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METALLURGICAL AND MATERIALS TRANSACTIONS B-PROCESS METALLURGY AND MATERIALS PROCESSING SCIENCE · 2024 ·Vol. 55 ·期 2 ·772-781 · IF 2.4

Experimental Analysis of High Purity Tellurium Prepared by Zone Refining

Tian Qinghua,He Zhiqiang,Xu Zhipeng,Li Dong,Guo Xueyi

High-purity tellurium is a supporting material for contemporary high-tech industries. Zone refining is commonly used as a reliable final purification step to achieve higher purity levels of tellurium. However, the removal of Selenium (Se)—the most troublesome impurity in tellurium often occurring in quite high amounts—stays as the challenge during zone refining, due to its very unfavorable distribution coefficient. In addition, there is an important factor, essential to predict the zone refining efficiency (required number of passes), which is still seldom explored. Therefore, in the present work, the effect of different number of passes on the purification effect of tellurium was investigated by using 4N tellurium as raw material. Firstly, the possibility of removing vaporized Se through introducing an reductive gas flux was studied by testing initial concentrations of Se (13 ppm) and undergoing different process parameters. The experimental results showed that when the number of passes was 3, the impurity removal rate was low and the purification effect was poor; when the number of zone refining reached 9, the removal rate of most impurities in tellurium reached 100 pct, the removal rate of impurity Se reached 80.15 pct, and the total removal rate reached 89.49 pct, and the purity of tellurium ingot was 5N7.

研究领域: 材料科学 · 冶金学 · 半导体技术
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Silicon · 2020 ·Vol. 13 ·期 2 ·531-541 · IF 1.499

Purification Mechanism of Quartz Sand by Combination of Microwave Heating and Ultrasound Assisted Acid Leaching Treatment

Li Feifei,Jiang Xuesong,Zuo Qiuxia,Li Jingwei,Ban Boyuan,Chen Jian

Iron is a major impurity in quartz sand and must be strictly removed in many applications. However, the iron removal rate in most of the conventional purification process is not high enough. In this study, a fast, low-energy consuming, environment-friendly and simple process for purifying quartz is demonstrated by a combination of microwave heating and ultrasound-assisted acid leaching treatment. Using the characteristics of selective heating of microwave, the micro-inclusions burst and generate cracks in the surrounding quartz matrix far below the α/β phase transition temperature, which enables removal of the impurities in the subsequent processing steps and reduces iron diffusion into the quartz matrix. Microwave process sequence, time, and temperature are all important factors, and appropriate parameters need to be explored. Ultrasound can assist acid leaching removal of Fe impurities through the cracks. Under optimized conditions, the iron content can be reduced to below 0.167 ppmw with one single purification pass.

CAS / MDL: 7697-37-2
研究领域: 材料科学 · 环境工程
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Analytical Methods · 2021 ·Vol. 14 ·期 4 ·401-409 · IF 2.896

Preparation of poly(ionic liquid@MOF) composite monolithic column and its application in the online enrichment and purification of tectochrysin in medicinal plants

Yamei Han,Shan Wang,Yijie Liu,Ligai Bai,Hongyuan Yan,Haiyan Liu

Herein, a poly(ionic liquid@MOF) composite monolithic column was prepared via in situ radical polymerization using ionic liquid (1-allyl-3-methylimidazolium hexafluorophosphate) and MOF (derivatized UIO66-2COOH) as copolymer monomers. The composite monolithic column was characterized via scanning electron microscopy (SEM), nitrogen adsorption–desorption isotherms and mercury intrusion porosimetry. Subsequently, the composite monolithic column combined with high performance liquid chromatography (HPLC) was used as a solid-phase extraction (SPE) absorbent for online purification and enrichment of tectochrysin in medicinal plants. The results indicated that the addition of the ionic liquid and MOF not only increased the surface area but also increased the adsorption capacity of the monolith for tectochrysin. The method showed good linearity in the concentration range of 0.01–500 μg mL−1. The calibration equation was y = 2154.6x − 8.3785 and the limit of detection (LOD, S/N = 3) and the limit of quantification (LOQ, S/N = 10) were 3.33 ng mL−1 and 10 ng mL−1, respectively. The relative standard deviation (RSD) of the intra-day and inter-day precision was less than 2.62%, the RSD of inter-column was less than 3.16%, and the recoveries ranged from 100.58% to 105.00%. Thus, results showed that this method is simple, accurate and convenient for the online enrichment and purification of tectochrysin from medicinal plants.

研究领域: 分析化学 · 药物分析 · 材料科学
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CHEMICAL PAPERS · 2018 ·Vol. 72 ·期 12 ·2997-3003 · IF 0.963

Application of Taguchi method for optimization of process parameters in preparation of high-purity molybdenum disulfide

Guo Dongqing,Fu Likang,Wang Shixing,Zhang Libo,Peng Jinhui

A new purification method for molybdenum disulfide via NaNO 3 –HCl–HNO 3 synergistic leaching at 80 °C was developed. The effects of the concentration of NaNO 3 , HCl, and HNO 3 , and liquid–solid ratio and the leaching time on the purification of molybdenum disulfide were investigated by orthogonal array design methodology. The results of Taguchi method utilizing L 25 (5 5 ) orthogonal array indicated that the NaNO 3 concentration had the greatest impact on the purification of molybdenum disulfide. The optimum conditions for the purification of molybdenum disulfide were as follow: concentration of NaNO 3  = 2.5%, concentration of HCl = 11%, concentration of HNO 3  = 1.0%, liquid–solid ratio = 3, and the leaching time = 10 h. Under optimum conditions, the content of molybdenum increased from 55.1 to 59%, and the contents of iron, copper, lead, and calcium decreased from 0.35 to 0.21%, 0.027 to 0.008%, 0.054 to < 0.005%, and 0.27 to 0.035%, respectively. Based on molecular formula of molybdenum disulfide, the content of molybdenum disulfide increased from 91.93 to 98.44%. XRD and SEM indicated that this method removed only the impurities and did not affect the phase and particle size of molybdenum disulfide. The results show that the new purification method avoids the roasting process and will achieve the “green” production. The new method based on orthogonal array is effective for the purification of molybdenum disulfide via acid leaching.

CAS / MDL: 7697-37-2 7647-01-0
研究领域: 材料科学 · 化学工程
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JOURNAL OF MOLECULAR LIQUIDS · 2018 · IF 4.513

Enhancing the purity of magnesite ore powder using an ethanolamine-based collector: Insights from experiment and theory

Wenbao Liu,Wengang Liu,Shujuan Dai,Ting Yang,Zhen Li,Ping Fang

Magnesite ore powder is the primary raw material used to prepare refractory magnesia. With the depletion of high-grade magnesite, methods to reduce the impurities and improve the quality of magnesite ore powder are urgently required. In this study, an ethanolamine-based surfactant, bis (2-hydroxyethyl) dodecylamine (BHDA), was first introduced into the flotation of magnesite ore as a novel collector, and the possibility of improving the purity of the ore was investigated by experiment and theory. Flotation tests, X-ray photoelectron spectroscopy, Fourier-transform-IR spectroscopy, and zeta potential measurements were carried out to study the behaviors and mechanisms by which the collector enhances the purity of magnesite ore powder. The flotation results revealed the noticeable difference in the floatability of quartz, magnesite, and dolomite when combined with the collector over a wide range of pulp pH values (4.18–9.17). The analytical results obtained from FTIR spectra, XPS, and zeta potential measurements indicate that BHDA was readily adsorbed on the surface of quartz, mainly by electrostatic and hydrogen bonding interactions, whereas it was adsorbed on the surfaces of magnesite and dolomite by weak electrostatic interactions. By introducing a hydroxyethyl group to the tertiary amine collector, more hydrogen bonds can form with the surface of quartz, strengthening the adsorption stability. Thus, compared to the traditional collector, dodecylamine, BHDA showed better desilication and purification performance for magnesite ore powder. Meanwhile, our results show that the simpler reagent system and process flow makes BHDA promising for the industrial purification of magnesite ore powder.

研究领域: 矿物加工工程 · 材料科学与工程 · 化学工程与技术
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Energy & Environmental Materials · 2022 ·Vol. 6 ·期 6 ·e12425 · IF 13.443

High Ion-Selectivity of Garnet Solid Electrolyte Enabling Separation of Metallic Lithium

Haitian Zhang,Jialiang Lang,Kai Liu,Yang Jin,Kuangyu Wang,Yulong Wu,Siqi Shi,Li Wang,Hong Xu,Xiangming He,Hui Wu

Ionic selectivity is of significant importance in both fundamental science and practical applications. For instance, an ion-selective material allows the passage of a particular kind of ions while blocking the others, which could be used for purification of materials. Herein, the Li-ion-selectivity of a garnet-type solid electrolyte is discussed by comparing the difference of activation energy between different ions migrating in solids. The high ion-selectivity is confirmed by harvesting high-purity metallic lithium (99.98 wt%) from low-lithium-purity sources (80 wt%) at a moderate temperature (190 °C). This gives it huge potential in separating lithium with impurities especially alkali and alkali-earth elements. The cost of metallic lithium production is only 25% of the international lithium price. The proposed electrochemical metallic lithium separating method is advantageous compared with the traditional process in terms of efficiency, safety, and cost.

研究领域: 材料科学 · 能源技术
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SEPARATION AND PURIFICATION TECHNOLOGY · 2025 · IF 9

Confinement-gradient crosslinking strategy for dynamic-gated iCOF@PEI ultrathin composite membranes toward precision H2/CO2 separation

Ziheng Li,Shenghan Ji,Fengting Yao,Yan Dai,Xuehua Ruan,Xiaobin Jiang,Wenji Zheng,Gaohong He

Covalent organic frameworks (COFs) are regarded as disruptive membrane materials owing to their versatile functionalities, high stability and ordered nanochannels. However, a major obstacle to the application of COF-based membranes in gas separation is the inherent size difference between their pore sizes and target gas molecules. Herein, we employed a confined cross-linking strategy to graft CO 2 -philic poly-ethyleneimine (PEI) onto carboxylic acid-type iCOF membranes, constructing a gradient wedge-shaped pore wall structure to enhance H 2 separation. High-density carboxyl group-containing iCOF nanosheets were prepared via an improved single-phase solution method and assembled into membranes. 1-ethyl-3-(3-dimethylami-nopropyl) carbodiimide/N-Hydroxysuccinimide (EDC/NHS) coupling chemistry was used to functionalize iCOF membranes with PEI. The introduction of a large number of amino groups via PEI enhances CO 2 adsorption by 81.4%. Meanwhile, the grafting of PEI reduces defects or pinholes on the membrane surface and improves the mechanical properties and stability. As a result, the PEI-functionalized iCOF@PEI-4 membrane exhibits a H 2 permeance of 1103 GPU and an H 2 /CO 2 selectivity of 21.3, positioning its performance among advanced membranes and surpassing the 2008 Robeson upper bound. Customized structural design of iCOF membranes through tailored functionalization may provide insights for designing molecularly selective COF membranes.

研究领域: 材料科学 · 膜分离技术 · 纳米材料 · 化学工程 · 功能高分子
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MINERALS ENGINEERING · 2025 · IF 5

Comprehensive XRD study of enhancing Al removal rate by microstructure refinement and phase transformation in quartz powder purification process

Hao Fu,Xuesong Jiang,Xiaotian Chen,Zhenyi Hu,Jifei Sun,Zongrong Zhou,Ling Wang,Boyuan Ban,Jian Chen

Al is one of the most difficult to remove impurities from quartz. Even with HF, only a limited removal efficiency was demonstrated. This study proposes a novel and environmentally friendly strategy centered on a combined process of ball milling, Na 2 CO 3 roasting, fluorine-free acid leaching, and chlorination roasting. The core innovation lies in the strategic induction of a consecutive and reversible phase transformation cycle (α-quartz → cristobalite → α-quartz), which serves as an internal grain refiner to achieve continuous microstructure refinement, thereby constructing abundant fast pathways for impurity migration. A comprehensive XRD analysis was introduced to observe the microstructure evolution. The results indicate that Na 2 CO 3 promotes the phase transformation from α-quartz into cristobalite at a relatively low temperature, while chlorination roasting facilitates the reverse transformation back to α-quartz. It revealed that these two distinct phase transformations not only disrupt the crystal integrity but also lead to significant microstructure refinement accompanied by abundant lattice defects. Through these defects, Al impurities rapidly migrate to the quartz particle surface, where they react with the acid solution and HCl gas, enabling efficient removal. Under the optimal process, the Al removal rate reached 90.5 %, the total impurity removal rate attained 98 %, and the quartz purity increased from 99.683 wt% to 99.994 wt%. This work highlights the crucial role of reversible phase transformation-induced grain refinement as an efficient strategy for lattice impurity removal, offering a green and high-performance alternative to HF-based purification with demonstrated advantages in environmental safety, energy efficiency, and product yield.

CAS / MDL: 7758-02-3
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Arabian Journal of Chemistry · 2021 · IF 5.165

One-step fabrication of hydrophilic lignosulfonate-decorated reduced graphene oxide to enhance the pervaporation performance of calcium alginate membranes

Saisai Li,Yaru Wu,Xia Zhan,Jiding Li,Jiandu Lei,Jing He,Luying Wang

In this study, a reduced graphene oxide (rGO)@sodium lignosulfonate (NaLS) composite material was fabtricated using a one-step method and then mixed with natural polysaccharide calcium alginate (CaAlg) to prepare the [email protected] /CaAlg pervaporation membrane. The appearance and physical properties of the [email protected] /CaAlg membrane were characterized by scanning electron microscopy and water contact angle. The swelling performance of the membrane and its dehydration performance to organic solvents were evaluated. The results indicate that the addition of [email protected] can increase the hydrophilicity of the [email protected] /CaAlg membrane and reduce its degree of swelling in the ethanol solution. The membrane incorporated with 6 wt% [email protected] exhibits the best pervaporation performance, and ethanol can be purified to 99.8%.

CAS / MDL: 10043-52-4 9005-38-3
研究领域: 材料科学 · 化学工程 · 膜技术
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MINERALS ENGINEERING · 2025 · IF 5

Study on synergistic purification of microcrystalline graphite by ammonium fluoride/EDTA: response surface methodology optimization and kinetic control

Yaqi Zhao,Xiuhua Chen,Zhengjie Chen,Wenhui Ma,Shilong Ye,Zirui Li,Xiaowei Chen,Yonghang Zhang

The efficient purification of microcrystalline graphite is the key to its high-value applications. Therefore, this study proposes a synergistic purification method involving ammonium fluoride roasting and ethylenediaminetetraacetic acid (EDTA) complex leaching. Using natural microcrystalline graphite (MG) as the raw material, the ammonium fluoride roasting process was optimized by response surface methodology (RSM), and the fixed carbon content of the roasted purified microcrystalline graphite (RMG) was obtained at 97.76 %. After subsequent EDTA complex leaching, the fixed carbon content in the final ERMG product reached 99.86 %. The MgF 2 component in the impurities was used as a representative model system for kinetic analysis, which indicated that the leaching process occurred in two stages. The first stage was controlled by the pore volume diffusion model, while the second stage was jointly controlled by interfacial transfer and product layer diffusion. Structural characterization confirmed that this process introduced nitrogen/fluorine co-dopants, which increased the interlayer spacing of graphite and formed macropores and mesopores. This method reduced the reliance on highly corrosive reagents, providing a promising alternative for the high-value utilization of microcrystalline graphite.

CAS / MDL: 1336-21-6 60-00-4
研究领域: 材料科学 · 无机化学 · 化学工程 · 矿物加工 · 碳材料
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SEPARATION AND PURIFICATION TECHNOLOGY · 2021 · IF 7.312

Highly efficient purification of natural coaly graphite via an electrochemical method

Ying Quan,Qinfu Liu,Kuo Li,Hao Zhang,Liang Yuan

Due to the fine granularity of CG with the dissemination of non-graphite minerals, highly efficient purification of natural coaly graphite (CG) by low-cost, low-energy consumption and low-pollution methods remains a challenge. In this study, a novel and efficient electrochemical method is demonstrated for purifying natural CG. The electrochemical purification is carried out in a mixed electrolyte containing 0.5 M (NH 4 ) 2 SO 4 and 10% HF with an optimum potential sequence starting at + 2.5 V for a few minutes followed by a short burst of + 5 V. The CG purification mechanism is proposed based on the experimental results. There are three main factors, namely, the type of the graphite anode, the electrolyte and the applied voltage are critical for effectively electrochemical purification. It is interesting to find that the main purified products are graphene mixed with graphite aggregates at a yield of 68%. Raman analysis indicates that the purified CG has fewer structural defects than the natural CG after removing the non-graphite minerals. Moreover, the XPS and FTIR analysis demonstrate that no other functional groups are grafted onto the parent graphite during this purification process. In comparison with the electrolyte only containing HF, the adding of 0.5 M (NH 4 ) 2 SO 4 in the HF electrolyte could reduce the amount of HF by more than 50%, which cuts the cost and alleviates the impact on the environment.

CAS / MDL: 7783-20-2
研究领域: 材料科学 · 化学工程 · 环境科学
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MICROPOROUS AND MESOPOROUS MATERIALS · 2020 · IF 4.551

Synthesis of well-shaped and high-crystalline Ce-based metal organic framework for CO2/CH4 separation

Junjie Zhou,Hao Liu,Yichao Lin,Chen Zhou,Aisheng Huang

A well-shaped Ce (IV)-based metal organic framework (Ce-BDC) is prepared under solvothermal method. The influence of synthesis time, temperature and the amount of acetic acid (HAc) as a modulator is studied to develop a new strategy for the synthesis of well-shaped Ce-based MOF. The relationship between the synthesis parameters and morphology as well as crystallinity of Ce-BDC is investigated by XRD and SEM. Furthermore, the obtained well-shaped Ce-BDC shows a CO 2 uptake capacity of 2.28 mmol g −1 at 0 °C and 1.0 bar. Meanwhile, the breakthrough curve behaviors of Ce-BDC are investigated for a CO 2 /CH 4 and CO 2 /N 2 mixture gas . It is found that the Ce-based MOF adsorbs CO 2 under ambient temperature and pressure, but completely excludes CH 4 and N 2 , suggesting that it is a promising adsorbent for efficient separation of CO 2 from natural gas.

研究领域: 材料科学 · 无机化学 · 多孔材料 · 气体分离 · 环境催化
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