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Immobilisation of Molybdenum in a Sulphate-Reducing Bioreactor 在硫酸盐还原生物反应器中固定钼
IF 2.6 4区 工程技术 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-25 DOI: 10.3390/separations11010009
P. Kousi, Dimitra-Artemis Strongyli, P. Tsakiridis, A. Hatzikioseyian, E. Remoundaki
This work presents a biological remediation process for molybdenum-bearing wastewater which may lead to the fabrication of biogenic Mo chalcogenide particles with (photo)catalytic properties. The process is based on dissimilatory sulphate reduction, utilising sulphate-reducing bacteria (SRB), and reductive precipitation of molybdate which is the predominant species of molybdenum in oxygenated water/wastewater. The SRB culture was established in a biofilm reactor which was fed with synthetic solutions containing sulphate (17.7 mM), molybdate molybdenum (2 mM), divalent iron (1.7 mM) and ethanol as the carbon/electron donor. The performance of the bioreactor was monitored in terms of pH, sulphate and molybdenum (Mo(VI) and total) content. The presence of thiomolybdate species was studied by scanning UV-Vis absorbance of samples from the reactor outflow while the reactor precipitates were studied via electron microscopy coupled with energy dispersive spectrometry, X-ray diffractometry and laser light scattering. A molar molybdate/sulphate ratio of 1:12.5 proved effective for molybdate reduction and recovery by 76% in 96 h, whereas sulphate was reduced by 57%. Molybdenum was immobilised in the sulphidic precipitates of the bioreactor, presumably via two principal mechanisms: (i) microbially mediated reduction and precipitation, and (ii) thiomolybdate formation and sorption/incorporation into iron sulphides.
本研究提出了一种含钼废水的生物修复工艺,可用于制造具有(光)催化特性的生物钼铬化物颗粒。该工艺的基础是利用硫酸盐还原菌(SRB)进行硫酸盐异纤还原,以及钼酸盐(含氧水/废水中最主要的钼)的还原沉淀。SRB 培养是在生物膜反应器中进行的,该反应器以含有硫酸盐(17.7 毫摩尔)、钼酸盐钼(2 毫摩尔)、二价铁(1.7 毫摩尔)和作为碳/电子供体的乙醇的合成溶液为原料。根据 pH 值、硫酸盐和钼(Mo(VI) 和钼总)含量对生物反应器的性能进行了监测。通过扫描反应器流出样品的紫外-可见吸光度来研究硫代钼酸盐的存在,同时通过电子显微镜结合能量色散光谱仪、X 射线衍射仪和激光光散射来研究反应器沉淀物。事实证明,钼酸盐/硫酸盐摩尔比为 1:12.5 能有效地还原钼酸盐,96 小时内还原率为 76%,而硫酸盐的还原率为 57%。钼被固定在生物反应器的硫酸盐沉淀物中,这可能是通过两种主要机制实现的:(i) 微生物介导的还原和沉淀,以及 (ii) 硫代钼酸盐的形成和吸附/并入硫化铁。
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引用次数: 0
Recovery of Valuable Metals from Polymetallic Refractory Concentrate by a Sulfuric Acid Curing and Leaching Method 用硫酸固化和浸出法从多金属耐火精矿中回收贵金属
IF 2.6 4区 工程技术 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-23 DOI: 10.3390/separations11010007
Wei Jiang, Jilai Xue, Kaixi Jiang, Xunxiong Jiang, Shengdong Wang, Jinping Hu, Derek O Northwood, K. E. Waters, Hao Ma
Sulfuric acid curing and leaching is a promising technology for treating refractory ores. In this work, a refractory concentrate containing 3191 ppm uranium (U), 2135 ppm niobium (Nb), and 0.7% rare earth minerals (REMs) went through two stages: curing by high-concentration H2SO4 and leaching by low-concentration H2SO4. We investigated the behavior of those valuable metals during the two stages. For both curing and leaching, the operating parameters include the acid-to-solid ratio, time, temperature, and H2SO4 concentration. The recovery for U, Nb, and REMs was as high as 95%, 86%, and 73.5% using a curing acid-to-solid ratio of 1:1, curing temperature of 200 °C, curing time of 1 h, H2SO4 concentration of 98%, leaching liquid-to-solid ratio of 4:1, leaching time of 2 h, leaching temperature of 60 °C, and leaching H2SO4 concentration of 5 g/L. A “sulfuric acid curing–leaching-U extraction by N235–Nb recovery by resin adsorption–REMs’ recovery by resin adsorption” method was implemented, where the overall U, Nb, and REMs’ recovery reached 93.1%, 84.5%, and 69.6%, respectively.
硫酸固化和浸出是处理难熔矿石的一项前景广阔的技术。在这项研究中,含有 3191 ppm 铀(U)、2135 ppm 铌(Nb)和 0.7% 稀土矿物(REMs)的难选冶精矿经过了两个阶段:高浓度 H2SO4 固化和低浓度 H2SO4 沥滤。我们研究了这些有价金属在这两个阶段中的表现。固化和浸出的操作参数包括酸固比、时间、温度和 H2SO4 浓度。在固化酸固比为 1:1、固化温度为 200 °C、固化时间为 1 小时、H2SO4 浓度为 98%、浸出液固比为 4:1、浸出时间为 2 小时、浸出温度为 60 °C、浸出 H2SO4 浓度为 5 克/升的条件下,U、Nb 和 REM 的回收率分别高达 95%、86% 和 73.5%。采用 "硫酸固化-浸出-N235 萃取-树脂吸附铌回收-树脂吸附 REMs 回收 "的方法,铀、铌和 REMs 的总体回收率分别达到 93.1%、84.5% 和 69.6%。
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引用次数: 0
Structure Elucidation and Immunoactivity Study of Armillaria mellea Fruiting Body Polysaccharides 瓜子黄癣菌果体多糖的结构阐释和免疫活性研究
IF 2.6 4区 工程技术 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-20 DOI: 10.3390/separations11010003
Qingqing Li, Ying Li, Huazhou Niu, Enhui Wang, Lili Jiao, Hui Li, Wei Wu
Polysaccharides are the main nutritional constituents in the Armillaria mellea fruiting bodies. The structure and immunoactivity of Armillaria mellea polysaccharide are valuable to be determined for development. In the present study, two polysaccharides, including Armillaria mellea neutral polysaccharide (AMPN) and Armillaria mellea acidic polysaccharide (AMPA), were prepared and determined. AMPN and AMPA were separated and refined by the ion exchange column and gel chromatographycolumn. Analysis of AMPN and AMPA revealed molecular weights of 4.432 × 103 Da and 7.323 × 103 Da. The monosaccharide composition analysis revealed that AMPN was mainly composed of 68.3%glucose, while AMPA consisted primarily of glucose, mannose, and galactose, accompanied by 8.9% galacturonic acid and 3% fucose. Then, infrared spectra analysis, Congo red staining, methylation, and NMR spectroscopy analysis were conducted as a means to clarify the structure of AMPN and AMPA. The NMR spectra demonstrated that the two polysaccharides included both α and β-configuration glycosidic bonds. The Congo red experiment suggests that AMPN and AMPA all had obvious triple helix structures.The effects of AMPN and AMPA on immune repair ability were compared by immune deficiency mice. The activity experiment showed that AMPN and acidic polysaccharides extracted from the Armillaria fruiting body have biological immune activity. Among them, AMPA showed higher immune activity. These findings suggest that Armillaria mellea fruiting bodies may be used as a source of dietary supplements and functional products.
多糖是黑木耳子实体的主要营养成分。多糖的结构和免疫活性具有重要的开发价值。本研究制备并测定了两种多糖,包括中性多糖(AMPN)和酸性多糖(AMPA)。采用离子交换柱和凝胶色谱柱对AMPN和AMPA进行分离和精制。分析表明,AMPN 和 AMPA 的分子量分别为 4.432 × 103 Da 和 7.323 × 103 Da。单糖成分分析表明,AMPN 主要由 68.3% 的葡萄糖组成,而 AMPA 主要由葡萄糖、甘露糖和半乳糖组成,此外还有 8.9% 的半乳糖醛酸和 3% 的岩藻糖。然后,通过红外光谱分析、刚果红染色、甲基化和核磁共振光谱分析等手段,明确了 AMPN 和 AMPA 的结构。核磁共振光谱显示,这两种多糖都含有α和β构型的糖苷键。用免疫缺陷小鼠比较了 AMPN 和 AMPA 对免疫修复能力的影响。活性实验表明,AMPN和从阿米巴子实体中提取的酸性多糖具有生物免疫活性。其中,AMPA 的免疫活性更高。这些研究结果表明,益母草子实体可作为膳食补充剂和功能性产品的来源。
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引用次数: 0
Investigation of a Hydraulic Channel for Plastic Particles Sorting via Experimental and Numerical Tools 通过实验和数值工具研究用于塑料颗粒分拣的水力通道
IF 2.6 4区 工程技术 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-20 DOI: 10.3390/separations11010005
Monica Moroni
In recent decades, the versatility of fossil-based polymers has led them to become one of the most used materials for the production of several consumer goods. The destiny of post-consumer plastics is crucial for environmental sustainability. Two are the alternatives to landfilling: (i) energy recovery, i.e., replacement of traditional fuel with plastic litter, and (ii) recycling, i.e., processing of plastic wastes to produce secondary raw materials that may substitute primary raw materials. This work presents the investigation of a device for the hydraulic separation of heterogeneous plastic wastes, which, when properly upscaled, may be efficiently used within recycling plants. This apparatus is suitable for the separation of granules or flakes of plastics with a density higher than 1000 Kg/m3 and may replace existing technologies for mechanical recycling. The purpose of the device is to separate the useful fraction from a mixture of plastics and water introduced inside. The separation procedure efficacy relies on the difference in density, dimension, and shape of the processed plastic particles and on the flow features within the device. Experiments were carried out to test the efficacy of the device as a function of those factors. To increase the range of variation in the key parameters influencing the apparatus’s working principles, Computational Fluid Dynamics was employed to build a numerical model of the device. The validated numerical model suitable to fully characterize the apparatus performance features a hybrid grid with an inner mesh of 3·10−3 m size, a careful modeling of the near-wall region, and the k-ω SST turbulent model.
近几十年来,化石基聚合物的多功能性使其成为生产多种消费品的最常用材料之一。消费后塑料的命运对环境可持续性至关重要。垃圾填埋的替代方法有两种:(i) 能源回收,即用塑料垃圾替代传统燃料;(ii) 循环利用,即对塑料废物进行加工,生产可替代主要原材料的二次原材料。这项工作介绍了一种用于液压分离异质塑料废物的装置的研究,该装置经适当升级后,可在回收厂内有效使用。该装置适用于分离密度大于 1000 公斤/立方米的颗粒状或片状塑料,可替代现有的机械回收技术。该设备的目的是从塑料和水的混合物中分离出有用的部分。分离过程的效率取决于被处理塑料颗粒的密度、尺寸和形状差异,以及装置内的流动特征。我们进行了实验来测试该装置的功效与这些因素的关系。为了扩大影响设备工作原理的关键参数的变化范围,我们采用了计算流体动力学来建立设备的数值模型。经过验证的数值模型适用于全面鉴定该装置的性能,其特点是采用了内网格尺寸为 3-10-3 m 的混合网格,对近壁区进行了仔细建模,并采用了 k-ω SST 湍流模型。
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引用次数: 0
Separation and Biological Activities of the Main Compounds from the Bark of Myrica rubra Siebold & Zucc 从红叶木树皮中分离出的主要化合物及其生物活性
IF 2.6 4区 工程技术 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-20 DOI: 10.3390/separations11010004
Tianyang Hao, Lingyang Fan, Yiyue Chang, Hui Yang, Kai He
Myrica rubra (Lour.) Siebold & Zucc bark is a traditional natural medicine used by the people of the Dong minority in western Hunan in China. In this study, the main compounds in Myrica rubra bark including epigallocatechin gallate, myricetrin, myricetin, taraxerol, myricanol, and 11-O-acetylmyricanol were separated using both silica gel column chromatography and high-speed countercurrent chromatography (HSCCC). Notably, it is the first report of discovering 11-O-acetylmyricanol from Myrica rubra bark. The results of the bioactivity studies suggested that epigallocatechin gallate showed the highest α-glucosidase inhibitory activity, while myricetin exhibited the highest reactive oxygen species (ROS) scavenging ability in zebrafish embryos. Intriguingly, myricanol exhibited strong apoptosis-inducing activity on HepG2 cells, and further studies revealed that myricanol was capable of promoting the cleavage of caspase 3, 8, and 9, then resulting in the apoptosis in HepG2 cells. The findings of the present study have important implications for the separation of the main compounds in Myrica rubra and will provide credence to the ethnomedicinal application of the isolated compounds against cardiovascular disease and cancer.
红没药(Myrica rubra (Lour.) Siebold & Zucc)树皮是中国湘西侗族人民使用的一种传统天然药物。本研究采用硅胶柱色谱法和高速逆流色谱法(HSCCC)分离了红豆杉树皮中的主要化合物,包括表没食子儿茶素没食子酸酯、没食子素、没食子素、蒲公英萜醇、没食子醇和 11-O-乙酰基没食子醇。值得注意的是,这是首次从红豆杉树皮中发现 11-O-acetylmyricanol 的报道。生物活性研究结果表明,表没食子儿茶素没食子酸酯对α-葡萄糖苷酶具有最高的抑制活性,而没食子素对斑马鱼胚胎的活性氧(ROS)清除能力最强。耐人寻味的是,三十烷醇对 HepG2 细胞具有很强的凋亡诱导活性,进一步研究发现,三十烷醇能够促进 Caspase 3、8 和 9 的裂解,进而导致 HepG2 细胞凋亡。本研究的发现对分离红叶女贞中的主要化合物具有重要意义,并将为分离出的化合物在防治心血管疾病和癌症方面的民族医药应用提供依据。
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引用次数: 0
Momilactones and Phenolics in Brown Rice: Enrichment, Optimized Extraction, and Potential for Antioxidant and Anti-Diabetic Activities 糙米中的莫米内酯和酚类物质:富集、优化提取以及抗氧化和抗糖尿病活性的潜力
IF 2.6 4区 工程技术 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-20 DOI: 10.3390/separations11010006
Mehedi Hasan, L. Anh, T. Xuan
This is the first study aiming to enrich momilactones A (MA) and B (MB) and phenolic compounds in germinated brown rice (GBR) and non-GBR var. Koshihikari and Milky Queen through the cooking process. Extraction methods for these compounds were optimized by applying various conditions, including solvents (80% methanol and 80% ethanol), heat (80 °C), and sonication (2 h). Momilactone and phenolic quantities were determined by ultra-performance liquid chromatography–electrospray ionization mass spectrometry (UPLC–ESI-MS) and high-performance liquid chromatography (HPLC), respectively. Accordingly, cooked Koshihikari GBR extract using 80% methanol and sonication (GKB4) revealed the highest amounts of tricin, caffeic, ρ-hydroxybenzoic, ρ-coumaric, ferulic, salicylic, and cinnamic acids (1.71, 1.01, 0.62, 0.45, 0.94, 2.50, and 0.37 mg/g DW, respectively), consistent with the strongest antiradical activities in DPPH and ABTS assays (IC50 = 1.47 and 1.70 mg/mL, respectively). Non-cooked GBR Koshihikari extract using 80% ethanol and sonication (GKB9) exhibited the highest MA and MB contents (147.73 and 118.8 μg/g DW, respectively). Notably, GKB9 showed potent inhibition of α-amylase and α-glucosidase (IC50 = 0.48 and 0.15 mg/mL, respectively), compared with the anti-diabetic drug acarbose (IC50 = 0.26 and 2.48 mg/mL, respectively). The findings hold significant implications for developing phenolic- and momilactone-enriched brown rice with health-beneficial properties.
这是第一项旨在通过蒸煮过程富集发芽糙米(GBR)和非 GBR 变种越光糙米(Koshihikari)及牛奶皇后糙米(Milky Queen)中的莫米内酯 A(MA)和 B(MB)以及酚类化合物的研究。对这些化合物的提取方法进行了优化,采用了各种条件,包括溶剂(80% 甲醇和 80%乙醇)、加热(80 °C)和超声(2 小时)。超高效液相色谱-电喷雾质谱法(UPLC-ESI-MS)和高效液相色谱法(HPLC)分别测定了桃内酯和酚类物质的含量。结果表明,使用 80% 甲醇和超声波处理的越光 GBR 熟提取物(GKB4)中三酸、咖啡酸、ρ-羟基苯甲酸、ρ-香豆酸、阿魏酸、水杨酸和肉桂酸的含量最高(1.71、1.01、0.62、0.45、0.94、2.50 和 0.37 毫克/克 DW),这与 DPPH 和 ABTS 试验中最强的抗自由基活性(IC50 分别为 1.47 和 1.70 毫克/毫升)一致。使用 80% 乙醇和超声处理的非蒸煮 GBR 越光提取物(GKB9)显示出最高的 MA 和 MB 含量(分别为 147.73 和 118.8 μg/g DW)。值得注意的是,与抗糖尿病药物阿卡波糖(IC50 分别为 0.26 和 2.48 毫克/毫升)相比,GKB9 对α-淀粉酶和α-葡萄糖苷酶(IC50 = 0.48 和 0.15 毫克/毫升)有很强的抑制作用。这些发现对开发富含酚类和莫米内酯、有益健康的糙米具有重要意义。
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引用次数: 0
Effects of Hydrolysis Condition and Detection Method on the Monosaccharide Composition Analysis of Polysaccharides from Natural Sources 水解条件和检测方法对天然来源多糖单糖成分分析的影响
IF 2.6 4区 工程技术 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-19 DOI: 10.3390/separations11010002
Meijuan Zhao, Fengyan Kuang, Yingyue Zhang, Guang-Ping Lv
Monosaccharide composition analysis is essential to the structural characterization and research into the biological activity of polysaccharides. In this study, a systematic comparison was performed among commonly used monosaccharide composition analysis methods, including colorimetric and chromatographic methods. These were tested on 16 aldoses, ketoses, alditols, amino sugars, and uronic acids. Furthermore, the effect of hydrolysis methods was also investigated. The results showed that the phenol sulfuric acid method is greatly affected by the type of monosaccharide that is used as the reference substance. The determination of uronic acid using sulfuric acid carbazole is less affected by neutral sugars than that method using m-hydroxybiphenyl. The high-performance thin-layer chromatography (HPTLC) method can simultaneously analyze multiple samples and accurately determine the type of uronic acid. High-performance liquid chromatography (HPLC) can provide a good qualitative and quantitative analysis of aldose, amino sugars, and uronic acids, while gas chromatography–mass spectrometry (GC-MS) can detect aldose, ketose, and alditols. Fructose was detected in a large amount in inulin and Codonopsis pilosula after one-step hydrolysis, while it was totally destroyed in two-step hydrolysis. The release of galacturonic acid significantly increased after two-step hydrolysis in pectin and Lycium barbarum, which indicated that one-step hydrolysis is not enough for acidic polysaccharides. The results of this study are beneficial for selecting appropriate hydrolysis and analysis methods in order to accurately analyze the monosaccharide compositions of natural polysaccharides.
单糖成分分析对于多糖的结构表征和生物活性研究至关重要。本研究对常用的单糖成分分析方法(包括比色法和色谱法)进行了系统比较。对 16 种醛糖、酮糖、醛糖醇、氨基糖和尿酸进行了测试。此外,还研究了水解方法的影响。结果表明,酚硫酸法受用作参照物的单糖类型影响很大。与使用间羟基联苯的方法相比,使用硫酸咔唑法测定尿酸受中性糖类的影响较小。高效薄层色谱法(HPTLC)可同时分析多个样品,并准确测定尿酸的类型。高效液相色谱法(HPLC)可以很好地定性和定量分析醛糖、氨基糖和尿酸,气相色谱-质谱法(GC-MS)可以检测醛糖、酮糖和醛糖醇。一步水解法在菊粉和党参中检测到大量果糖,而两步水解法则完全破坏了果糖。果胶和枸杞经两步水解后,半乳糖醛酸的释放量明显增加,这表明一步水解对酸性多糖来说是不够的。本研究的结果有助于选择适当的水解和分析方法,以准确分析天然多糖的单糖成分。
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引用次数: 0
Nanomaterials for CO2 Capture from Gas Streams 从气体流中捕获二氧化碳的纳米材料
IF 2.6 4区 工程技术 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-19 DOI: 10.3390/separations11010001
Francisco José Alguacil
Since CO2 is an important component of gas emissions, its removal from gas streams is of the utmost importance to fulfill various environmental requirements. The technologies used to accomplish this removal are based mainly on absorption, as well as adsorption and membrane processing. Among the materials used in the above separation processes, materials in nano forms offer a potential alternative to other commonly used macromaterials. The present work reviews the most recent publications (2023) about CO2 capture using different nanomaterials, and whilst most of these publications were dedicated to investigating the above, several presented data on the separation of CO2 from other gases, namely nitrogen and methane. Furthermore, a number of publications investigated the recyclability of nanomaterials under continuous use, and just three of the references were about computational modeling; all others were experimental papers, and only one reference used a real industrial gas.
由于二氧化碳是气体排放的重要组成部分,因此从气体流中去除二氧化碳对满足各种环境要求至关重要。用于实现这种去除的技术主要基于吸收、吸附和膜处理。在上述分离过程中使用的材料中,纳米材料是其他常用大分子材料的潜在替代品。本研究综述了有关使用不同纳米材料捕获二氧化碳的最新出版物(2023 年),虽然这些出版物大多致力于研究上述问题,但也有一些出版物介绍了从其他气体(即氮气和甲烷)中分离二氧化碳的数据。此外,一些出版物还研究了纳米材料在连续使用情况下的可回收性,其中只有三篇参考文献涉及计算建模;其他均为实验论文,只有一篇参考文献使用了真实的工业气体。
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引用次数: 0
Breaking the Equilibrium and Improving the Yield of Schiff Base Reactions by Pervaporation: Application to a Reaction Involving n-butylamine and Benzaldehyde 通过渗透蒸发打破席夫碱反应的平衡并提高产率:正丁胺与苯甲醛反应的应用
IF 2.6 4区 工程技术 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-18 DOI: 10.3390/separations10120602
Rana Salem Al Khulaifi, Mohammed Mousa Alshehri, Inas Al-Qadsy, Mona A. Al Jufareen, Waseem. Saeed, A. Badjah-Hadj-Ahmed, Taieb Aouak
A comparative study of a Schiff base reaction involving benzaldehyde and n-butylamine was carried out to improve the yield of the resulting imine. This reaction was carried out at different temperatures without and with the elimination of the water produced during the process by the pervaporation (PV) technique using a typical cylindrical cell. To reach this goal, different dense membranes made of crosslinked poly(vinyl alcohol) with different oxalic acid (crosslinker) contents were prepared by the solvent casting method. Different parameters influencing the performance of the membrane in the separation process including swellability, diffusivity, crosslinking density, and thermal properties were investigated. The total and partial cumulative transmembranar fluxes as well as the separation factor were studied and the separation process was monitored by HPLC analysis. The n-butyl-1-phenylmethanimine produced was characterized by FTIR and 1HNMR analyses. The results obtained were a clear improvement in the yield of the reaction. For example, the yield obtained from the Schiff base reaction occurring without assistance by PV varied from 58 to 84 wt% when the temperature changed from 5 to 45 °C. On the other hand, when the PV process was used to eliminate water from this reaction mixture, the yield went from 90.4 to 98.6% by weight in this same temperature order. The cumulative total and partial fluxes significantly decreased with time. On the other hand, the separation factor reached a maximum at about one hour at 5, 15, and 45 °C. At 25 °C, the maximum total flux was reached at about 2 h of the PV process. The best selectivity of the PVA-0.5 membrane with regard to water was obtained at 15 °C. It was also revealed from the results obtained that the cumulative total and partial flux decreased rapidly with time and the separation factor reached a maximum at one hour into the PV process, in which 1.51 × 104 was reached at 15 °C, 6.25 × 103 and 3.50 × 103 at one hour of the separation process, and 10.23 × 103 at 25 °C at 2 h of the water removal by PV.
对涉及苯甲醛和正丁胺的希夫碱反应进行了比较研究,以提高所得亚胺的产率。该反应是在不同温度下进行的,使用了一个典型的圆柱形电池,在不使用或使用渗透蒸发(PV)技术去除反应过程中产生的水的情况下进行的。为实现这一目标,采用溶剂浇铸法制备了由不同草酸(交联剂)含量的交联聚(乙烯醇)制成的不同致密膜。研究了影响膜在分离过程中性能的不同参数,包括溶胀性、扩散性、交联密度和热性能。研究了总和部分累积跨膜通量以及分离因子,并通过高效液相色谱分析对分离过程进行了监测。傅立叶变换红外光谱和 1HNMR 分析对生成的正丁基-1-苯基甲亚胺进行了表征。结果表明,反应的产率明显提高。例如,当温度从 5 ℃ 升至 45 ℃ 时,在没有 PV 辅助的情况下发生的希夫碱反应的产率从 58% 到 84% 不等。另一方面,当使用 PV 工艺去除该反应混合物中的水分时,在相同的温度顺序下,产率从 90.4% 增加到 98.6%(重量百分比)。随着时间的推移,累积总通量和部分通量显著下降。另一方面,在 5、15 和 45 °C 下,分离因数在约一小时后达到最大值。在 25 °C,PV 过程约 2 小时后总通量达到最大值。PVA-0.5 膜对水的最佳选择性是在 15 °C 时获得的。研究结果还显示,随着时间的推移,累积总通量和部分通量迅速下降,分离因子在 PV 过程开始一小时后达到最大值,其中在 15 °C 时达到 1.51 × 104,在分离过程一小时后达到 6.25 × 103 和 3.50 × 103,在 25 °C 时达到 10.23 × 103,PV 除水过程进行了 2 小时。
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引用次数: 0
Compositional Analysis of Metal(IV) Phosphate and Phosphonate Materials—Pitfalls and Best Practices 金属(IV)磷酸盐和膦酸盐材料的成分分析--陷阱与最佳实践
IF 2.6 4区 工程技术 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-18 DOI: 10.3390/separations10120600
R. Koivula, Wenzhong Zhang
Metal(IV) phosphate and phosphonates materials have increasingly found their applications in water purification, heterogeneous catalysis, drug delivery, and proton-exchange membrane fuel cells. The strong linkage between tetravalent metal cations and phosphate/phosphonate groups offers a unique bottom-up design platform, resulting in chemically stable inorganics or hybrids. Task-specific physiochemical functionalities could be deposited by modifying the phosphate/phosphonate groups before the material synthesis. The high reactivity between the metal centre and the phosphorus-containing linker, on the other hand, often leads to obtaining unordered materials (amorphous solids or coordination polymers). The chemical composition of the prepared materials is a key parameter in guiding the synthetic approach and in governing their performances. This narrative review focuses on critically summarising the traditional and advanced analytical methods for probing the composition of these materials. The reader is introduced to and guided on the advances and restrictions of different analysis techniques when probing metal(IV) phosphates/phosphonates. Both solution-based and solid-state spectroscopic techniques are covered with a focus on understanding the quantity and the linkage status of the phosphorus-containing moieties. These techniques include atomic spectroscopy, mass spectroscopy, nuclear magnetic resonance spectroscopy, X-ray-based methods, and neutron activation analysis.
金属(IV)磷酸盐和膦酸盐材料越来越多地应用于水净化、异相催化、药物输送和质子交换膜燃料电池。四价金属阳离子与磷酸盐/膦酸盐基团之间的强联系提供了一个独特的自下而上的设计平台,从而产生了化学性质稳定的无机物或混合物。在材料合成之前,可以通过修改磷酸盐/膦酸盐基团来沉积特定任务的理化功能。另一方面,金属中心和含磷连接体之间的高反应性往往会导致获得无序材料(无定形固体或配位聚合物)。所制备材料的化学成分是指导合成方法及其性能的关键参数。这篇叙述性综述着重批判性地总结了探测这些材料成分的传统和先进分析方法。在探究金属(IV)磷酸盐/膦酸盐时,将向读者介绍并指导不同分析技术的进步和限制。本书涵盖了溶液光谱和固态光谱技术,重点是了解含磷分子的数量和连接状态。这些技术包括原子光谱、质谱、核磁共振光谱、基于 X 射线的方法和中子活化分析。
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引用次数: 0
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Separations
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