水热法从含钛电炉熔分渣中制备纳米片状结构二氧化钛光催化剂

采用水热法,以氢氧化钠为分离剂,从含钛电炉熔分渣中成功制备出纳米片状结构二氧化钛光催化剂,并探讨了水热反应时间、水热温度以及碱液浓度对分离提取纳米片状结构二氧化钛的影响．随着水热反应时间的延长,水热温度以及氢氧化钠溶液浓度的提高,从含钛电炉熔分渣中分离提取的二氧化钛结晶度越好,微观形貌更趋近于纳米片状结构．水热法处理含钛电炉熔分渣的最佳反应条件是：水热温度高于180℃,水热反应时间大于24h,碱液浓度达到12mol·L^-1．以制备得到的纳米片状结构二氧化钛为光催化剂,在氙灯光照90min后,甲基蓝降解率可达81．1％．     

由熔融高炉渣制备微晶玻璃

采用熔融法,由熔融高炉渣制备性能稳定的基础玻璃.通过对基础玻璃的差热分析确定微晶玻璃的热处理工艺制度.结合X射线衍射分析、扫描式电子显微镜观察等现代研究方法,确定了微晶玻璃热处理制度的最佳工艺参数,并研究了微晶玻璃的晶体生长方式.微晶玻璃的热处理最佳工艺参数为：核化温度850℃,保温1.5 h;晶化温度935℃,保温1 h.玻璃首先从表面开始析晶,然后逐步向内部生长.实验所得微晶玻璃的力学性能,如抗折强度、耐酸碱性和硬度,均优于天然大理石.     

Preparation and visible-light photocatalytic property of nanostructured Fe-doped TiO2 from titanium containing electric furnace molten slag

Nanostructured Fe-doped titanium dioxide was synthesized from titanium containing electric furnace molten slag (TCEFMS) by using an alkali fusion, followed by a hydrolyzation-acidolysis-calcination route. The effects of alkali/slag mass ratio, calcinating temperature, calcinating time, and water/slag mass ratio on the extraction efficiency and purity of products were systematically studied in this paper. It is indicated that the best extraction efficiency of nanostructured Fedoped titanium dioxide is 99.35%, when the molten slag is calcinated at 700°C for 1 h with the mass ratio of alkali/molten slag of 1.5:1. The influence of alkali/slag mass ratio on the photocatalytic activity of final products was evaluated by the photodegradation of methyl blue under visible light irradiation. A maximum photodegradation efficiency of 88.12% over 30 min was achieved under the optimum conditions.     

CaCl2熔盐电解钛精矿制备TiFe合金

在CaCl2熔盐中,以通Ar气保护条件下经过熔融后再凝固的钛精矿作为阴极,进行电解制备钛铁合金,探讨电解过程中TiFe合金的形成机制。在电解电压为3.1V,电解温度900℃时,研究了电解时间对电解产物的影响。研究结果表明,实验室条件下,可以通过熔盐电解钛精矿的方法制备成分均匀的TiFe合金。钛精矿在电解过程中经历了优先生成Fe,然后逐步形成TiFe的合金化历程,中间产物包括CaTiO3、TiO2、Ti2O3、TiO、Fe、TiFe2,Ti的还原是分多步完成的。     

Direct electrochemical reduction of titanium dioxide to titanium in molten calcium chloride

Many reactive metals are difficult to prepare in pure form without complicated and expensive procedures. Although titanium has many desirable properties (it is light, strong and corrosion-resistant), its use has been restricted because of its high processing cost. In the current pyrometallurgical process--the Kroll process--the titanium minerals rutile and ilmenite are carbochlorinated to remove oxygen, iron and other impurities, producing a TiCl4 vapour. This is then reduced to titanium metal by magnesium metal; the by-product MgCl2 is removed by vacuum distillation. The prediction that this process would be replaced by an electrochemical route has not been fulfilled; attempts involving the electro-deposition of titanium from ionic solutions have been hampered by difficulties in eliminating the redox cycling of multivalent titanium ions and in handling very reactive dendritic products. Here we report an electrochemical method for the direct reduction of solid TiO2, in which the oxygen is ionized, dissolved in a molten salt and discharged at the anode, leaving pure titanium at the cathode. The simplicity and rapidity of this process compared to conventional routes should result in reduced production costs and the approach should be applicable to a wide range of metal oxides.     

高纯二氧化钛的制备

利用ＳｉＣｌ４水解倾向大于ＴｉＣｌ４的原理,采用部分水解法可制得Ｓｉ质量分数约１０μｇ／ｇ的ＴｉＯ２。它可以艇用作制备高纯三氧化二钛的原料。     

溶胶-凝胶法制备纳米二氧化钛

主要介绍了通过溶胶-凝胶法制备纳米二氧化钛的方法,讨论了加水量、加酸量、加醇量及溶液pH等因素对溶胶-凝胶法的影响,通过反复试验分析,得出各影响因素的最佳值.对制出的TiO2进行表征,得出在本实验条件下制出的TiO2为锐钛矿型,粒径小于20nm.     

Pure metal extraction from molten oxide slag by short-circuit galvanic cell

The oxygen-ion-permeable membrane galvanic short-circuit method has been developed, in which pure metal was directly extracted from the molten oxide slag, and no external voltage is applied. The galvanic cell employed in the experiment was as follows: graphite rod|[O]_{Fe+C saturation}|ZrO₂(MgO)|(FeO)_(siag)|Fe rod. The reduction current in the galvanic cell consisted of an external short-circuit current and an interior short-circuit current in the oxygen-ion-permeable membrane. The real-time variation of external circuit reduction ratio of the molten slag could be obtained from the curve of the external circuit current to the time.     

Preparation of CaO-Al2O3-SiO2 system glass from molten blast furnace slag

To use the potential heat of molten blast furnace slag completely, a CaO-Al₂O₃-SiO₂ system glass (MSG) was prepared from the molten industrial slag. The corresponding method proposed in this study utilized both slag and its potential heat, improving the production rate and avoiding the environmental pollution. Using appropriate techniques, an MSG with uniform color and superior performances was produced. Based on the experimental results and phase diagram, the chemical composition of MSG by mass is obtained as follows: CaO 27%–33%, SiO₂ 42%–51%, Al₂O₃ 11%–14%, MgO 6%–8%, and Na₂O+K₂O 1%–4%. Thermodynamic processes of MSG preparation were analyzed, and the phases and microstructures of MSG were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results show that alkali metal oxides serve as the fluxes, calcium oxide serves as the stabilizer, and alumina reinforces the Si-O network. XRD and SEM analyses show that, the prepared MSG displays the glass-feature patterns, the melting process is more complete, and the melt viscosity is lowered with an increase in calcium oxide content; however, a continuous increase in slag content induces the crystallization of glass, leading to the formation of glass subphase. The optimum content of molten slag in MSG is 67.37wt%. With respect to bending strength and acid/alkali resistance, the performance of MSG is better than that of ordinary marble.     

低温燃烧法合成纳米二氧化钛粉体研究

采用一种简便、快速、低温的溶胶凝胶自蔓延燃烧法制备了纳米TiO2粉体颗粒.从柠檬酸络合反应的机理阐释了纳米TiO2粒子的形成过程.通过热综合分析、X射线衍射和透射电镜分析探讨了金属离子与柠檬酸的摩尔比和溶液杂质离子的存在对TiO2粉体颗粒物相组成及粉末晶粒尺寸大小的影响.本实验制备了粒径为40～90 nm分散性较好的球形状TiO2纳米颗粒.X射线衍射结果表明,当摩尔比为0.5时,自燃合成产物中金红石相的质量分数达到91%.     

工业TiOSO4液直接沉淀法制备二氧化钛/膨胀石墨吸附-光催化材料

以工业钛液为钛源,通过插层、包覆引入到可膨胀石墨上,经高温膨胀制备得到高膨胀体积二氧化钛/膨胀石墨复合材料. 分别用扫描电镜、红外光谱仪、X射线衍射仪和电子能谱对复合材料进行表征. 结果发现：工业钛液直接沉淀制备的复合材料中二氧化钛能较好固着于膨胀石墨表面,随钛液加入量增加,二氧化钛/膨胀石墨复合材料的含钛增加但膨胀体积减小. 复合材料中二氧化钛为锐钛型与金红石型的混和型态. 红外光谱分析表明复合材料保持了类拟膨胀石墨的性能. 复合材料的脱色效率优于纯膨胀石墨.     

钛白废盐制备高纯MnO_2纳米棒

以钛白生产中产生的废盐为原料,采用水热法合成制备了高纯MnO2纳米棒,研究了不同反应条件对产品纯度和产率的影响.以纯度和产率为指针,确定了制备高纯MnO2纳米棒的最佳工艺条件,并对样品进行了XRD、FT-IR、SEM、ICP表征.研究结果表明,MnO2纳米棒的纯度随水热反应pH增大而增大,当pH为2.0时,制得的MnO2纳米棒纯度最大,继续增大pH,样品纯度下降,MnO2纳米棒的产率随水热反应pH增大而增大,当pH为4.0时,产率最大,继续增大pH,产率下降;当NaCl的加入量为0.08 g时,纯度和产率同时达到最大;MnO2纳米棒纯度几乎不随NaClO3加入量的变化而变化,而产率随着NaClO3加入量的增加而增加.     

纳米TiO2膜的制备及表征

通过溶胶-凝胶工艺制备了表面均匀的纳米TiO2光催化薄膜．用UV—Vis、AFM、XRD和XPS等对薄膜的表面形貌、结构和组成等进行了表征．结果表明，TiO2膜的表面均匀，颗粒大小约50nm，晶型为锐钛矿型．     

溶胶-凝胶法制备纳米TiO2研究

采用溶胶-凝胶法制备纳米TiO2，讨论了反应过程中各影响因素对纳米TiO2粒度的影响，并设计正交实验优化出制备纳米TiO2实验条件，用透射电镜对制得的纳米TiO2粉末进行了表征．     

高炉渣酸溶物基水热合成光催化剂的研究

以冶金高炉渣酸溶物为原料,采用水热法合成制备光催化剂,利用傅里叶变换红外光谱(FTIR)和扫描电镜(SEM)对光催化剂的化学组分、比表面积等物性进行表征,并研究了水热反应过程中pH值、反应温度和反应时间对高炉渣酸溶物制光催化剂催化活性的影响。结果表明,所制光催化剂是一种比表面积较大的多孔材料,且具有良好的光催化活性;光催化氧化浓度为2 5 mg/L的甲基橙溶液陈化0.5 h后,其脱色率达到98.9%。     

TiO2纳米粒子制备及其光催化性能研究

以无机盐四氯化钛为原料,采用加碱中和水解法制备出纳米级二氧化钛粒子.采用正交实验方法研究了温度、浓度、反应终了pH值、分散剂用量以及反应时间对粒子大小、分散性能和光催化性能的影响,并得到了二氧化钛光催化剂的最佳制备工艺条件,同时研究了不同条件制得的二氧化钛光催化剂对苯酚水溶液的催化降解特性.实验发现除锐钛型TiO2具有光催化活性外,无定型水合TiO2粒子也具有良好的催化活性.     

Preparation of calcium carbonate particles coated with titanium dioxide

The preparation of a new mineral composite material, calcium carbonate particles coated with titanium dioxide, was studied. The mechanism of the preparation process was proposed. The new mineral composite material was made by the mechanoehemieal method under the optimum condition that the mass ratio of calcium carbonate particles to titanium dioxide was 6.5:3.5. The mass ratios of two different types of titanium dioxide (anatase to rutile) and grinding media to grinded materials were 8:2 and 4:1 respectively, and the modified density was 60%. Under this condition, the new material was capable of forming after 120-min modification. The hiding power and oil absorption of this new material were 29.12 g/m2 and 23.30%, respectively. The results show that the modification is based on surface hydroxylation. After coating with titanium dioxide, the hiding power of calcium carbonate can be improved greatly. The new mineral composite materials can be used as the substitute for titanium dioxide.     

富硼渣盐酸法制取硼酸和氢氧化镁

采用富硼渣盐酸法来处理富硼渣,通过单因素试验和正交试验确定富硼渣盐酸浸出的最佳试验条件.针对盐酸浸出液,开发了制备硼酸联产氢氧化镁和硫酸钙工艺.研究结果表明:浸出温度为95℃,盐酸用量为理论用量的95％,浸出时间为40 min,浸出液固比为1:1时,B浸出率为94.60％,Mg浸出率达到90.56％.制得的硼酸纯度为99.55％,氢氧化镁的纯度达到80％以上,副产品硫酸钙纯度达到98.81％.     

高炉渣稳定熔融态转炉渣中游离CaO的实验研究

通过配加高炉渣,改变R(R=w(CaO)/w(SiO_2))来对转炉渣进行稳钙改质处理。结果表明:高炉渣可以有效稳定转炉渣中f-CaO,当R=1.5,1 500℃下恒温30 min时,f-CaO的消解率达到80.22%;经过XRD分析和FESEM显微观察可知,熔混渣主要矿相为钙铝黄长石、镁黄长石和镁铁尖晶石,f-CaO含量降低与钙铝黄长石、镁黄长石的增加呈正相关。     

黄磷渣提磷联产二氧化硅工艺分析

探索黄磷渣提磷联产二氧化硅的最优工艺,减少磷渣中磷对环境的污染,实现磷渣废渣资源化综合利用。以不同粒径研磨混匀的黄磷渣为原料,分析了磷提取率及联产高含量二氧化硅的影响因素,并采用SEM、FTIR对精制二氧化硅表征定性。结果表明:4~6h阶段,磷提取率维持在20%~22.86%,5h时,磷提取效果最佳为22.86%;对最佳液固比和反应时间制备的二氧化硅进行精制,其纯度提高为94.25%。