ScF_3的水热法制备及掺Ce~(3+)光谱性质研究

首次用低温水热法制备了ScF_3晶体及其掺杂Ce~(3+)的粉体.通过X射线粉末衍射(XRD),扫描电镜(SEM),荧光光谱(FS)对样品进行了表征.结果表明,所用氟化物的种类和反应温度对ScF_3的制备至关重要.以NaF作为原料更容易得到纯的ScF_3.当水热温度为120℃时,产物为ScF_3晶体,而温度升高至180℃时则为NaScF4复合氟化物.所制备的ScF_3呈针尖棒状放射形.考察了ScF_3:Ce~(3+)粉体荧光光谱性质,讨论了其与同类型的稀土氟化物的荧光光谱的比较.     

水浸液P507转型制备低杂质混合氯化稀土

工业上水浸液通过P507转型多采用一步转型的工艺,得到的混合氯化稀土非稀土杂质含量较高。通过改变工艺方式,采用模拟逆流串级等工艺制备混合氯化稀土,考察反萃液中非稀土杂质含量的变化。研究结果证明,采用逆流串级工艺,当萃取混合时间大于9 min,料液酸度在pH=4,洗涤液酸度pH=1.5,反萃相比为20,反萃液酸度为6 mol/L时,反萃液中Mn4+、Zn2+、SO42-、Mg2+、Ca2+的含量较原工艺下降50%以上。     

Hydrothermal Synthesis and Characterization of Pyrochlore Titanate R2Ti2O7(R=Gd3+, Tb3+, Dy3+)

Pyrochlore titanate oxides, R2Ti2O7(R=Gd3+, Tb3+, Dy3+), were synthesized under mild hydrothermal conditions. The crystal growth of pyrochlore titanate oxides and taking place of chemical reaction in the hydrothermal processing were sensitive to the alkalinity, temperature, reaction time, the nature of the rare earth ion and the composition of initial reaction mixture. The as-prepared samples were characterized by powder X-ray diffraction, scanning electron microscopy, Raman spectrum and variable temperature dc magnetic susceptibility(Superconductivity quantum interference device, SQUIDS). The magnetic studies gave 7.29×10-23 A·m2/Gd3+ and -8.28 K, 8.75×10-23 A·m2/Tb3+ and -19.7 K, and 8.85×10-23 A·m2/Dy3+ and 0.84 K effective moments and Weiss constants for Gd2Ti2O7,Tb2Ti2O7 and Dy2Ti2O7, respectively.     

Synthesis and Structures of A Series of Novel Rare Earth Transition Metal Sulfates

Seven new rare earth transition metal sulfates were synthesized by hydrothermal reactions under conditions slightly above the critical point of water. Their crystal structures were determined from single crystal X-ray data. The compositions of the new compounds can be represented by two general formulae ： REM （OH） 3 （SO4） and RE2M （OH） 3 （SO4） 2F （H2O） with RE = Gd, Tb, Dy ; M = Ni, Cu. Three different crystal structure types were found for the formula REM （OH） 3 （SO4）. The structures of the new compounds all feature infinite chains of REOn coordination polyhedra, which are connected to chains of CuO6 or NiO6 octabedra. The limited size range of the rare earth cations observed in these compounds is most likely because of interactions between the octabedral chains and the chains of REOn polyhedra. The new compounds are closely related to the known yttrium transition metal sulfates.     

土壤中可给态稀土元素的研究进展

本文综述了土壤中可给态稀土元素与植物生长的相关性，土壤中可给态稀土浸提剂的选择以及定量测定方法的研究，详细讨论了我国主要土壤中可给态稀土元素的含量、分布及其影响因子，并提出在今后研究中应值得关注的几个方面，为合理施用稀土微肥提供科学依据。     

硅钼蓝分光光度法测定氟化稀土中二氧化硅

氟化稀土是一种用途广泛的材料,其中二氧化硅的含量是衡量产品品质的一个关键指标,直接影响生产合金的工艺和产品的质量。实验采用碳酸钠-硼酸混合熔剂(m_碳酸钠:m_硼酸=4:1)熔融试样,经盐酸酸化,加入0.4 mL硫酸(1+5)控制显色体系的pH≈1,正硅酸与钼酸铵沸水浴保温时间为3～5 s时形成硅钼杂多酸,用草酸-硫酸混合酸破坏磷、砷等干扰元素,抗坏血酸还原硅钼杂多酸为硅钼蓝,建立了光度法测定氟化稀土中二氧化硅含量的方法。试验表明,显色液中二氧化硅质量浓度在0.04～2.0 μg/mL范围内符合比尔定律,方法中二氧化硅的检出限和测定下限分别为0.002 8%和0.010%(质量分数)。方法用于3个氟化稀土实际样品中二氧化硅量的测定,结果的相对标准偏差(RSD,n=10)为2.3%～5.2%;测定值与电感耦合等离子体原子发射光谱法(ICP-AES)的测定结果一致。     

纳滤膜对稀土离子的动态吸附行为及截留特性

采用经碳纳米管改性的亲水化纳滤膜浓缩提取稀土浸出液中的稀土离子,探究纳滤膜表面对La3+、Nd3+、Pr3+、Ce3+和Y3+5种稀土离子吸附动力学行为,考察稀土离子半径的大小对纳滤膜吸附性能和截留性能的影响.结果表明,Freundlich吸附方程比Langmuir方程能更好地描述稀土离子在纳滤膜表面上的动态吸附行为,用Freundlich吸附方程拟合后的结果相关度系数R2能达到0.999以上;在初始浓度为5×105 μg/L,温度为25 ℃,运行压力为0.6 MPa的实验条件下,纳滤膜对稀土离子的浓缩提取过程中,初始阶段的截留机理取决于纳滤膜表面的吸附作用和膜孔的机械筛分效应,膜面吸附达到平衡后以膜孔的机械筛分效应为主,此时La3+、Nd3+、Pr3+、Ce3+和Y3+的截留率分别为94.21 %、81.25 %、85.80 %、89.90 %和81.18 %,表明经碳纳米管改性的亲水化纳滤膜能高效浓缩截留稀土浸出液中的稀土离子.      

纳滤浓缩稀土母液沉淀上清液的实验研究

以赣州某稀土公司浸矿所得稀土母液经NH₄HCO₃除杂沉淀后的上清液为处理对象,主要研究纳滤技术对原液中稀土离子的浓缩效率,以及对NH₃-N分离回收情况,以期能够为工业化分离应用提供借鉴.实验表明,当原液中稀土离子浓度为142.9 mg/L,氨氮浓度为346.1 mg/L时,在操作压力为0.8 MPa,进水pH值为6.49,运行温度为25 ℃的条件下,浓缩液侧稀土离子截留率达到95 %以上,Ca2+、Mg2+、Mn2+、Zn2+等杂质离子截留率能够达到75 %~90 %,透过液侧氨氮浓度为原浓度的60 %左右,有一定的浓缩效果;6.0 L的稀土母液沉淀上清液浓缩至0.6 L时,RE3+浓度升高至1 242.0 mg/L,浓缩了近8.69倍.      

Study on Anticoagulation Factor I from Agkistrodon Acutus Venom by Rare Earth Ion Probes

Ｓｎａｋｅｖｅｎｏｍｓｃｏｎｔａｉｎｃｏｍｐｌｅｘｐｒｏｔｅｉｎｓｗｈｉｃｈｐｏｓｓｅｓｓｖａｒｉｏｕｓｂｉｏｌｏｇｉｃａｌａｃｔｉｖｉｔｉｅｓ ,ｉｎ ｃｌｕｄｉｎｇａｃｌａｓｓｔｈａｔａｆｆｅｃｔｓｃｏａｇｕｌａｔｉｏｎｓｙｓｔｅｍｗｉｔｈｃｏａｇｕｌａｎｔｏｒａｎｔｉｃｏａｇｕｌａｎｔａｃｔｉｖｉｔｉｅｓ .Ａｎａｎｔｉｃｏａｇｕｌａｎｔｆａｃｔｏｒ (ＡＣＦ)ｗａｓｐｒｅｖｉｏｕｓｌｙｉｓｏ ｌａｔｅｄｆｒｏｍｔｈｅｖｅｎｏｍｏｆＡｇｋｉｓｔｒｏｄｏｎａｃｕｔｕｓｆｒｏｍｓｏｕｔｈｅｒｎＡｎｈｕ…     

Stability of Rare Earth Ion-N, N′-bis（2′-Pyridine）methyl-1,10-Phenanthroline-2,9-Dimethanmine Binary Complexes

1 ,10 Phenanthrolinehasbeenextensivelyusedasanazaheterocyclicchelateligandinbothanalyticalandpreparativecoordinationchemistry[1] .Asanim portantligand ,1,10 phenanthrolineunitplaysanim portantroleforthedevelopmentofthesupramolecularchemistry .Manynovelsupramolecularcompoundsin clude 1,10 phenanthrolineunit[2～ 4 ] .Furthermore ,consideringtheuniquecombinationofchemicalstabil ities ,redoxproperties ,luminescenceemissionandex citedstatelifetime ,derivativesof 1,10 phenanthrolinehaveplayedama…     

Primary Study on Effects of New Rare Earth Agro-Materials on Potato

Using common phosphate as a check, we studied the growth and yield of potato by new rare earth agro-materials including rare earth phosphate (base fertilizer), rare earth whole plant nutrient fertilizer, and amino acid chelated rare earth ( top dressing), which were used in a single or mixed way in Dingxi city, Gansu Province.The results are as follows that ( 1 ) After using new rare earth materials, the plant height increases by 0.4 ～ 5.6 cm and the ripen period is delayed by 4 ～ 9 d.(2) They can improve the potato economic characteristics, enhance productivity, decrease black leg and late blight.The disease index is decreased by 1.6% ～ 10.6%, single plant potato number increases by 0.3 ～ 0.5, and single plant yield increases by 80 g ～ 130 g.(3) The effect of increased yield is significant, and mixed use is better than single use.In the single material treatments, rare earth phosphate is the best, rare earth whole plant nutrient fertilizer and amino acid chelated rare earth are the second, and the increased rate are 14.5%, 8.4%, 9.2% so the material mixture-rare earth phosphate mixed of rare earth whole plant nutrient fertilizer or with amino acid chelated rare earth is economically useable, and increase rate are 25.2% and 24.4% compared with common phosphate.     

2,3,5-吡啶三酸与重稀土配合物的合成、表征及光致发光性质

采用水做溶剂,用2,3,5-吡啶三酸做配体和重稀土铽、镝、铒、镱、镥、钇六种稀土元素的氯化物在常温下反应合成了六种重稀土的配合物。通过EDTA络合滴定分析,确定了六种配合物中稀土离子含量;并对配合物进行了熔点测定、红外光谱测试,并测试了铽和镝配合物的光致发光性质,结果表明,铽和镝配合物在紫外光的激发下具有良好的发光性质。     

Decomposition of the mixed rare earth concentrate by microwave-assisted method

A novel process was proposed to strengthen the decomposition of the mixed rare earth concentrate by utilizing the microwave radiation.Mineralogical information on the mechanisms by which microwave heating improved the leaching behavior of rare earth elements(REEs),and an interpretation of the interrelationship between mineralogy,decomposition process,and leaching process were provided in this study.The influences of the temperature,time of microwave heating and contents of NaO H(mass ratio of NaO H to mixed rare earth concentrate)on the decomposition of mixed rare earth concentrate were investigated.The results revealed that the temperature was the main factor affecting the decomposition process.The recovery of REEs by hydrochloric acid leaching reached 93.28% under the microwave heating conditions:140 oC,30 min and 35.35% NaO H.The BET specific surface area and SEM analysis indicated that the particles of mixed rare earth concentrate were non-hole,while the particles presented a porous structure after heating the concentrate by microwave radiation.For the microwave treated sample after water leaching,the BET specific surface area was 11.04 m~2/g,which was higher than the corresponding values(6.94 m~2/g)for the mixed rare earth concentrate.This result could be attributed to the phase changes of bastnaesite and monazite,and a number of cracks induced by thermal stress.The increase of BET specific surface area resulted in an increase of the recovery of REEs by promoting interaction within the system of acid leaching.     

Decomposition Reaction of Mixed Rare Earth Concentrate and Roasted with CaO and NaCl

The reaction of the mixed rare earth concentrate including monazite ( REPO4 ) and bastnaesite ( REFCO3 )decomposed by CaO and NaCl additives at the temperature range from 100 to 1000 ℃ was studied by means of XRD and TG-DTA.The results show that when CaO and NaCl are not added, only REFCO3 can be decomposed at the temperature of 377 ～ 450 ℃.The decomposition products include REOF, RE2O3 and CeO2.However, REFCO3 can not be decomposed.When CaO is added, the decomposition reactions occur at the temperature range from 660 to 750 ℃.CaO has three decomposition functions: ( 1 ) REPO4 can be decomposed by CaO and the decomposition products include RE2O3 and Ca3 (PO4)2; (2) CaO can decompose REOF, and the decomposition products are RE2O3 and CaF2; (3)CaO can decompose REPO4 with CaF2, and the decomposition products are RE2 O3, Ca5 F( PO4 )3.The decomposition ratio of the mixed rare earth concentrate increased obviously, when CaO and NaC1 were added.NaC1 can supply the liquid for the reaction, improve the mass transfer process and accelerate the reaction.At the same time, NaC1 participated in the reaction that REPO4 was decomposed by CaO.     

Geochemistry of Rare Earth Elements in Aktishikan Gold Deposit,Xinjiang

The characteristics and the models of rare earth elements in the geological bodies and the hydrothermal water balancel with the adamellite were comprehensivealy studied in Aktishikan gold deposit,Nurt area of Altay,Xinjiang,And the behavior of rare earth elements during metasomatic alteration was discussed by using the isocon method of Grant,The results show that the rare earth elements are inert during metasomatic alteration,the hydrotheraml water has no relation to the magmatic water,and the gold material sources mainly stem from the wall rock.     

Synthesis,crystal structures of novel complexes of rare earth with norfloxacin,interaction with DNA and BSA

Three novel rare earth complexes [N(CH 3) 4 ][Ln(NF) 4 ]·6H 2 O(Ln=Nd(III)(1),Sm(III)(2),Ho(III)(3)) were synthesized using hydrothermal method from norfloxacin HNF=1-ethyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl)-3-quinoline carboxylic acid,C 16 H 18 FN 3 O 3),imidazole and rare earth nitrates.The complexes were characterized by elemental analysis,FT-IR,TG-DTG and X-ray single crystal diffraction.Each rare earth ion was eight-coordinated with carboxyl-O atoms and keto-O atoms from norfloxacin.Four of the norfloxacin ions acted as bidentate chelate group took part in the coordination with rare earth ion.The structures of complexes were tetragonal system with space group I4 1 /acd,which were allomerism.The interaction between complex 1 and DNA was studied by electronic absorption spectra and fluorescence spectroscopy.The binding interaction between the complex 1 and bovine serum albumin(BSA) was studied by fluorescence spectroscopy.The complex 1 bound to DNA by the mode of partial intercalation.Complex 1 had a strong ability to quench the fluorescence from BSA.The complex interaction was mainly a static quenching process with BSA together with formation of two binding sites.     

混合稀土La-Ce对一种抗冲击防护钢组织与冲击性能的影响

为了研究不同混合稀土含量下一种抗冲击防护钢的冲击性能,对钢在室温和-40℃低温冲击性能进行测试,并对其冲击断口形貌及显微组织进行观察分析。结果表明,试验钢中加入混合稀土La-Ce后,改善了回火马氏体组织、细化了奥氏体晶粒,同时,变质了钢中的夹杂物,长条状的MnS夹杂物变质为球状复合稀土夹杂物,夹杂物尺寸由6μm减小到2μm;与不含稀土的试验钢相比,含混合稀土试验钢的室温冲击性能和-40℃低温冲击性能均有所提高,混合稀土La-Ce含量为102×10^-6时,防护钢的室温冲击功增加了24.5%,-40℃低温冲击功增加了17.4%。     

Rare earth recovery from fluoride molten-salt electrolytic slag by sodium carbonate roasting-hydrochloric acid leaching

Fluorinated rare earth molten-salt electrolytic slag contains a considerable amount of rare earth elements,as well as a variety of heavy metals and fluorides that cause environmental pollution.Therefore,it is of great importance to fully utilise this resource.In this study,the transformation mechanism of fluorinated rare earth molten-salt electrolytic slag roasted with sodium carbonate,and the regulation mechanism of rare earth leaching under different roasting conditions were investigated with ...     

溶样方法对电感耦合等离子体质谱法测定岩石和土壤中稀土元素的影响

基于电感耦合等离子体质谱法(ICP-MS)测定稀土元素的优势,在优化仪器工作参数的基础上,探究了敞口混合四酸法(HNO₃-HCl-HF-HClO₄)、敞口混合五酸法(HNO₃-HCl-HF-HClO₄-H₂SO₄)和高压密闭法(HNO₃-HCl-HF)3种溶样方法对ICP-MS测定岩石和土壤中稀土元素的影响。结果表明:敞口混合四酸法因样品消解不完全不适宜用于ICP-MS测定岩石和土壤中稀土元素;敞口混合五酸法和高压密闭法均可以实现ICP-MS对岩石和土壤中稀土元素的测定;敞口混合五酸法结合ICP-MS测定稀土元素的方法检出限为0.001~0.035μg/g,相对标准偏差为1.4%~6.4%,相对误差在±9%范围内,加标回收率为92%~110%;高压密闭溶样法的检出限为0.001~0.009μg/g,相对标准偏差为1.0%~9.2%,相对误差在±4%范围内,加标回收率为93%~107%。敞口混合五酸法具有处理流程短的优点,适用于大批量样品处理;高压密闭溶样法具有检出限低,测试精度高及用酸量少等特点,但处理流程长不适用于大批量样品处理。     

Effect of roasting activation of rare earth molten salt slag on extraction of rare earth,lithium and fluorine

A new process was proposed to extract rare earth elements(REEs),Li and F from electrolytic slag of rare earth molten salt by synergistic roasting and acid leaching.Firstly,the thermodynamic analysis of roasting reaction was carried out,then the effects of roasting factors on leaching REEs,Li and F in slag were investigated.In additions,the mineral phase and morphology of molten salt slag,roasting slag and acid leaching slag were characterized,and the migration mechanism of REES,Li and F minerals...