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Journal of the Taiwan Institute of Chemical Engineers · 2023 · IF 5.7

Short flow and green process for the production of V2O3 powder via ammonia reduction method

Tao Zhang,Guiqing Zhang,Zuoying Cao,Mingyu Wang,Wenjuan Guan,Shengxi Wu,Qinggang Li

Background The NH 3 , a clean reductant, generated by the thermolysis of NH 4 VO 3 , is not effectively utilized in the conventional process of vanadium metallurgy. Additionally, the preparation process of V 2 O 3 is both long and costly. Ammonia recovery is essential to prevent environmental issues resulting from ammonia release. By direct thermolysis of NH 4 VO 3 and effectively utilizing of active NH 3 , it is possible to achieve the short flow and green process for the production of V 2 O 3 . Method In an open NH 3 atmosphere, one end of the flange was connected to the liquid ammonia gas cylinder, while the other end was connected to the tail gas absorber. Furthermore, in a closed NH 3 atmosphere, both ends of the tube furnace were sealed with flanges, and the initial atmosphere in the tube was pre-injection NH 3 . The products of NH 4 VO 3 thermolysis were characterized using various techniques, including XRD, FT-IR, ICP-OES, SEM, XPS, and TG. Significant finding The thermolysis process of NH 4 VO 3 with pre-injection of NH 3 under the sealed condition was a simulation of the continuous production process of V 2 O 3 using a rotary kiln in industrial production. The rational utilization of ammonia resulted in the reduce of energy consumption, extra reductant consumption, and significant NH 3 emissions compared to the traditional V 2 O 3 production process. It was observed that V 2 O 3 was easily obtained through the thermolysis of NH 4 VO 3 with pre-injection of NH 3 under the sealed condition at 600 °C for 3 h, using a dosage of NH 4 VO 3 ranging from 2 g to 10 g. During this process, the NH 4 VO 3 went through the phase transition as follows: NH 4 VO 3 →NH 4 V 3 O 8 →(NH 4 ) 0.38 V 2 O 5 →V 6 O 13 →VO 2 →V 4 O 7 →V 3 O 5 →V 2 O 3 , and the relevant characterization of products showed that the V 2 O 3 obtained was qualified. These experimental results were of great significance to the industrial practice of vanadium metallurgy. Based on these results, short flow and green process of V 2 O 3 could be achieved in industry by partially improving the calcination process of NH 4 VO 3 in large-scale rotary kilns.

CAS / MDL: 7803-55-6
研究领域: 冶金学 · 材料科学 · 环境工程
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Journal of Natural Fibers · 2023 · IF 3.5

A Facile Method to Manufacture the Sesamum Indicum Fibers by Glycolic Acid Assisted with Microwave

Boya Li,Kai Nie,Linlin Li,Gang Fu,Chunguo Liu,Shouwu Gao,Guangting Han,Tao Zhao,Wei Jiang

The Sesamum indicum bast contains more hemicellulose, lignin, and flaky parenchymal cells than the commonly used ramie bast, which are rigid for the degumming process. We explored a facile and greener method by using glycolic acid microwave-assisted treatment combined with alkaline treatment to effectively and low-cost prepare the high-quality Sesamum indicum single fibers. The chemical and physical properties of fibers were analyzed by chemical composition analysis, SEM, FTIR, XRD, TG, and GPC analysis. The residual gum content was decreased from 34.4% to 4.2%, resulting in a cleaner micro-surface of the Sesamum indicum fibers with increased cellulose crystallinity (75.2%–82.5%) and thermal stability (357°C–365°C). The fiber fineness (2.5 dtex) and breaking tenacity (4.9 cN/dtex) of the fibers produced by the novel treatment method exhibited the same level compared with the traditional two-step alkaline fibers. Besides, both the consumption of water and the chemicals was decreased compared with traditional degumming. This work provided a novel green and facile degumming method for processing the natural bast fibers.

研究领域: 材料科学 · 植物学
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JOURNAL OF THE ELECTROCHEMICAL SOCIETY · 2021 ·Vol. 168 ·期 12 ·123509 · IF 4.316

Preparation of MoB2 Nanoparticles by Electrolysis of MoS2/B Mixture in Molten NaCl-KCl at 700 °C

Xianglin Liu,Yongsong Ma,Peng Li,Huayi Yin,Dihua Wang

MoB2 is synthesized by the electrochemical reduction of solid MoS2/B mixture in molten NaCl-KCl at 700 °C. Unlike the traditional methods, the electrolysis method employs the low-cost MoS2 feedstock and the boronization reaction happens at a low temperature of 700 °C. The electrochemically induced boronization involves two steps: the electrochemical desulfurization to generate Mo and the reaction of Mo with B to form MoB2. The S2− released from the reduction of MoS2 transfers to the carbon anode and is oxidized to sulfur gas, realizing a green synthetic process. In addition, the influences of molar ratio of MoS2 and amorphous boron and electrolysis cell voltage on the phase composition and morphology of electrolytic products were studied. The obtained MoB2 particles possess a uniform nodular morphology. Overall, this paper provides a straightforward and green process to prepare MoB2 nanoparticles using economically affordable raw materials at low temperature, and this method can be extended to prepare other borides.

研究领域: 材料科学 · 电化学
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ACS Sustainable Chemistry & Engineering · 2022 · IF 9.224

Green Electrorefining of Crude Lead with High-Quality Deposits in an Additive-Assisted Methanesulfonic Acid System

Changliu Xiang,Sijun Zhu,Jinbo Song,Yougang Li,Tao Luo,Cong Chang,Junjie Qu,Shenghai Yang,Changhong Wang,Yongming Chen

The conventional electrorefining process of crude lead (Pb)─employing a bone glue (BG)- and calcium lignosulfonate (CL)-synergistically assisted fluosilicic acid (H2SiF6) system─suffers the undesired environment burden caused by the high saturated vapor pressure and low stability of H2SiF6. Herein, we propose an additive-assisted methanesulfonic acid (MSA) system for green and efficient electrorefining of crude Pb based on the low volatility and high stability of MSA. Combinations of MSA with additives are evaluated and screened using photographic images, SEM observations, XRD, white light interference, etc. The electrochemical analysis of cyclic voltammetry and chronoamperometry elucidates the Pb deposition behavior in the Lugalvan BNO12-assisted MSA system, in which a three-dimensional nucleation model is applicable. Using MSA as the solvent and β-naphthol ethoxylate (Lugalvan BNO12) as the assisted additive, the bench-scale operation of crude Pb electrorefining experimentally achieves an electric energy requirement (W) of 87 kWhe/t Pb and a cathodic current efficiency (η) of 99.6%. This is very competitive with the W of 120 kWhe/t Pb and η of 95.0% for the BG-CL-assisted H2SiF6 system. Also, the bench-scale operation obtains a plat and dense deposit sample with a Pb purity of >99.99%. The distribution behavior of elements shows that most of the Pb element is recovered in the form of the cathodic Pb, elements Sn, Zn, and Fe mainly accumulate in the electrolyte, and elements As, Sb, Bi, Ag, and Cu remain in the anode slime. This work opens new directions for more technically and economically feasible Pb electrorefining.

研究领域: 冶金工程 · 环境科学
✓ 已验证 DOI 高影响因子
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SEPARATION AND PURIFICATION TECHNOLOGY · 2023 · IF 8.6

Environmentally friendly and efficient green recovery of fluoride from waste aluminum electrolytic sediment using Al2O3

Wenju Tao,Jiaxin Yang,Liyu Chen,Yifan Zhang,Shaohua Wu,Jiaming Li,Zhaoshun Liu,Jingui He,Zhaowen Wang

Green and efficient recovery of solid waste from aluminum electrolysis is of great significance. In this study, the sediment generated by aluminum electrolysis at the bottom of the waste tank was used as an alternative F resource. A new process of low-temperature acidification roasting with Al 2 O 3 as the catalyst was performed to effectively recover F. The results of the single-factor experiment showed that a long reaction time and high acid-material ratio were conducive to improving the extraction rate of F. Under the conditions of 275 °C and 5 doses of sulfuric acid, the optimum F extraction rate was realized by roasting for 4 h with 1 dose of Al 2 O 3 as the catalyst. The results of the XRD, SEM and chemical analyses showed that NaAl(SO 4 ) 2 was the main component produced in the calcination reaction using Al 2 O 3 as the catalyst, rather than NaHSO 4 (produced in the calcination process without a catalyst). This ensured complete combination of H and F, which greatly improved the extraction rate of F (from 80.76 to 99.76%). The proposed mechanism can provide not only an optimization scheme for the roasting of waste sediment at the furnace bottom, but also a more effective recovery treatment for the acidification roasting of other solid wastes with low Al 2 O 3 content.

研究领域: 环境科学 · 冶金工程
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Journal of Sustainable Metallurgy · 2024 · IF 2.5

Preparation of High-Purity PbO Powder from Waste Lead Paste via Leaching Reagents Recovery

Yang Yi,Ouyang Lun-ao,He Yapeng,He Puqiang,Tu Jian,Huang Hui,Guo Zhongcheng

The hydrometallurgical recycling of spent lead-acid battery has received extensive attention benefitting from its features of cleanability and process controllability, but the process still suffers from significant challenges of huge chemical consumption and low economic efficiency. Here, a sustainable green approach that enables closed-loop recovery of leaching reagent NH 4 Ac to obtain high-purity PbO powder from discarded lead paste is proposed. The process includes dissolution, chemical transformation, carbonization, and calcination stages. Under the optimal leaching condition of NH 4 Ac concentration 4.5 mol L –1 , H 2 O 2 /PbO 2 molar ratio 1.5, reaction temperature 40 °C, and time 60 min, the leaching ratio of lead reaches as high as 99.35%. The exceptionally high concentration of NH 4 Ac to dissolve PbSO 4 phases than theoretical ratio could be attributed to the distribution state of Pb substances. With (NH 4 ) 2 CO 3 as carbonizing agent, above 99.9% of lead could be precipitated as PbCO 3 products when the molar ratio CO 3 2– /Pb is 1.2. High-purity β-PbO powder is subsequently achieved from the thermal decomposition of PbCO 3 precursor, where the effect of calcination temperature and atmosphere on the chemical compositions are examined. Economic analysis reveals the economic feasibility and profits of the recycling approach. The process produces high-purity PbCO 3 and PbO products enabling leaching reagents NH 4 Ac reuse, providing a practicable solution for sustainable recovery of lead from waste lead paste. Graphical

研究领域: 环境科学 · 冶金工程
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JOURNAL OF HAZARDOUS MATERIALS · 2020 · IF 9.038

Recycling lithium cobalt oxide from its spent batteries: An electrochemical approach combining extraction and synthesis

Jianbo Wang,Juan Lv,Mingxing Zhang,Miqi Tang,Qi Lu,Yufei Qin,Yan Lu,Bo Yu

LiCoO 2 LiCoO2 is still the most extensively used cathode material in Li-ion battery for portable electronics currently. The increasing usage of electronics has resulted in the growing discard of LiCoO 2 LiCoO2 with the stream of its spent battery. Current recycling approaches for LiCoO 2 LiCoO2 from spent batteries are dominantly based on hydrometallurgy and pyrometallurgy , which usually require multiple complicated steps and involve the use of high temperature or harmful chemicals, like acids and alkalis. There remains an urgent need for green and simple processes. Here we report a single step approach based on suspension electrolysis to directly recycle LiCoO 2 LiCoO2 in one reactor at atmospheric condition without any usage of acid and alkalis. The electrolyte of the suspension electrolysis system is only comprised of NH 4 HCO 3 NH4HCO3 , NH 4 2 SO 3 NH42SO3 and NaF NaF . The reaction system of LiCoO 2 LiCoO2 leaching in the anode region and simultaneously re-synthesizing in the cathode region in the electrochemical system is established. Mechanism analysis indicates that NH 4 + NH4+ only serves as a provider for complexing agent of NH 3 NH3 and is virtually not consumed. This work provides potentially meaningful strategies for recovering LiCoO 2 LiCoO2 in a shorter procedure and an environmentally friendly manner.

研究领域: 材料科学 · 环境科学 · 电化学
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INTERNATIONAL JOURNAL OF HYDROGEN ENERGY · 2019 · IF 4.084

Molten salt electrochemical production and in situ utilization of hydrogen for iron production

Kaiyu Xie,Ali Reza Kamali

The low voltage electrochemical extraction of iron from iron oxide powder is reported. Hydrogen gas can be generated in molten LiCl at 660 °C by the electrochemical decomposition of steam at a voltage as low as only 0.97 V. Interestingly, individual submicrometer-sized iron oxide particles simply immersed in the melt can directly be reduced to semi-spherical metallic iron particles with a particle size of about 5 μm under the influence of hydrogen gas generated in-situ in the molten salt. The direct reduction of Fe 2 O 3 powder, instead of sintered Fe 2 O 3 pellets, which are commonly used as the cathode in the conventional molten salt electro-deoxidation processes, enhances the simplicity, energy consumption and the reaction kinetics of the molten salt hydrogen reduction process. In this method, the bottom surface of the graphite crucible acts as the cathode, resulting in a high rate of hydrogen cations discharge, hence a high current. The high temperature and low voltage characteristics of this method offer a scalable strategy for direct reduction of metal oxide particles in a green and low-cost way, where there is no requirement for the compaction of metal oxide powders into pellets. The mechanism involved in this hydrogen production and utilization methodology is discussed.

CAS / MDL: 1309-37-1 20344-49-4
研究领域: 冶金学 · 电化学 · 能源科学
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Journal of Analysis and Testing · 2023 · IF 4.7

Extraction of Eugenol from Essential Oils by In Situ Formation of Deep Eutectic Solvents: A Green Recyclable Process

Shen Lingqi,Jin Xiangzi,Zhang Zhihui,Yi Yuexing,Zhang Jingyu,Li Zuguang

Eugenol is extensively utilized in chemical industry. In actual production, it is mainly separated from clove essential oils (EOs) through acid–base solutions. In this work, a simple, rapid and effective extraction process was developed for the extraction of eugenol from EOs samples by directly forming deep eutectic solvents (DESs) without using acid–base solutions. The proposed process is designed to dissolve EOs in n -hexane and eugenol was highly selective extracted into DESs with tetrabutylammonium chloride (TBAC). Hydrogen bonds in DESs can be broken by addition of water, resulting in a separation of the two phases, thus obtaining a hydrophobic yellowish eugenol in the upper layer. The quaternary ammonium salt in the lower aqueous solution can be reused after recovery. The most determining influence factors such as the structure of quaternary ammonium salt, the mole ratio of quaternary ammonium salt to eugenol and the amount of n -hexane were investigated. The forming conditions of DESs were studied by Box–Behnken design (BBD). Experiment was carried out under the optimal conditions and good experimental result was demonstrated by the developed process, a high extraction recovery of 92.51% and the purity was about 98.50%, which verifies the excellent performance for the proposed process.

研究领域: 化学工程 · 环境科学
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CHEMICAL ENGINEERING & TECHNOLOGY · 2020 ·Vol. 43 ·期 11 ·2160-2166 · IF 1.543

Hybrid Extraction of Oily Sludge by Tertiary Amines and Protonated Tertiary Amines

Shanshan Dai,Xiaojiang Li,Jihe Zhao,Hongsheng Lu

A green and effective extraction of oily sludge was completed by a hybrid process with tertiary amines (TA) and protonated tertiary amines (PTA), where PTA is the protonated state of TA. Compared with only TA, the crude oil recovery was improved by 3–5 % by the addition of PTA and less solid remained in the recovered crude oil. Additionally, the wettability improved with the absorption of positively charged ions of PTA on the sludge, and the interaction between heavy alkanes of crude oil and PTA promotes the detachment of crude oil from the sludge surface, enhancing the hydrophilicity of sludge. More importantly, the incomplete recovery of TA exactly takes the role of the PTA in the regenerated mixture, which can reduce the loss of solvent.

研究领域: 环境科学 · 化学工程
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RSC Advances · 2021 ·Vol. 11 ·期 62 ·39153-39168 · IF 3.361

Electroless deposition of Ni–P/Au coating on Cu substrate with improved corrosion resistance from Au(III)–DMH based cyanide-free plating bath using hypophosphite as a reducing agent

Bo Wu,Baizhao Tan,Guizhen Tan,Ming Zeng,Jinyi Luo,Guanghui Hu,Jiye Luo,Zhifeng Hao,Shaomei Lai,Binyun Liu

The green cyanide-free gold deposition is an important development direction in electroless gold plating. However, the commonly Au(I) based cyanide-free gold plating bath always suffers from severe corrosion to the Ni–P layer and unsatisfactory service life of the bath. In this work, a green and environmentally friendly cyanide-free gold plating bath was developed with hypophosphite added as a reducing agent into the Au(III)–DMH (5,5-dimethylhydantoin) based plating bath to retard the corrosion of the Ni–P layer. SEM micrographs combined with XRD and XPS analysis indicated that the electroless deposited gold was pure and compact. And XRD also revealed that the oriented deposition of gold was growing preferentially on Au (111). Corrosion tests, including salt spray tests, potentiodynamic polarization tests, and electrochemical impedance spectroscopy tests, indicated that the obtained Cu/Ni–P/Au coatings had significantly improved corrosion resistance performance with the loading of hypophosphite as the reducing agent. The baths remained transparent and no turbidity or precipitates were detected for 210 days, reflecting good stability. The detection for the Ni2+ concentration in the bath showed that adding hypophosphite could retard the replacement reaction between Au3+ and the Ni–P layer in part and this is important for decreasing the severe corrosion of the Ni–P layer. Moreover, Au was inactive for catalyzing the oxidation of hypophosphite during the deposition process which was confirmed furthermore via quantum chemical calculations. Therefore, our developed green cyanide-free electroless gold deposition process can beneficially provide research value and application prospects in microelectronic industry.

研究领域: 材料科学 · 电化学 · 环境科学
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SEPARATION AND PURIFICATION TECHNOLOGY · 2025 · IF 9

Development of a green and optimized process for isolating high-purity naringin and neohesperidin from Qu aurantii fructus

Ziwei Wang,Xiaojing Hou,Junxuan Jin,Yuchen He,Kejun Wu

This study introduces a green, optimized process for efficiently extracting high-purity naringin and neohesperidin from Qu Aurantii Fructus, a valuable traditional Chinese medicine. The total flavonoids from Qu Aurantii Fructus were extracted using ultrasonic-assisted ethanol extraction and subsequently purified with AB-8 resin, followed by the separation of high-purity naringin and neohesperidin through polyamide column chromatography. The investigation into the effect of ultrasound duration on the yield of total flavonoids revealed that at an ultrasonic duration of 25 min, the extraction yield of total flavonoids can reach its maximum. A thin-layer chromatography (TLC) system was employed to optimize the solvent system for the separation of naringin and neohesperidin, utilizing machine vision to assist in calculating and predicting the optimal solvent ratio, thereby simplifying the process and reducing variability and bias. The optimal solvent ratio (ethanol/ethyl acetate = 0.2848) was identified, leading to the successful isolation of high-purity naringin and neohesperidin (95.15 % and 99 %, respectively) through polyamide column chromatography and recrystallization. This process is devoid of toxic organic reagents, which enhances process safety and presents potential prospects for industrial applications, offering an efficient and eco-friendly method for the extraction and purification of valuable natural products

CAS / MDL: 7664-38-2
研究领域: 中药化学 · 天然产物分离纯化
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