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FirePhysChem · 2023 · IF 0

Purity analysis and by-product separation of pentazole sodium

Xinyi Li,Yuangang Xu,Jianxin Zhou,Tianyang Hou,Ze Xu,Pengcheng Wang,Ming Lu

As an important intermediate in the synthesis of most energetic pentazole compounds, the reaction system of sodium pentazole is complex and has many by-products, but there is no suitable HPLC analysis method. Based on the study of ultraviolet absorption peak of sodium pentazole aqueous solution, the HPLC purity analysis method of sodium pentazole was successfully established and its sensitivity, accuracy and repeatability were verified. When the detection wavelength was 192 nm, the chromatographic column was Agilent WondaSil C18 Superb (4.6 × 250 mm, 5 μm), the mobile phase was 95% water and 5% acetonitrile mixed solution, the flow rate was 0.8 ml/min, the analysis time was 8 min, the sample size was 1 μL and the column temperature was 40 °C, a liquid phase map of sodium pentazole was obtained. The analysis results showed that the retention time of pentazole sodium was 3.76 min, and showed a good linear relationship in the range of 0.3068–0.3288 g/L. The linear equation is y = -217447.64+835837.85 x , the correlation coefficient R 2 is 0.99997, and it has good sensitivity, accuracy and repeatability. In addition, three by-products from the synthesis of sodium pentazole were simply separated.

研究领域: 分析化学 · 有机合成
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JOURNAL OF MOLECULAR CATALYSIS B-ENZYMATIC · 2013 · IF 2.823

Resolution of (R, S)-ethyl-2-(4-hydroxyphenoxy) propanoate using lyophilized mycelium of Aspergillus oryzae WZ007

Jian-Yong Zheng,Jia-Yu Wu,Yin-Jun Zhang,Zhao Wang

The mycelium of Aspergillus oryzae WZ007 was successfully developed to kinetic resolution of ( R , S )-ethyl-2-(4-hydroxyphenoxy) propanoate (( R , S )-EHPP) for production of ( R )-ethyl-2-(4-hydroxyphenoxy) propanoate (( R )-EHPP). The key biocatalytic process parameters (pH, temperature, rotation speed and substrate concentration) were optimized. Under the optimum conditions, the optical purity of ( R )-EHPP was improved up to >99% when the conversion was above 49%. A. oryzae WZ007 whole-cell lipase exhibited high reaction capacity, enantioselectivity and good reusability. The tolerable substrate concentration was 0.5   mol/L, and dry mycelium of A. oryzae WZ007 maintains over 80% of its initial activity after eight repeating cycles. Therefore the enzymatic preparation of ( R )-EHPP route was suitable for industrial application.

CAS / MDL: 123-31-9
研究领域: 生物化学 · 微生物学 · 制药工程
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FOOD CHEMISTRY · 2013 · IF 3.334

Separation of long chain fatty acids with different number of unsaturated bonds by fractional extraction: Experimental and COSMO-RS study

Huabin Xing,Xiao Zhang,Qiwei Yang,Ruiyang Liu,Zongbi Bao,Baogen Su,Yiwen Yang,Qilong Ren

Long chain unsaturated fatty acids (LCUFAs) are important food components and dietary supplements due to their beneficial health effects. The key process to produce high-purity LCUFAs is to separate long chain fatty acids (LCFAs) with different degrees of unsaturation and chain lengths. This process faces great challenge because of similar physico-chemical properties of fatty acids concerned. In this work, fractional extraction is proposed to separate LCFAs, using eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA), conjugated linoleic acids (CLAs), oleic acid (OA) and stearic acid (SA) as model LCFAs. COSMO-RS calculations were performed for fast extractant screening and exploring the potential separation mechanism. Satisfactory distribution coefficients and high selectivities were obtained in extraction equilibrium experiments. Simulation and experimental validation of fractional extraction were performed, and high purity and high yield of CLAs were obtained. EPA and DHA could be separated thoroughly from OA, though they could not be separated each other.

CAS / MDL: 112-80-1 9005-38-3
研究领域: 食品科学 · 生物化学
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Journal of Environmental Chemical Engineering · 2025 · IF 7.2

Preparation of high-purity hexagonal flaky magnesium hydroxide and high-purity magnesium oxide from seawater bittern

Furong Jia,Yun Li,Hongfei Guo,Xueqing Chen,Jilin Cao

Currently, comprehensive utilization technology of seawater bittern faces several challenges, including low resource utilization efficiency, limited value of magnesium salt products, and high energy consumption. This study proposes an innovative approach to prepare high-purity MgO. This process begins with the reaction of brine with a mixed alkaline solution of NaOH-Na 2 CO 3 to synthesize basic magnesium carbonate (4MgCO 3 ·Mg(OH) 2 ·4 H 2 O). Subsequently, 4MgCO 3 ·Mg(OH) 2 ·4 H 2 O is transformed into a high-purity Mg(OH) 2 structure through the hydrothermal conversion method. Finally, high-purity MgO is obtained by calcining magnesium hydroxide. The effects of mixed alkali precipitation and hydrothermal reaction conditions on the structure, morphology, and purity of intermediate products and MgO are systematically investigated. The optimal conditions for preparing high-purity MgO are determined as follows: the molar ratio of Mg 2 + :CO 3 2− :OH − in seawater bittern to the NaOH-Na 2 CO 3 mixed alkali is 5:4.7:2, at a reaction temperature of 60 °C, stirring speed of 200 rpm, stirring time of 10 min, and reaction time of 35 min. Under these conditions, spherical 4MgCO 3 ·Mg(OH) 2 ·4 H 2 O is initially obtained. Subsequently, the 4MgCO 3 ·Mg(OH) 2 ·4 H 2 O underwent hydrothermal treatment at a solid-to-liquid ratio of 8:100 and a temperature of 120 °C. Polyethylene glycol (PEG) is added as a surfactant at 3  wt % of the solid content of 4MgCO 3 ·Mg(OH) 2 ·4 H 2 O, along with 5 g of NaOH (accounting for 62.5  wt %), for 2 h. This process yielded high-purity Mg(OH) 2 with a thin flake morphology. Finally, the high-purity Mg(OH) 2 is calcined at 500 °C for 4 h, resulting in cubic crystal nano-MgO with a purity of 99.8 % and an average particle size of approximately 30 nm.

CAS / MDL: 25322-68-3
研究领域: 材料科学 · 化学工程 · 无机合成 · 纳米技术 · 资源利用
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CHINESE JOURNAL OF CHEMICAL ENGINEERING · 2025 · IF 3.7

Exosomes separation with aqueous two-phase systems from bovine milk

Jing-Jing Sun,Ruo-Que Mao,Xiao-Qian Fu,Shan-Jing Yao,Dong-Qiang Lin

The exosomes hold significant potential in disease diagnosis and therapeutic interventions. The objective of this study was to investigate the potential of aqueous two-phase systems (ATPSs) for the separation of bovine milk exosomes. The milk exosome partition behaviors and bovine milk separation were investigated, and the ATPSs and bovine milk whey addition was optimized. The optimal separation conditions were identified as 16% (mass) polyethylene glycol 4000, 10% (mass) dipotassium phosphate, and 1% (mass) enzymatic hydrolysis bovine milk whey. During the separation process, bovine milk exosomes were predominantly enriched in the interphase, while protein impurities were primarily found in the bottom phase. The process yielded bovine milk exosomes of 2.0×10 11 particles·ml −1 whey with high purity (staining rate>90%, 7.01×10 10 particles·mg −1 protein) and high uniformity (polydispersity index <0.03). The isolated exosomes were characterized and identified by transmission electron microscopy, zeta potential and size distribution. The results demonstrated aqueous two-phase extraction possesses a robust capability for the enrichment and separation of exosomes directly from bovine milk whey, presenting a novel approach for the large-scale isolation of exosomes.

CAS / MDL: 25322-68-3 7758-11-4
研究领域: 生物技术 · 医学工程
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ANALYTICAL CHEMISTRY · 2022 · IF 8.008

Less Configuration and More Dimensionality: Preparative Heart-Cut Multidimensional Liquid Chromatography Based on Trapping Arrays

Yulin Zhai,Guoli Li,Kai Peng,Zhaosong Ge,Weibing Zhang,Duxin Li

The resolving power of multiple dimensional liquid chromatography (mD-LC) is multiplicative as it adds dimensions. However, the issue in creating a preparative mD-LC system is that the higher the dimensionality, the more complicated the system configuration. Thus, we presented a new configuration of preparative mD-LC using one set of LC modules and trapping array-based multiple heart-cut interfaces. A preparative two-dimensional liquid chromatography (2D-LC) separation of herbal medicine formulation produced 40 compounds with a purity of >90%. During the separation process, the interface stores the fractions and allocates positions for the fractions from a different dimension; LC draws the fraction from the interface, makes nD separation, and sends isolated fractions to the interface. By repeating this process, we achieved variable dimensionality of LC separations. We also presented a preparative 3D-LC separation of herbal medicines to validate the principle of “less configuration and more dimensionality”. Thus, we can explore the higher dimensional preparative separations. The developed preparative mD-LC displayed exceptional power in the isolation of various compounds and has great potential in the application of natural products.

研究领域: 分析化学 · 天然产物化学
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JOURNAL OF FLUORESCENCE · 2025 · IF 3.1

Luminescence Investigation of Red Phosphors La3Ga5SnO14:Eu3+ with High Color Purity and Application in w-LEDs

Lei Yanhua,Zhang Anlin,Li Dongdong,Li Feng,Sun Huapeng,Deng Bin

A series of newly synthesized red-emitting phosphors, La 3 Ga 5 SnO 14 :Eu 3+ , were produced through high-temperature solid-state synthesis methods. The phase purity, particle morphology and optical properties were systematically investigated in this work. The prepared fluorescent material has high phase purity. La 3 Ga 5 SnO 14 :Eu 3+ has a strong red emission peak at 612 nm at the excitation at 268 nm, which is caused by the radiative transitions of electrons ( 5 D 0 → 7 F 2 ). The optimal doping concentration of Eu 3+ was observed to be 30 mol% in this series of La 3 Ga 5 SnO 14 :Eu 3+ . The mechanism of concentration quenching was determined to be dipole-quadrupole interaction. The chromaticity coordinates of La 3 Ga 5 SnO 14 :30 mol%Eu 3+ were (0.648, 0.352) with a corresponding high color purity of 100%. The thermal stability of the phosphor was also characterized. The luminous intensity could be sustained at 54% at 480 K. The quantum efficiency of the La 3 Ga 5 SnO 14 :30 mol%Eu 3+ phosphor is 64.4%. The exhaustive findings from this study form the basis for advocating the application of these phosphors in light-emitting devices.

研究领域: 材料科学 · 光学
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BIOTECHNOLOGY LETTERS · 2019 ·Vol. 41 ·期 6 ·789-799 · IF 2.154

Biocatalytic synthesis and characterization of sn-1/3 and sn-2 monoacylglycerols

Wang Xiuwen,Cheng Yang,Jin Qingzhe,Wei Wei,Wang Xingguo

Objectives To investigate the lipase-catalyzed synthesis of high purity sn -1/3 and sn -2 monoacylglycerols (1/3-MAG and 2-MAG) of different fatty acids (FAs). Results The 1/3-MAGs of three FAs (16:0, 17:0, 16:1) were synthesized using lipase-catalyzed esterification of glycerol with FAs. The 2-MAGs were obtained from the ethanolysis of synthetic triacylglycerols using sn -1,3 regiospecific lipase. The effects of lipase types, substrate ratio, temperature, reaction time and lipase load on the MAG conversion were studied. Under the optimal conditions, high purities (96.74%, 95.44%, 92.96%) with acceptable isolated yields (51.00%, 54.28%, 46.00%) were obtained for 1/3-16:0-MAG, 1/3-17:0-MAG, and 1/3-16:1-MAG, respectively. For 2-16:0-MAG, 2-17:0-MAG, and 2-16:1-MAG, the purities were 92.64, 95.04, and 96.48%, with isolated yields of 50.64, 52.16, and 26.12%, respectively. The molecular structures of the synthetic compounds were confirmed by 1 H NMR, and MS and the melting points were characterized by DSC. Conclusions High purity MAG isomers can be synthesized via lipase-catalyzed reactions to be building blocks for production of functional lipids, the melting points of which are largely governed by the hydrophobic interactions among the alkanyl chains.

CAS / MDL: 506-12-7 75-65-0
研究领域: 食品科学 · 生物化学
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CERAMICS INTERNATIONAL · 2024 · IF 5.1

Low-temperature synthesis and properties of high-purity boron nitride microspheres

Yiang Du,Chong Wang,Wenjun Liu,Tuo Yan,Jiaxuan Li,Bing Wang,Yingde Wang

Boron nitride (BN) has excellent high temperature resistance, thermal conductivity , strong insulation, and wave-transparent properties. Spherical BN is an essential filler in polymer matrix composites due to good particle mobility and high filler content. In this paper, we present a large-scale preparation for BN microspheres with uniform particle size distribution in the range of 1.0–2.8 μm via solvothermal method at low cost and high yield (∼90%), which is two orders of magnitude lower than the diameter of the spherical BN prepared by other methods. BN microspheres can achieve good crystallinity (>70%) and high purity (>99.9%) at 800 °C. The temperature resistance study showed that the BN microspheres could maintain the dense particle morphology at 1200 °C. In addition, the prepared BN microspheres have good dielectric and thermal conductivity properties (dielectric constant ∼3.4, dielectric loss ∼2.0 × 10 −3 , and thermal conductivity of 9.8 W m −1  K −1 ), which show great potential in the field of wave-transparent and thermal conductive composites. The synthesis process of BN microspheres proposed in this study provides a new idea for the preparation of ceramic micro or nano materials by polymer-derived ceramics.

研究领域: 材料科学 · 陶瓷材料
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JOURNAL OF HAZARDOUS MATERIALS · 2024 · IF 12.2

Deep removal of trace arsenic from acidic SbCl3 solution by in-situ galvanically coupled Cu2Sb/Cu particles

Junfeng Kong,Huazhen Cao,Weilun Qian,Lining Yu,Anyang Tang,Wenyu Feng,Huibin Zhang,Guoqu Zheng

Arsenic is a harmful associated element in antimony ore, which might bring out the risk of leakage during complex industrial production of high-purity antimony. Herein, we reported a novel and efficient way to remove the trace arsenic impurity from acidic SbCl 3 solution by utilizing copper-system bimetallic particles. Specifically, galvanically coupled Cu 2 Sb/Cu was in-situ synthesized by introducing precursor copper powder to the specific SbCl 3 solution. DFT studies revealed that Sb(III) was easily reduced by Cu to form Cu 2 Sb due to the strong adsorption of Sb(III) on Cu (111) crystal plane. The Cu 2 Sb/Cu coupling exhibited excellent activity for As(III) reduction, over 99.4% arsenic were removed under optimal conditions and residual arsenic concentration dropped to only 2.7 mg L −1 . Crucially, Sb(III) concentration changes could be neglected. Besides, the dearsenization residues were extensively characterized to analyze the evolvement and cause in the reaction process. The results confirmed that the arsenic removal mechanisms by Cu 2 Sb/Cu particles were multi-affected, including adsorption, displacement, and precipitation. And the strong electrostatic attraction of AsO + under high HCl conditions was identified as a key step to achieving dearsenization. This research will provide a theoretical guidance for the green synthesis of high-purity antimony and related products.

CAS / MDL: 10025-91-9 7647-01-0
研究领域: 冶金学 · 环境科学 · 材料科学
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Journal of Materials Chemistry A · 2022 ·Vol. 10 ·期 13 ·7300-7313 · IF 14.511

Fabricating Ga doped and MgO embedded nanomaterials for sorption-enhanced steam reforming of methanol

Zhao Sun,Junpeng Liu,Rongjun Zhang,Yu Wu,Hongwei Li,Sam Toan,Zhiqiang Sun

Sorption-enhanced steam reforming of methanol (SE-SRM) is a promising approach to creating a high-purity hydrogen supply. However, catalysts suffer from activity deactivation and low CO2 uptake capacity. In this study, we investigate the role of Ga doping of Cu–MgO in SE-SRM by synthesizing a series of MgO embedded xGaCuMg catalytic sorbents via a sol–gel method. The TEM-EDX mapping results indicate that MgO nanoparticles can be successfully embedded in the bulk-phase of the catalytic sorbent with a stabilized microstructure. The results from in situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) reveal that the Ga-doped catalytic sorbent is conducive to promoting the conversion of C-containing intermediates in SE-SRM, and absorbing CO2 in the form of bidentate carbonate rather than monodentate carbonate. Experimental studies verify that the best uptake capacity of 18GaCuMg catalytic sorbent (36.25 mg CO2/g MgO) achieves almost complete conversion of methanol (99.70%) with 100% H2 selectivity at 200 °C. Specifically, no CO is formed during the kinetic-control stage of SE-SRM. Density functional theory (DFT) calculations based on the Cu(111)Ga2O3(202)MgO(200) model revealed that the Ga doping can enhance the adsorption energies of methanol and carbon dioxide, promoting methanol activation and increasing CO2 uptake capacity. These findings provide valid strategies for functionalized nanomaterial design, which will substantially promote the SE-SRMR performance with desired catalytic sorbent recyclability.

研究领域: 材料科学 · 催化化学 · 能源工程
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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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