共沉淀-火焰原子吸收光谱法测定卤水中的痕量钴

以碳酸钙共沉淀,用火焰原子吸收光谱法测定卤水中的痕量钴,对试剂的加入量富集时间,酸度等因素进行了实验,选择了最佳的共沉淀条件.方法已用于卤水分析,加标回收率:钴94.6%-98.7%.检出限:钴为1.89μg·L-1.本法测定手续简便、快速、结果满意.     

污泥生物淋滤过程中黄铁矾对重金属离子的吸附与共沉淀作用的模拟研究

生物淋滤处理可加速污泥中重金属(Zn,Cu和Cr)的溶出.但在淋滤后期,约有31%的已溶出的Cu2 被重新固持.并且,Cu2 浓度的再次下降与Fe3 沉淀形成黄铁矾的反应在时间上具有同步性.为阐明Cu2 固持机理,文章利用氧化亚铁硫杆菌的生物催化氧化作用,模拟生物淋滤环境在纯体系合成了黄铁矾.吸附试验表明,在pH 2.0～2.5的范围内(污泥生物淋滤过程中重金属溶出范围),黄铁矾对10 mg·L-1Cu2-(该浓度与供试污泥生物淋滤中的Cu2 浓度相近)的吸附率低于9%,不能完全解释Cu2 的重新固持现象.共沉淀试验表明,Cu容易与黄铁矾形成共沉淀而掺入矿物的晶格.当Cu2 为10 mg·L-1时,约有44.6%的Cu2 与黄铁矾产生共沉淀而进入固相.可以认为,Cu与黄铁矾的共沉淀效应,是导致污泥生物淋滤后期Cu2 浓度再次下降的主要原因,黄铁矾对Cu2 的吸附只起极小的作用.     

Soft chemistry synthesis of the perovskite CaCu3Ti4O12

The perovskite CaCu₃Ti₄O₁₂ (CCT) has been obtained after calcination of oxalate precursors at 900–1000 °C in air. Those precursors are prepared using a soft chemistry method, the coprecipitation. The oxalate powders consist of disk-like particles of 2–3 μm diameter and 300–400 nm thickness. By varying the ratio of the initial amounts of metal chlorides, additional phases (CaTiO₃, TiO₂ and CuO) could be obtained besides CCT. The corresponding multiphased ceramics present improved dielectric properties.     

8-羟基喹啉快速共沉淀分离富集原子吸收光谱法测定啤酒中的Cu和Pb

研究了用8-羟基喹啉-Mg(Ⅱ)共沉淀体系,以Mn(Ⅱ)为内标,快速共沉淀分离富集啤酒中的铜和铅,并用火焰原子吸收光谱(FAAS)测定的方法.共沉淀受pH值、载体镁和内标锰用量的影响.结果显示在pH为9的条件下,能够定量共沉淀试样中的铜和铅.当试液为100 mL时,方法的检出限分别为铜6.28×10-3 μg·mL-1,Pb 2.26×10-2 μg·mL-1回收率为97.6%～103.0%,基本消除了基体干扰,取得了较为满意的结果.该方法无需收集全部沉淀,与传统的共沉淀方法比较,克服了收集沉淀费时的缺点.方法快速、简便、重现性好.