溶胶-凝胶法制备堇青石陶瓷粉体的研究

以结晶氯化铝(AlCl3·6H2O)、结晶氯化镁(MgCl2· 6H2O)和正硅酸乙酯(TEOS)为原料,用溶胶-凝胶法制备堇青石粉体,采用XRD、SEM等测试手段对堇青石粉体进行了表征,探讨了溶胶-凝胶法制备堇青石粉体在低温下的烧结机理与析晶机制.结果表明:α-堇青石的开始形成温度为1150℃,在1200℃时晶化完全...     

SiO_2/海泡石复合材料表征及其对天然橡胶的增强

海泡石是一种天然的纤维状含水镁硅酸盐黏土矿物,具有孔道结构和优良的吸附性能。以正硅酸乙酯为硅源,采用溶胶-凝胶法制备SiO_2/海泡石复合材料,通过XRD、FTIR、TG和SEM/EDS等测试手段对复合材料的结构和形貌进行表征。结果表明,利用溶胶-凝胶法可以成功将SiO_2固载于酸改性海泡石上,且不会改变海泡石的结构。酸改性海泡石和SiO_2/海泡石对天然橡胶均有补强作用,相比天然橡胶,SiO_2/海泡石加入可以将橡胶拉伸强度提高50.19%,表明SiO_2和海泡石纤维具有良好的协同增效效果。     

玻璃膜基材料的制备及电致变色机理研究

采用溶胶-凝胶技术,以[CH3(CH2)3O]4Ti、La2O3、CoCl2·6H2O为前驱体,在ITO（氧化铟锡）玻璃基板上成功制备了Ti、Ti/La、Ti/Co不同摩尔配比的复合膜,确定了电致变色玻璃膜基材料制备的最佳工艺参数。采用XRD、热重-差热分析（TG-DTA）及电化学检测其膜基材料的循环伏安特性,并分析其电致变色特征机理。研究表明：(1) TiO2薄膜试样的烧成温度、镀膜层数、[CH3(CH2)3O]4Ti掺量、掺杂类别是影响膜基材料结构和性能的主要因素;(2)使用二乙醇胺作为螯合剂能够有效抑制Ti (OH)4沉淀的生成;(3)掺杂La2O3和CoCl2·6H2O制备的TiO2玻璃膜基溶胶电致变色性能优良;(4)制备的TiO2变色膜基材料透过率好,循环可逆性高,循环伏安特性明显。研究结果为电致变色膜基材料的开发和应用提供了理论和基础实验依据。     

三水碳酸镁法制备碱式碳酸镁过程研究

以菱镁矿为原料,先合成MgCO_3·3H_2O晶须,并以此为前驱体,制备了高纯414型碱式碳酸镁,主要研究机械搅拌作用对结晶过程的影响。利用X射线衍射(XRD)和扫描电镜(SEM)分析了碱式碳酸镁物相组成及微观形貌。结果表明,搅拌有助于加快相转变进程,热解温度70℃,搅拌作用下,60 min时,MgCO_3·3H_2O全部转变为形貌均匀的多孔棒状4MgCO_3·Mg(OH)_2·4H_2O;而无搅拌作用下,90 min时MgCO_3·3H_2O全部转变为多孔玫瑰花状4MgCO_3·Mg(OH)_2·4H_2O微球。4MgCO_3·Mg(OH)_2·4H_2O晶体中,Mg~(2+)呈现两种不同的正八面体配位,MgO_6正八面体通过共顶点和共棱的方式连接而成,分别沿[100]和[001]方向快速生长,最终形成球状或棒状形貌。     

硅藻土原位制备纳米结构MgFe_2O_4及Cr(Ⅵ)吸附性能研究

以MgCl_2·6H_2O为镁源,Fe C_2O_4为铁源,NH_3·H_2O为沉淀剂,十六烷基三甲基溴化铵(CTAB)为模板剂,通过低温水热法,在硅藻土藻盘表面原位制备花片状纳米结构Mg Fe_2O_4;采用XRD、SEM、TEM、BET、XPS、ZPC等对样品进行了表征。所制备纳米结构Mg Fe_2O_4呈多晶态,比表面积为335 m~2/g。研究了Mg Fe_2O_4/硅藻土样品对Cr(Ⅵ)吸附与价态转化行为,其中样品在无光(黑暗)下对Cr(Ⅵ)的饱和吸附容量为543 mg/g,在可见光及紫外光等光照下,对Cr(Ⅵ)的饱和吸附量分别为556 mg/g、570 mg/g。样品具有一定的光响应能力。     

凝胶-溶胶法制备单分散菱柱形草酸镍的研究

以Ni(OH)2凝胶为前驱体.采用凝胶-溶胶法制备了单分散菱柱形二水草酸镍.采用SEM,XRD 等方法及Imagetool图像分析软件,对所制备的NiC2O4·2H2O粉末形貌及形成机理等进行了研究,结果表明,控制适当条件,可使NiC2O4·2H2O颗粒在低过饱和度下均匀生长,其形成机理为溶解-再结晶;随温度升高,粉末...     

V~(5+)掺杂TiO_2凝胶的相变过程研究

采用溶胶-凝胶法制备了V5+掺杂Ti O2纳米粉体,利用TG-DTA和XRD对凝胶的相变过程进行表征。考察了不同煅烧温度对V5+掺杂Ti O2纳米粉体的晶体结构、晶粒尺寸和金红石相对含量的影响。结果表明:Ti O2-V2O5复合凝胶在煅烧温度为400℃左右时由非晶态向锐钛矿相转变,600℃左右时开始由锐钛矿向金红石相转变;掺杂0.5%的V5+抑制了锐钛矿向金红石转变。     

结晶法制备锆酸锂及其吸收CO_2试验研究

以LiOH·H_2O和Zr(NO_3)_4·5H_2O为主要原料,在两者摩尔比为2.0条件下通过结晶法制备高纯Li_2ZrO_3。当煅烧温度T为1123 K时,Li_2ZrO_3主要以单斜相存在。在模拟CO2吸收反应中可知,当反应时间为42 min,温度为517℃,压强为2.0 MPa时,Li_2ZrO_3吸收CO2量达到峰值,Li_2ZrO_3质量增重为9.2%。     

硅酸钠溶液水热法深度脱铝研究

以Na_2SiO_3·9H_2O、NaAlO_2和CaCl_2为原料,采用水热法将溶液中的铝转化成水化石榴石沉淀进行脱铝。通过对水热温度160℃、时间1～16h条件下得到的粉体进行X射线衍射和扫描电镜分析,得到硅酸钠溶液深度脱铝的最佳条件。结果表明,水热1h,反应体系中Ca_5Si_6O_(16)(OH)_2、Ca_5Si_6O_(16)(OH)_2·8H_2O和低铝水化石榴石Ca_5Si_5Al(OH)O_(17)·5H_2O絮状混合沉淀大量生成;当水热时间为10～12h时,体系中同时存在高铝水化石榴石Ca_(2.93)Al_(1.97)Si_(0.64)O_(2.56)(OH)_(9.44)与低铝水化石榴石Ca_5Si_5Al(OH)O_17·5H_2O物相,铝脱除率可达98.05%,可实现反应体系的深度脱铝。     

通化地区煤系高岭岩制备纳米级α-Al2O3

以煤系高岭岩提取氯化铝的工艺流程及溶胶－凝胶技术制备出纳米级α-Al2O3，确立了溶胶－凝胶制备纳米级α-Al2O3的最佳试剂条件和煅烧条件。生成的Al(OH)3溶胶经干燥、煅烧后得到纳米级氧化铝粉末，为α相，粒度为100nm左右。     

Surface properties of enargite in MAA depressant solutions

Enargite (Cu₃AsS₄) is a common penalty mineral in the copper mining industry. Different treatment methods have been proposed to passivate the enargite surface for effective flotation of non-arsenic copper minerals, including pulp potential control, pre-oxidation and chemical depression. Magnesium ammonium mixture (MAA) has been previously tested, showing good selectivity for arsenic rejection. It was hypothesised that MAA would make the enargite surface hydrophilic by adsorption of magnesium ammonium arsenate hexahydrate (MgNH₄AsO₄·6H₂O). Here we show that MAA does not selectively adsorb onto the enargite surface as conjectured. X-ray photoelectron spectroscopy and cyclic voltammetry show that magnesium compounds do not precipitate onto the enargite surface at pH 10, whereas magnesium hydroxide on the enargite surface is formed at pH 12. MgNH₄AsO₄·6H₂O was not observed at either pH 10 or pH 12. The effect of pre-oxidation to promote dissolution of (AsO₄)³⁻ before conditioning with MAA, which could help catalyse the formation of MgNH₄AsO₄·6H₂O, was also tested. However, the results were the same as those without pre-oxidising the sample. Our investigation shows that under alkaline conditions it is not possible to passivate the enargite surface in MAA solutions for effective flotation of non-arsenic copper minerals.     

Visible light induced TiO2 pillared MMT photocatalyst coupling-doped with S and N

Visible light induced titanium dioxide (TiO₂) pillared montmorillonite clay (MMT) photocatalyst coupling-doped with S and N elements was prepared by the two-step adsorption method. The photocatalyst was characterized by X-ray photoelectron spectroscopy (XPS) and ultraviolet-visible (UV-vis) absorption spectroscopy. The photocatalysic efficacy of the prepared photocatalyst for degrading gaseous formaldehyde was evaluated under visible light irradiation. The degrading rate of gaseous formaldehyde is nearly 85% in 300 min visible light irradiation. The results demonstrate that the much higher visible light photocatalytic activity of the photocatalyst is due to the synergistic effects of coupling-doping of S and N elements to TiO₂, extensive specific surface area of MMT and quantum sized efficacy between layers of MMT. Supported by the Scientific Research Foundation for the Returned Overseas Chinese Scholars, State Education Ministry, China (LX-2006-3311)     

Effect of cyanobacteria Synechococcus PCC 7942 on carbonation kinetics of olivine at 20 °C

By accelerating the naturally-occurring carbonation of magnesian silicates, it would be possible to sequester some of the anthropogenic excess of CO₂ in more geologically-stable solid magnesium carbonates. Reaction rates can be accelerated by decreasing the particle size, raising the reaction temperature, increasing the pressure, using a catalyst, and hypothetically, by bacterial addition. We aimed here at assessing quantitatively the added value of photosynthetic microbial activity on the efficiency of Mg-silicates carbonation processes. Synechococcus PCC 7942 (freshwater cyanobacteria) was selected for this study. Two magnesian silicate minerals (substrates) were chosen: a synthetic forsterite with nanometer-sized grains and an industrial ultramafic slag (scoria). All tests were performed at 20 ± 1 °C in closed and sterile 1L Schott® glass bottle reactors. With the aim to elucidate the interaction between mineral phases and bacteria, we used pH and concentration measurements, scanning and transmission electron microscopy along with Raman spectroscopy. The results show that, at ambient temperature, cyanobacteria Synechococcus can accelerate silicate dissolution (i.e. Mg²⁺ release) and then magnesium carbonate nucleation and precipitation by adsorption on the produced exopolymeric substances and local pH increase during photosynthesis, respectively.     

The interaction of sodium mercaptobenzothiazole with gold electrode and nanorod surfaces

Attenuated total reflectance Fourier transform infrared spectroscopy, Raman spectroscopy, X-ray photoelectron spectroscopy and transmission electron microscopy have been applied to characterise and investigate the interaction of sodium mercaptobenzothiazole (MBT) with gold surfaces and gold nanorods. Gold nanorods (Au NRs) with average aspect ratio of 4.04 ± 0.08 were synthesised and reacted with MBT. Gold(I) mercaptobenzothiazole and the dithiolate, 2,2′-dithiobisbenzothiazole ((MBT)₂) were synthesised and characterised to provide a basis for compound identification. It was concluded that MBT could link two Au NRs by adsorption through the exocyclic S atom on one NR and the endocyclic S atom on the other NR, thereby leading to the formation of Au nanochains in the suspension. The MBT flotation of 100 μm gold particles was also investigated utilising controlled potential techniques. The gold metal particles floated in the cell when the potential reached 0.5 V. At that potential, (MBT)₂ was observed on the gold particles, and their floatability was attributed to the adsorption of that dithiolate species.     

Preparation of magnesium hydroxide from serpentinite by sulfuric acid leaching for CO2 mineral carbonation

Carbon capture and storage (CCS) by mineral carbonation is a promising way for CO₂ emissions mitigation that has been under studied for decades. In this work, the preparation of magnesium hydroxide from Finnish serpentinite using sulfuric acid leaching as the first step of a CO₂ mineral carbonation process was studied. Some details of leaching behavior of the ore were revealed and a valuable metal was recovered in this study. It was found that leaching yield of magnesium increased with sulfuric acid dosage, limited by a product layer formed on the ore particles, resulting in incomplete serpentinite decomposition. Agitation and ultrasonication were demonstrated to be effective in controlling the thickness of product layer. About 95% of iron was recovered from the leachate and leaching residues and valuable Fe-rich substances were obtained as by-products. After the iron extraction, a fine Mg(OH)₂-rich powder could be prepared from the Mg-rich solution by precipitation using sodium hydroxide solution.     

Using Calcium Carbonate/Hydroxide and Barium Carbonate to Remove Sulphate from Mine Water

This study evaluated the effectiveness of using barium bicarbonate to remove sulphate from neutralized AMD. The Ba(HCO₃)₂ was produced by dosing a BaCO₃ solution with CO₂ to form Ba(HCO₃)₂. This greatly increased the barium ion concentration, which rapidly removed sulphate linked to either calcium or magnesium. Following sulphate removal, the Ca(HCO₃)₂ or Mg(HCO₃)₂ containing water can be stabilised by CO₂ stripping with air, which results in CaCO₃ precipitation. The MgCO₃ remains in solution.     

Gemini trisiloxane surfactant: Synthesis and flotation of aluminosilicate minerals

In this paper, an amino-trisiloxane Gemini cationic surfactant, butane-1,4-bis(dimethyl-(3-(3-aminopropyl trisiloxane-3-yl)-propyl)-ammonium bromide) (BBAB) was prepared, and its flotation potential was assessed on kaolinite, pyrophyllite and illite minerals. The flotation results showed that changes to the pulp pH did not significantly influence BBAB’s collecting power in floating three aluminosilicate minerals. In addition, BBAB was a stronger collector than the conventional monomeric surfactant dedecyl trimethylammonium bromide (DTAB) or dodecylamine (DDA). The results of FTIR spectra, zeta potential measurements and density functional theory (DFT) calculations indicated that the interaction of BBAB with the three aluminosilicates was mainly through electrostatic attraction. BBAB’s unique properties, such as high positive grouping Mulliken charge of –CH₂N⁺(CH₃)₂(CH₂)₄(CH₃)₂N⁺CH₂–, and “parachute” shape structure of [(CH₃)₃SiO]₂SiCH₃, resulted in superior collecting powers for the aluminosilicate minerals.     

Mn掺杂和还原氧化石墨烯复合对NiAl-LDHs超级电容性能影响

采用水热法制备了水滑石（layered double hydroxides,LDHs) NiAl-LDHs、NiMnAl-LDHs及其分别与还原氧化石墨烯(reduced graphene oxide,rGO)的复合材料。利用X射线衍射仪、扫描电子显微镜、能谱仪、X射线光电子能谱、拉曼光谱、电化学工作站对合成的材料进行了结构形貌和电化学性能表征,并研究了Mn离子掺杂和rGO复合对超级电容性能的影响。研究发现：Mn离子掺杂降低了LDHs的结晶度和片层尺寸,提高了分散性,降低了内阻,使倍率性能提高;与rGO复合后,导电性和比容量进一步提高,其中,NiAl-LDHs/rGO具有最高比电容,在1A/g时达1345F/g,在5A/g循环1000次后容量保持率为82.9%。     

The effects of LiOH and NaOH on the carbonation of SrSO4 by dry high-energy milling

In this work, the effects of alkaline hydroxides (NaOH and LiOH) on the direct mechanochemical carbonation using dry high-energy milling of celestine (SrSO₄) under CO₂ atmosphere was investigated with X-ray diffraction (XRD), infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and carbon analyses. It was observed that SrSO₄ was not directly carbonated by dry high-energy milling under CO₂ atmosphere without LiOH or NaOH additives. Direct mechanochemical SrCO₃ formation was observed during milling of the SrSO₄ and NaOH mixture under CO₂ atmosphere, and it was shown that a minimum 50% of the initial SrSO₄ was mechanochemically carbonated in the presence of NaOH and CO₂ gas. LiOH does not stimulate the direct carbonation. However, it was observed that washing of the milled mixture with water resulted in strontium carbonate (SrCO₃) formation because of the enhanced dissolution of Li₂CO₃ and SrSO₄, promoted by the activation effect of high-energy milling. Depending on the alkaline hydroxide used during the milling, strontium carbonates with different space group settings were formed, which have different (split or single) main carbonate absorption bands.     

水热法制备超细氢氧化镁

以水镁石为原料,通过煅烧,制得氧化镁粉末,然后将氧化镁和尿素碱溶液反应,通过氧化镁水合法制备出了超细氢氧化镁颗粒,同过利用X-射线衍射仪(XRD)和扫描电子显微镜(SEM)对所制得氢氧化镁颗粒的晶相、形貌和颗粒尺寸进行了表征。试验结果表明,溶液浓度和添加剂对氢氧化镁晶体的晶相和颗粒尺寸有显著的影响,当溶液浓度为2.5 mol/L,添加剂为PEG 6000的情况下,制备出了半径为250 nm,片厚约150 nm,晶形完整,大小均一的六方片形超细氢氧化镁颗粒,但是样品的纯度有待于进一步的提高。