过氧化氢分光光度法测定湿法提钒工艺中钒

为了提高湿法提钒工艺过程控制效率,采用以过氧钒离子(VO(O₂)⁺)显色特性为基础的过氧化氢分光光度法测定钒含量,实现了样品中钒含量的现场快速测定。首先通过在试样溶液中加入适量氢氧化钠溶液,调整溶液pH值至9～10,然后加入过氧化氢将低价态钒全部氧化至钒(V),再加入硫酸调整溶液至酸性,钒(V)与过氧化氢在室温下形成稳定的红棕色过氧钒离子(VO(O₂)⁺),于450 nm处测定吸光度。钒质量浓度在2.0~400 mg/L内与吸光度值符合比尔定律。采用实验方法测定3种湿法冶金提钒液体试样(包括钒浸取溶液、钒盐沉淀后溶液以及废水等)中钒,结果的相对标准偏差(RSD,n=10)分别为0.38%、3.5%和7.6%;与高锰酸钾氧化-硫酸亚铁铵滴定法结果相一致。     

Catalytic spectrophotometric determination of trace vanadium in fly ash and coal gangue by Triton X-1O0 enhancing effect

Trace Ⅴ(Ⅴ) catalyzes mightily the decolorization reaction of arsenazo Ⅲ(AsA Ⅲ) by oxidizing with H2O2 in a pH 4.0 HAc-NaAc buffer solution, and the addition of Triton X-100 can further increase the sensitivity of the reaction and its catalytic extent is linear with the content of Ⅴ(Ⅴ). A catalytic spectrophotometric procedure for determining trace Ⅴ(Ⅴ)was developed. The results show that the maximun absorption of the color solution is at 560 nm and the detection limit of the method for Ⅴ(Ⅴ) is 0.014 mg.L^-1. Beer‘s law is obeyed for Ⅴ(Ⅴ) in the range of 0.00-0.20 mg.L^-1.The recoveries are 99.0%-104.6%, and the relative standard deviations (RSD) are 2.7%-3.7%. Combined with ion-exchange resin, the method has been applied to the determination of trace vanadium in fly ash and coal gangue with satisfactory results.     

钼酸铵在氢气气氛中的还原行为

通过Ｘ射线衍射（ＸＲＤ）分析，研究了三种多相钼酸铵在高温下的氢还原行为。结果表明，高温下氢气气氛中，钼酸铵首先发生热分解的，生成ＭｏＯ３，再发生还原生成ＭｏＯ２。热分解过程形成（ＮＨ４）２Ｍｏ１４Ｏ４３和（ＮＨ４）２Ｍｏ２２ｏＯ６７中间相，这些中间相在氢气气氛中要较空气气氛中更稳定。ＭｏＯ３在还原过程中形成ＭｏＯ２＼８０和Ｍｏ４Ｏ１１中间相。     

模具盐浴稀土钒硼共渗的组织与性能

研究了Ｃｒ１２Ｍｏｖ．Ｃｒ１２，９ＣｒＳｉ和Ｔ８等钢的盐浴稀土钒硼共渗共艺，渗层组织与性能；讨论了共渗工艺参数、共渗剂成分配比及稀土元素添加量等因素对共渗层的影响。冷作模具的使用寿命经ＲＥ－Ｖ－Ｂ共渗处理后比常规工艺处理的提高３～７倍。     

FCC捕钒剂的研究进展

论述了钒在催化裂化过程中的危害及危害机理，对捕钒剂的捕钒机理及实验室评价方法作了叙述，介绍了国外几种捕钒剂产品及应用效果。     

硫化氢与钾碱脱碳液中五价钒价态变化初探

从理论和实践两方面研讨了进入钾碱脱碳液中H2S对五价钒的还原行为。通过一系列计算以及现场生产监测数据的整理分析，提出了H2S在工艺条件下对五价钒还原的新认识，为合理确定H2S控制指标提供了一个可借鉴的依据。     

（Nb_yTi_（1－y））C_x单晶体制备及其结构研究

用熔剂法制备了（Ｎｂ＿ｙ．Ｔｉ＿（１－ｙ））Ｃ＿ｒ单晶体，用Ｄｅｂｙｅ照相法及四圆衍射仪对其晶体结构进行了研究。实验结果表明，（Ｎｂ＿ｙＴｉ￣（１－ｙ）Ｃ＿ｘ中存在类似于作化学计量化合物ＴｉＣ＿ｘ及ＮｂＣ＿ｘ的有序一无序转变现象，转变温度随其化学成份改变在１１７５～１２８０Ｋ范围内变化。高温型（Ｎｂ＿ｙＴｉ￣（１－ｙ））Ｃ＿ｘ的晶体结构属ＮａＣｌ型结构，碳空位呈随机分布；低温型（Ｎｂ＿ｙＴｉ￣（１－ｙ））Ｃ＿ｘ的晶体中碳空位呈短程有序分布，可用Ｖ＿６Ｃ＿５晶体结构模型进行描述。     

钒硅中孔分子筛的合成、表征及其催化性能研究

在碱性环境中，采用水热合成法制备得到了不同硅钒比的钒硅中孔分子筛V－MCM－41，利用XRD，IR，TG等表征方法考察了钒的搀杂量与其结构和性能之间的关系，该催化剂对苯乙烯氧化反应具有较好的催化活性，在一定的反应条件下，以H2O2溶液（30％）为氧化剂，以乙腈为溶剂，V－MCM－41（Si/V=25)能使苯乙烯的转化率达到95％以上，产物（苯甲醛＋苯甲酸）的选择性不低于90％。     

在VPO催化剂上丁烷选择氧化的质谱研究

The selective oxidation of n-butane to maleic anhydride(MA) on a vanadium-phosphorus oxide (VPO) catalyst was studied using on-line gas-chromatography combined with mass spectrometry(GC-MS) and transient response technique.The reaction intermediates,butene and furan,were found in the reaction effuent under near industrial feed condition (3% butane 15% O2),while dihydrofuran was detected at high butane concentration (12% butane,5%O2).Some intermediates of MA decomposition were also identified.Detection of these intermediates shows that the vanadium phosphorus oxides are able to dehydrogenate butane to butene,and butene further to form MA.Based on these observations,a modified scheme of reaction network is proposed.The transient experiments show that butane in the gas phase may directly react with oxygen both on the surface and from the metal oxide lattice,without a proceeding adsorption step.Gas phase oxygen can be adsorbed and transformed to surface lattice oxygen but it can not participate in selective oxidation.Adsorbed oxygen leads to deep oxidation,while lattice oxygen leads to selective oxidation.