HEDTA离子交换色层法分离重稀土

用2-羟乙基乙二胺三乙酸(HEDTA)作为淋洗剂,通过离子交换色层法分离重稀土元素钬和镥,研究室温条件下(25℃)淋洗剂的浓度、酸度、流速、柱比(吸附柱长度与分离柱长度的比值)等对钬、镥分离效果的影响.通过ICP-AES测定淋洗液浓度,绘制淋洗曲线,根据曲线中交叉区大小判断分离效果.结果表明:淋洗液的酸度是影响重稀土分离的关键因素,酸度越高,钬、镥分离效果越好,但分离周期越长;在一定范围内柱比越大,钬、镥分离效果越好,但柱比高于1:6时,分离效果下降.以钬、镥分离工艺进行镱、镥分离,也可以得到满意的分离效果.     

HL－P_（507）萃淋树脂色层法分离铥、镱、镥单一产品探索性试验研究

介绍了以ＨＬ－Ｐ（５０７）萃淋树脂为萃取色层材料，盐酸溶液作淋洗剂，从铥镱镥稀土富集物中提取大于９９％的Ｔｍ２Ｏ３、Ｙｂ２Ｏ３、Ｌｕ２Ｏ３单一产品的工艺试验，试验选择了合适的工艺条件包括铥镱镥富集物的分解、料液的制备、柱上色层分离、草酸沉淀和灼烧等工序．料液经色层梯度淋洗分部收集流出液即可得到大于９９％的Ｔｍ２Ｏ３、Ｙｈ２Ｏ３、Ｌｕ２Ｏ３单一产品。     

HL-P507萃淋树脂色层法分离铥、镱、镥单一产品探索性试验研究

介绍了以HL-P₅₀₇萃淋树脂为萃取色层材料, 盐酸溶液作淋洗剂, 从铥镱镥稀土富集物中提取大于99%的Tm₂O₃、Yb₂O₃, 、Lu₂O₃单一产品的工艺试验, 试验选择了合适的工艺条件包括铥镱镥富集物的分解、料液的制备、柱上色层分离、草酸沉淀和灼烧等工序。料液经色层梯度淋洗分部收集流出液即可得到大于99%的Tm₂O₃、Yb₂O₃、Lu₂O₃单一产品。      

HL—P507萃淋树脂色层法分离铥,镱,镥单一产品探索性试验研究

介绍了以ＨＬ－Ｐ５０７萃淋树脂为萃取色层材料，盐酸溶液作淋洗剂，从铥镱镥稀土富集物中提取大于９９％的Ｔｍ２Ｏ３、Ｙｂ２Ｏ３、Ｌｕ２Ｏ３单一产品的工艺试验，试验选择了合适的工艺条件包括铥镱镥富集物的分解、料液的制备、柱上色层分离、草酸沉淀和灼烧等工序。料液经色层梯度淋洗分部收集流出液即可得到大于９９％的Ｔｍ２Ｏ３、Ｙｂ２Ｏ３、Ｌｕ２Ｏ３单一产品。     

铥,镱,镥富集物全分离新工艺的研究

本研究采用P507-HCI体系进行Tm／Yb／Lu三出口萃取粗分离及P507萃淋树脂萃取色层分离提纯相衔接的方法，成功地实现了铥、镱、镥富集物的全分离，分别获得纯度大于99．95％的高纯Tm2O3、Yb2O3和Lu2O3产品，结果是令人满意的。本研究成果，在国内属高效、快速分离铥、镱、镥富集物的新工艺。对于进一步开发和应用我国南方的重稀土资源有较大的现实意义。     

铥、镱、镥富集物全分离新工艺的研究

本研究采用P₅₀₇-HCl体系进行Tm/Yb/Lu三出口萃取粗分离及P₅₀₇萃淋树脂萃取色层分离提纯相衔接的方法, 成功地实现了铥、镱、镥富集物的全分离, 分别获得纯度大于99.95%的高纯Tm₂O₃、Yb₂O₃和Lu₂O₃产品, 结果是令人满意的。本研究成果, 在国内属高效、快速分离铥、镱、镥富集物的新工艺。对于进一步开发和应用我国南方的重稀土资源有较大的现实意义。      

由还原渣提取高纯氧化铥和氧化镥新工艺研究

研究了以铥、镱、镥富集物经金属镧热还原法提取金属镱后所得的还原渣为原料，经酸溶配料，用稀土硫酸钠复盐沉淀除去镧，滤液用Ｐ５Ｓ７萃淋树脂萃取色层法提取高纯氧化铥、氧化镱，氧化镥（纯度均大于９９．９５％），并获得较高的收率。确定了稀土硫酸钠复盐沉淀除镧和萃取色层法分离铥、镱、镥的最佳分离条件。     

CL-P507-HCl体系萃取色层法分离铒、铥、镱

研究了用CL-P507-HCl体系萃取色层法分离铒、铥、镱,考察了树脂粒度、溶液温度、淋洗液酸度、树脂负载量、进样质量比等条件对分离效果的影响.结果表明,铥、镱之间存在着萃取抑制现象;以1.65 mol/L盐酸淋洗铒,1.90 mol/L盐酸淋洗铥和镱,在溶液温度50 ℃时可实现3者的分离;以99.9%氧化铥为原料,单柱一次分离可获得高纯铥溶液.     

同还原渣提取高纯氧化铥和氧化镥新工艺研究

研究了以铥、镱、镥富集物经金属镧热还原法提取金属镱石所得的还原渣为原料，经酸溶配料，用稀土硫酸钠复盐沉淀除去镧，滤液用Ｐ５０７萃淋树脂萃取色层法提取高纯氧化铥、氧化镱，氧化镥（纯度均大于９９．９５％），并获得较高的收率。确定了稀土硫酸钠复盐沉淀除镧和萃取色层法分离铥、镱、镥的最佳分离条件。     

冶金信息

1992年10月 23日,中国有色金属总公司对南方冶金学院部分科研成果进行了技术鉴定,通过鉴定的有下列成果: 由铥镱镥富集物直接提取 金属镱新工艺研究 长期以来国内外一直没有突破使用价格昂贵的单一纯氧化镱制取金属镱的冶炼方法。本成果采用P_(507)萃取分组所得铥镱镥氧化物富集物为原料,在高温真空条件下,通过还原-蒸馏的方法直接提取金属镱。本工艺具有原料价格便宜、镱的纯度和收率高(分别为>98％和>86％)、工艺过程稳定、技术先进、产品成本低的特点,属国际首创。     

氢电极预烧温度对丝网印刷YSZ电解质薄膜的影响

采用丝网印刷法制备了Y2O3稳定ZrO2(YSZ)电解质薄膜,并对固体氧化物电解池(SOEC)的NiO-YSZ氢电极预烧温度进行了优化。结果表明,NiO-YSZ氢电极适宜的预烧温度为1 000℃,YSZ电解质薄膜化后制备的SOEC在800℃、850℃和900℃三种电解温度下,1.50V时的产氢速率分别为386mL/(cm2.h)、255mL/(cm2.h)和142mL/(cm2.h)。采用丝网印刷法将YSZ电解质薄膜化制备后可以有效降低电解池的欧姆阻抗。     

Nonuniformity of NaOH concentration and effective bubble diameter in CO2 injection into aqueous NaOH solution

Mixed CO₂-N₂ gas was blown into an aqueous NaOH solution through a submerged nozzle of 3 mm ID, and the net absorption rate of CO₂ from the gas bubbles during their ascent was determined. The size distribution and the rising velocity of bubbles were also measured. The enhancement factor was estimated from the reported reaction rate constant as 1.16 to 8.20 at the NaOH concentration from 0.01 to 0.3 mol · dm^-3. It was deduced that NaOH concentration in the plume zone in which gas bubbles ascended was markedly lower than that of the bulk solution when NaOH concentration of the bulk solution was lower than 0.1 mol · dm^-3. The measured size distribution of bubbles had two peaks at approximately 0.15 and 2.3 cm. However, the effective bubble diameter defined as mean diameter based on the amount of absorbed CO₂ was 2.3 cm and it was close to the mean of larger bubbles.     

双环己酮草酰二腙光度法测定合金中高含量铜

以双环己酮草酰二腙（BCO）光度法快速测定合金中高含量铜,并对最佳显色条件进行了探讨。结果表明：在pH 8.5~10.0的氨水-氯化铵缓冲溶液中,铜与BCO形成蓝色络合物,该络合物的最大吸收波长为600 nm;BCO浓度为0.1 g/L;显色温度为20 ℃;显色时间是10 min;柠檬酸铵用量为1 mL。铜在0.4~4.0 μg/mL范围内符合比尔定律,表观摩尔吸光系数ε=1.6×10⁴ L·mol^-1·cm^-1。方法应用于高温合金及铜合金标准样品中高含量铜的测定,测定值与认定值相符,相对误差＜1.0%,相对标准偏差＜6.5%。     

真空蒸馏法制备高纯碲

采用真空蒸馏法提纯4N(99.99%)碲,在550℃、0.5Pa的动态真空条件下,大部分杂质从86×10-6降到7×10-6。延长冷凝段长度,蒸汽压比碲高的杂质(除Se外),即Cd、Zn和As明显减少。5N(99.999%)碲总的收率达到97%,平均蒸馏速度1.4×10-4g/(cm2.s)。     

Tritium permeation through clean incoloy 800 and sanicro 31 alloys and through steam oxidized incoloy 800

The tritium permeabilities,DK, of Incoloy 800 and Sanicro 31 have been determined for tube samples that were protected from surface oxidation by electroplated nickel. The permeabilities of these analogous alloys over the 400 to 750°C range were essentially equal;DK = 0.566 exp (-16120/RT) and 0.367 exp (-15610/RT cm³ (T2 · STP) · mm/(cmsu2 · min · torr^1/2), respectively. The effects ofin-situ steam oxidation of Incoloy 800 were observed to reduce tritium permeabilities by factors up to 400 at 150 days. Permeation rates through oxide-coated Incoloy 800 were observed to be 0.5 rather than 1.0 power dependent on the tritium pressure. Permeabilities of the oxides formed at 520, 660 and 725°C were determined to be 5.4 E-11, 4.9 E-10 and 2.4 E-9 cc (T₂,STP) · mm/(cm² · min · torr^1/2), respectively. Severe thermal shock was observed to essentially destroy the permeation barrier characteristics of the oxide coatings while mild temperature cycling had no observable effects on permeation rates through the oxide coated material. H. F. BITTNER formerly on the Research Staff, Oak Ridge National Laboratory.     

In vitro investigations of drug release and penetration--enhancing effect of ultrasound on transmembrane transport of flufenamic acid

Percutaneous absorption studies are performed in various in vitro models to determine the rate of drug absorption via the skin. We designed an phonophoretic drug delivery system to investigate the influence of ultrasound on transmembrane transport of different drugs. Phonophoresis is defined as the migration of drug molecules, contained in a contact agent, through the skin under the influence of ultrasound. We investigated the absorption of flufenamic acid in a buffer medium in dependence of ultrasound energy and application time. For evaluating membrane penetration of flufenamic acid, the concentration range of buffer solution was measured. Flufenamic acid was determined by using a fluorimetric method. Ultrasound energy was supplied for between 5 and 30 min at a range of intensities (0; 0.3; 0.6; 0.9; 1.2; 1.5 W/cm2). energy levels commonly used for therapeutic purpose. The pronounced effect of ultrasound on the transmembrane absorption of the drug was observed at all ultrasound energy level studied. The time of application was found to play an important role in delivery and transport of drug. Dependent on time, we observed an arise of temperature up to 4.5 degrees. It appears that there was no difference between an intensity of 0.3 and 1.5 W/cm2 and the measured drug concentrations in solution. The highest penetration was observed at an intensity of 1.0 W/cm2 after 30 min. These results were not significantly different from concentration in measurements after 30 min and 0.5 and 1.5 W/cm2. It seems that the arise of drug concentration is caused by effects of temperature and by variation of membrane delivery in dependence of temperature.     

离子交换法回收废钨催化剂碱浸液中钨的研究

用201树脂离子交换回收废钨催化剂碱浸液中钨,研究了交前液流速、温度及所含阴离子杂质对钨吸附的影响和不同解吸剂解吸钨的影响。结果表明,交前液的流速从2．0mL／min增加到8．0mL／min,WO3的饱和交换容量从332．9mg／g减少到150．9mg／g。当交前液含10g／LAlO2、10g／L,CO3^2-和5g／L OH^-时．饱和交换容量相应减少为169．2、201．6和231．04mg／g。用2mol／LNaCl和1mol／LNaOH的混合液解吸效果好,解吸率可达98．2％。     

离子色谱法测定废气中甲酸

采用离子色谱法分离电导检测废气中甲酸的含量。考察Dionex IonPac AS18和Ion-PacAS11-HC色谱分离柱在不同淋洗液浓度条件下对甲酸的分离效果,淋洗液流速对分离的影响。讨论绘制校准曲线时标准溶液介质的选择。结果表明:当用Dionex IonPac AS18柱,5mmol/L氢氧化钾为淋洗液,以1.0 mL/min的淋洗速度进行梯度洗脱并用吸收液配制校准曲线的标准溶液时可达到预期废气中甲酸分析的目的。该法线性范围为0.1~10 mg/L和10~100 mg/L,检出限为0.007 mg/m3。用本法测定甲酸生产装置30 m高度排气筒废气中的甲酸回收率为88%~104%。     

利用选钛尾矿制备微晶泡沫玻璃及其性能研究

利用攀枝花选钛尾矿为主要原料,添加硼砂助熔剂经熔融、水淬、发泡、微晶、退火等系列工艺制备出微晶泡沫玻璃。研究了发泡剂种类、用量及稳泡剂用量、发泡时间、发泡温度、微晶化温度及时间等因素对微晶泡沫玻璃的表观密度、抗压强度和吸水率的影响。并通过SEM扫描分析制备的试样,内部出现充满连通且封闭的不规则气泡,孔壁较厚,体积膨胀明显的多孔状结构。研究结果表明:当发泡剂CaCO_3的添加量为2%,稳泡剂Na_3PO_4·12H_2O的添加量为5%时,在发泡温度840℃时发泡20 min,550℃微晶化处理90 min后可以制备孔径1.8~2.2 mm,表观密度1.31g/cm~3,抗压强度16.7 MPa,吸水率为11.3%的微晶泡沫玻璃。     

Effect of composition of starting materials of Mo–Si on self-propagating high temperature SHS reaction

Abstract

An experimental study of the self-propagating high temperature synthesis of Mo–Si alloys was conducted from elemental powder compacts. Test specimens with seven compositions, including Mo/Si?=?1∶1·25, 1∶1·50, 1∶1·75, 1∶2·00, 1∶2·25, 1∶2·50 and 1∶2·75 respectively, were employed. Experimental evidence showed that a combustion wave featuring a spinning reaction zone can be observed. When the powder compacts are from Mo∶1·25Si to Mo∶1·75Si, the combustion temperature and the propagation velocity of combustion wave increase with increasing silicon in the sample, and the combustion products are composed of MoSi₂, Mo₅Si₃ and Mo. However, when the powder compacts are from Mo∶2·25Si to Mo∶2·75Si, the combustion temperature and the propagation velocity decrease rapidly as the silicon in the compact increases, and the combustion products are composed of MoSi₂ and Si. The sample with Mo/Si?=?1∶2·00 possesses the highest combustion temperature (1628·9 K) and propagation velocity (3·13 mm s^?1). A single-phase MoSi₂ is synthesised by the Mo/Si?=?1∶2·00 sample.