Vanadium extraction from stone-coal was investigated by oxygen pressure acid leaching and solvent extraction.The mineralogy of the stone-coal from Tongren City of Guizhou Province,China,was investigated by various det...Vanadium extraction from stone-coal was investigated by oxygen pressure acid leaching and solvent extraction.The mineralogy of the stone-coal from Tongren City of Guizhou Province,China,was investigated by various determination methods. The effects of leaching time,leaching temperature,leaching agent concentration,leaching L/S ratio,granularity of material,additive consumption were investigated based on the mineralogy.The results show that under the conditions of leaching time of 3-4 h, temperature of 150℃,sulfuric acid consumption of 25%?30%,ratio of liquid to solid of 1.2:1,the granularity less than 0.074 mm, additive consumption of 3%-5%,and oxygen pressure of 1.2 MPa,and the vanadium leaching rate can be more than 92%by the method of two-step pressurized acid leaching.The powdery V2O5 product with 99.52%in V2O5 content is obtained by the flowsheet of acid recovery,removing iron by reduction process,solvent extraction,precipitating vanadium with ammonium water,and pyrolysis from the stone-coal oxygen pressure acid-leaching solution.The total recovery efficiency of vanadium is above 85%,which is more than 20%higher than that obtained in the conventional process.Furthermore,the new process does not cause air pollution since no HCl or Cl2 is released by calcination of the raw material.展开更多
To extract vanadium in an environment friendly manner, this study focuses on the process of leaching vanadium from vanadium slag by high pressure oxidative acid leaching. Characterizations of the raw slag, mineralogy ...To extract vanadium in an environment friendly manner, this study focuses on the process of leaching vanadium from vanadium slag by high pressure oxidative acid leaching. Characterizations of the raw slag, mineralogy transformation, and the form of leach residues were made by X-ray diffraction, scanning electron microscopy, and energy dispersive X-ray spectroscopy. The result shows that the vana-dium slag is composed of major phases of fayalite, titanomagnetite, and spinel. During the high pressure oxidative acid leaching process, the fayalite and spinel phases are gradually decomposed by sulfuric acid, causing the release of vanadium and iron in the solution. Meanwhile, unreacted silicon and titanium are enriched in the leach residues. With the initial concentration of sulfuric acid at 250 g·L^-1, a leaching tem-perature of 140℃, a leaching time of 50 min, a liquid-solid ratio of 10：1 mL·g^-1, and oxygen pressure at 0.2 MPa, the leaching rate of vana-dium reaches 97.69%.展开更多
[Objectives]To explore the process of simultaneous extracting total flavonoids and chlorogenic acid from Flos Lonicerae by pressure assisted extraction.[Methods]Based on the single factor experiment,orthogonal experim...[Objectives]To explore the process of simultaneous extracting total flavonoids and chlorogenic acid from Flos Lonicerae by pressure assisted extraction.[Methods]Based on the single factor experiment,orthogonal experiments were carried out to investigate the effects of solvent concentration,solid-to-liquid ratio,extraction pressure,extraction time and extraction temperature on the extraction rate of total flavonoids and chlorogenic acid.[Results]The results showed that the extraction pressure had a significant effect on the extraction of two kinds of chemical constituents from F.Lonicerae.The optimum process conditions were as follows:solvent concentration was 60%,solid-liquid ratio was 1∶20(g/mL),extraction pressure was 2 MPa,extraction time was 30 min,extraction temperature was 70℃.The process conditions are stable,and the extraction efficiency is higher than that of ultrasonic assisted extraction method.Under the test conditions,the extraction rates of total flavonoids and chlorogenic acids were respectively 15.66%and 3.89%.[Conclusions]This study provides a new theoretical basis for the development and utilization of F.Lonicerae.展开更多
The aim of the present study was to evaluate the effects of baobab seed washing and origin on the chemical composition of the oil extracted by pressing. Six (6) oil samples were obtained from seeds of three (3) geogra...The aim of the present study was to evaluate the effects of baobab seed washing and origin on the chemical composition of the oil extracted by pressing. Six (6) oil samples were obtained from seeds of three (3) geographical origins. The identification and quantification of fatty acids and the polyphenolic profile were carried out by GC-MS and HPLC-UV, respectively. Analysis of fatty acid methyl esters allowed the identification and quantification of 18 fatty acids. Oils from unwashed seeds were richer in palmitic (C16:0), stearic (C18:0), oleic (C18:1) and arachidic (C20:0) acids. In addition, HPLC-UV analysis at 279 nm shows that oils from unwashed seeds are richer in tyrosol, hydroxytyrosol and caffeic acid. With regard to the polyphenolic profile, gallic acid and quercetin were not detected in these baobab oils. Principal component analysis of fatty acid and phenolic compound content showed that oils from unwashed seeds would best preserve their chemical and associated potential bioactive characteristics.展开更多
Zinc silicate ore was characterized mineralogically and the results showed that zinc exists mainly as hemimorphite and smithsonite in the sample.Sulfuric acid pressure leaching of zinc silicate ore was carried out to ...Zinc silicate ore was characterized mineralogically and the results showed that zinc exists mainly as hemimorphite and smithsonite in the sample.Sulfuric acid pressure leaching of zinc silicate ore was carried out to assess the effect of particle size,sulfuric acid concentration,pressure,reaction time and temperature on the extraction of zinc and the dissolution of silica.Under the optimum conditions employed,up to 99.25% of zinc extraction and 0.20% silica dissolution are obtained.The main minerals in leaching residue are quartz and small amounts of undissolved oxide minerals of iron,lead and aluminum are associated with quartz.展开更多
The present study was designed to establish and optimize a new method for extracting chlorogenic acid and cynaroside from Lonicera japonica Thunb. through orthogonal experimental designl. A new ultrahigh pressure extr...The present study was designed to establish and optimize a new method for extracting chlorogenic acid and cynaroside from Lonicera japonica Thunb. through orthogonal experimental designl. A new ultrahigh pressure extraction （UPE） technology was applied to extract chlorogenic acid and cynaroside from L. japonica. The influential factors, including solvent type, ethanol concentration, extraction pressure, time, and temperature, and the solid/liquid ratio, have been studied to optimize the extraction process, The optimal conditions for the UPE were developed by quantitative analysis of the extraction products by HPLC-DAD in comparison with standard samples. In addition, the microstructures of the medicinal materials before and after extraction were studied by scanning electron microscopy （SEM）. Furthermore, the extraction efficiency of different extraction methods and the 2, 2-diphenyl-1-picrylhydrazyl （DPPH） radical scavenging activities of the extracts were investigated. The optimal conditions for extracting chlorogenic acid and cynaroside were as follows： ethanol concentration, 60%; extraction pressure, 400 MPa; extraction time, 2 rain; extraction temperature, 30 ℃; and the solid/liquid ratio, 1 ： 50. Under these conditions, the yields of chlorogenic acid and cynaroside were raised to 4.863% and 0.080%, respectively. Compared with other extraction methods, such as heat reflux extraction （HRE）, ultrasonic extraction （UE）, and Sohxlet extraction （SE）, the UPE method showed several advantages, including higher extraction yield, shorter extraction time, lower energy consumption, and higher purity of the extracts. This study could help better utilize L. japonica flower buds as a readily accessible source of natural antioxidants in food and pharmaceutical industries.展开更多
建立了高效液相色谱串联质谱技术（Liquid chromatography tandem mass spectrometry,LC-MS/MS）同时测定土壤中邻苯二甲酸酯（Phthalic acid esters,PAEs）的分析方法。确定了土壤样品加速溶剂萃取最优条件是以正己烷为萃取溶剂,在160...建立了高效液相色谱串联质谱技术（Liquid chromatography tandem mass spectrometry,LC-MS/MS）同时测定土壤中邻苯二甲酸酯（Phthalic acid esters,PAEs）的分析方法。确定了土壤样品加速溶剂萃取最优条件是以正己烷为萃取溶剂,在160℃下,静态萃取4次,每次12 min,萃取液经旋转蒸发浓缩,以乙腈-0.1%甲酸溶液为流动相梯度洗脱分离后,用LC-MS/MS结合大气压化学源（Atmospheric pressure chemical ionization,APCI）进行定性及定量分析。土壤中11种PAEs的浓度与其峰面积呈良好的线性关系,检出限为0.03-13.0μg/kg,样品的加标平均回收率为72.8%-101.8%,相对标准偏差（RSD）为1.7%-6.7%。方法简便快速,且灵敏度高,适用于土壤中11种邻苯二甲酸酯的同时测定。展开更多
为探索提高石煤中钒的浸出效率,以湖北通山某石煤矿石为研究对象,进行了石煤焙烧—加压酸浸提钒工艺研究。结果表明：在焙烧温度为850℃、焙烧时间为60 min、釜内压力为1.0 MPa、硫酸初始浓度为15%、液固比为1.5 m L/g、浸出温度为150...为探索提高石煤中钒的浸出效率,以湖北通山某石煤矿石为研究对象,进行了石煤焙烧—加压酸浸提钒工艺研究。结果表明：在焙烧温度为850℃、焙烧时间为60 min、釜内压力为1.0 MPa、硫酸初始浓度为15%、液固比为1.5 m L/g、浸出温度为150℃、浸出时间为120 min条件下,钒浸出率可达80.51%。采用红外光谱法分析了加压浸出前后云母矿物的晶体结构,并从动力学的角度揭示了浸出温度对钒浸出的影响机理。结果表明：加压浸出可以破坏云母晶格,进而有利于释放云母晶格中的钒,提高钒浸出效果。浸出过程动力学分析结果表明：浸出温度对浸出过程影响显著,浸出温度为60-120℃时,表观活化能为41.603 k J/mol,浸出过程受化学反应控制;150-210℃时,表观活化能为4.319 k J/mol,浸出过程受内扩散控制;加压浸出能够将浸出温度提高至100℃以上,有效提高了硫酸破坏云母晶格的速率,是提高钒浸出效率的关键。展开更多
基金Project(2006AA06Z130)supported by the High-tech Research and Development Program of ChinaProject(50874053)supported by the National Natural Science Foundation of ChinaProject(2007GA010)supported by Science and Technology Bureau of Yunnan Province,China
文摘Vanadium extraction from stone-coal was investigated by oxygen pressure acid leaching and solvent extraction.The mineralogy of the stone-coal from Tongren City of Guizhou Province,China,was investigated by various determination methods. The effects of leaching time,leaching temperature,leaching agent concentration,leaching L/S ratio,granularity of material,additive consumption were investigated based on the mineralogy.The results show that under the conditions of leaching time of 3-4 h, temperature of 150℃,sulfuric acid consumption of 25%?30%,ratio of liquid to solid of 1.2:1,the granularity less than 0.074 mm, additive consumption of 3%-5%,and oxygen pressure of 1.2 MPa,and the vanadium leaching rate can be more than 92%by the method of two-step pressurized acid leaching.The powdery V2O5 product with 99.52%in V2O5 content is obtained by the flowsheet of acid recovery,removing iron by reduction process,solvent extraction,precipitating vanadium with ammonium water,and pyrolysis from the stone-coal oxygen pressure acid-leaching solution.The total recovery efficiency of vanadium is above 85%,which is more than 20%higher than that obtained in the conventional process.Furthermore,the new process does not cause air pollution since no HCl or Cl2 is released by calcination of the raw material.
基金supported by the National High Technology Research and Development Program of China(No.2012AA062303)the National Natural Science Foundation of China(Nos.U1202274,51004033,and 51204040)the Doctoral Fund Project of China(No. 20120042110011)
文摘To extract vanadium in an environment friendly manner, this study focuses on the process of leaching vanadium from vanadium slag by high pressure oxidative acid leaching. Characterizations of the raw slag, mineralogy transformation, and the form of leach residues were made by X-ray diffraction, scanning electron microscopy, and energy dispersive X-ray spectroscopy. The result shows that the vana-dium slag is composed of major phases of fayalite, titanomagnetite, and spinel. During the high pressure oxidative acid leaching process, the fayalite and spinel phases are gradually decomposed by sulfuric acid, causing the release of vanadium and iron in the solution. Meanwhile, unreacted silicon and titanium are enriched in the leach residues. With the initial concentration of sulfuric acid at 250 g·L^-1, a leaching tem-perature of 140℃, a leaching time of 50 min, a liquid-solid ratio of 10：1 mL·g^-1, and oxygen pressure at 0.2 MPa, the leaching rate of vana-dium reaches 97.69%.
基金Supported by Scientific Research Project of Hunan Provincial Department of Education in 2017(17C1603)
文摘[Objectives]To explore the process of simultaneous extracting total flavonoids and chlorogenic acid from Flos Lonicerae by pressure assisted extraction.[Methods]Based on the single factor experiment,orthogonal experiments were carried out to investigate the effects of solvent concentration,solid-to-liquid ratio,extraction pressure,extraction time and extraction temperature on the extraction rate of total flavonoids and chlorogenic acid.[Results]The results showed that the extraction pressure had a significant effect on the extraction of two kinds of chemical constituents from F.Lonicerae.The optimum process conditions were as follows:solvent concentration was 60%,solid-liquid ratio was 1∶20(g/mL),extraction pressure was 2 MPa,extraction time was 30 min,extraction temperature was 70℃.The process conditions are stable,and the extraction efficiency is higher than that of ultrasonic assisted extraction method.Under the test conditions,the extraction rates of total flavonoids and chlorogenic acids were respectively 15.66%and 3.89%.[Conclusions]This study provides a new theoretical basis for the development and utilization of F.Lonicerae.
文摘The aim of the present study was to evaluate the effects of baobab seed washing and origin on the chemical composition of the oil extracted by pressing. Six (6) oil samples were obtained from seeds of three (3) geographical origins. The identification and quantification of fatty acids and the polyphenolic profile were carried out by GC-MS and HPLC-UV, respectively. Analysis of fatty acid methyl esters allowed the identification and quantification of 18 fatty acids. Oils from unwashed seeds were richer in palmitic (C16:0), stearic (C18:0), oleic (C18:1) and arachidic (C20:0) acids. In addition, HPLC-UV analysis at 279 nm shows that oils from unwashed seeds are richer in tyrosol, hydroxytyrosol and caffeic acid. With regard to the polyphenolic profile, gallic acid and quercetin were not detected in these baobab oils. Principal component analysis of fatty acid and phenolic compound content showed that oils from unwashed seeds would best preserve their chemical and associated potential bioactive characteristics.
基金Project(2007CB613605) supported by the National Basic Research Program of China
文摘Zinc silicate ore was characterized mineralogically and the results showed that zinc exists mainly as hemimorphite and smithsonite in the sample.Sulfuric acid pressure leaching of zinc silicate ore was carried out to assess the effect of particle size,sulfuric acid concentration,pressure,reaction time and temperature on the extraction of zinc and the dissolution of silica.Under the optimum conditions employed,up to 99.25% of zinc extraction and 0.20% silica dissolution are obtained.The main minerals in leaching residue are quartz and small amounts of undissolved oxide minerals of iron,lead and aluminum are associated with quartz.
基金supported by the PAPD(A Project Funded by the Priority Academic Program Development of Jiangsu Higher Education Institutions)
文摘The present study was designed to establish and optimize a new method for extracting chlorogenic acid and cynaroside from Lonicera japonica Thunb. through orthogonal experimental designl. A new ultrahigh pressure extraction （UPE） technology was applied to extract chlorogenic acid and cynaroside from L. japonica. The influential factors, including solvent type, ethanol concentration, extraction pressure, time, and temperature, and the solid/liquid ratio, have been studied to optimize the extraction process, The optimal conditions for the UPE were developed by quantitative analysis of the extraction products by HPLC-DAD in comparison with standard samples. In addition, the microstructures of the medicinal materials before and after extraction were studied by scanning electron microscopy （SEM）. Furthermore, the extraction efficiency of different extraction methods and the 2, 2-diphenyl-1-picrylhydrazyl （DPPH） radical scavenging activities of the extracts were investigated. The optimal conditions for extracting chlorogenic acid and cynaroside were as follows： ethanol concentration, 60%; extraction pressure, 400 MPa; extraction time, 2 rain; extraction temperature, 30 ℃; and the solid/liquid ratio, 1 ： 50. Under these conditions, the yields of chlorogenic acid and cynaroside were raised to 4.863% and 0.080%, respectively. Compared with other extraction methods, such as heat reflux extraction （HRE）, ultrasonic extraction （UE）, and Sohxlet extraction （SE）, the UPE method showed several advantages, including higher extraction yield, shorter extraction time, lower energy consumption, and higher purity of the extracts. This study could help better utilize L. japonica flower buds as a readily accessible source of natural antioxidants in food and pharmaceutical industries.
文摘建立了高效液相色谱串联质谱技术（Liquid chromatography tandem mass spectrometry,LC-MS/MS）同时测定土壤中邻苯二甲酸酯（Phthalic acid esters,PAEs）的分析方法。确定了土壤样品加速溶剂萃取最优条件是以正己烷为萃取溶剂,在160℃下,静态萃取4次,每次12 min,萃取液经旋转蒸发浓缩,以乙腈-0.1%甲酸溶液为流动相梯度洗脱分离后,用LC-MS/MS结合大气压化学源（Atmospheric pressure chemical ionization,APCI）进行定性及定量分析。土壤中11种PAEs的浓度与其峰面积呈良好的线性关系,检出限为0.03-13.0μg/kg,样品的加标平均回收率为72.8%-101.8%,相对标准偏差（RSD）为1.7%-6.7%。方法简便快速,且灵敏度高,适用于土壤中11种邻苯二甲酸酯的同时测定。
文摘为探索提高石煤中钒的浸出效率,以湖北通山某石煤矿石为研究对象,进行了石煤焙烧—加压酸浸提钒工艺研究。结果表明：在焙烧温度为850℃、焙烧时间为60 min、釜内压力为1.0 MPa、硫酸初始浓度为15%、液固比为1.5 m L/g、浸出温度为150℃、浸出时间为120 min条件下,钒浸出率可达80.51%。采用红外光谱法分析了加压浸出前后云母矿物的晶体结构,并从动力学的角度揭示了浸出温度对钒浸出的影响机理。结果表明：加压浸出可以破坏云母晶格,进而有利于释放云母晶格中的钒,提高钒浸出效果。浸出过程动力学分析结果表明：浸出温度对浸出过程影响显著,浸出温度为60-120℃时,表观活化能为41.603 k J/mol,浸出过程受化学反应控制;150-210℃时,表观活化能为4.319 k J/mol,浸出过程受内扩散控制;加压浸出能够将浸出温度提高至100℃以上,有效提高了硫酸破坏云母晶格的速率,是提高钒浸出效率的关键。
