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JOURNAL OF CHEMICAL ENGINEERING OF JAPAN · 2018 ·Vol. 51 ·期 6 ·524-529 · IF 0.635

Optimization Synthesis of Morphologically Homogeneous and Rod-Like Structure Barium Trinitroresorcinate Produced by Segmented Flow

Shuangfei Zhao,Nan Zhou,Peng Zhu,Huanming Xia,Yong Yang,Ruiqi Shen,Yinghua Ye

BaTNR (barium trinitroresorcinate) particles were first synthesized through a segmented flow synthesis method. The optimal synthesis conditions of barium trinitroresorcinate (BaTNR) were obtained by orthogonal experimental design using segmented flow technology. The optimal synthesis conditions are composed of barium nitrate solution with a pH value of 5.5 and molar concentration of 0.20 mol·L−1, magnesium styphnate solution with a pH value of 4.5 and molar concentration of 0.15 mol·L−1, and reaction temperature of 65°C. The optimized batch conditions were compared with segmented flow arrangements through a reproducibility experiment, which indicates that BaTNR synthesized by segmented flow is superior to a conventional technique in terms of crystal morphology, uniformity and yield. In addition, the possibility of continuous and safe synthesis of BaTNR using micro-segmented flow technology is introduced.

CAS / MDL: 629-59-4
研究领域: 化学工程 · 材料科学 · 纳米技术
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PROPELLANTS EXPLOSIVES PYROTECHNICS · 2017 ·Vol. 43 ·期 3 ·286-293 · IF 1.908

Micro-Segmented Flow Technology Applied for Synthesis and Shape Control of Lead Styphnate Micro-Particles

Shuangfei Zhao,Fanyuhui Yan,Peng Zhu,Yong Yang,Huanming Xia,Ruiqi Shen,Yinghua Ye

In this study, the technology of micro-segmented flow was applied for continuous synthesis safely and shape control accurately to lead trinitroresorcinate (LTNR) particles. Besides, a micro chemical reaction and crystallization system were built. Crystal shape control technology of LTNR and micro-segmented flow technology were first combined using the system. Additionally, the effects of the flowing rate and chemical additives on LTNR micro-particles preparation were researched for shape control. The LTNR micro-particles were analyzed by XRD, DSC, laser scanning confocal microscope and laser particle size analyzer. The results shows that the LTNR particles size can be controlled from 20 to 400 μm by the flow rate and the concentration of hexadecyl trimethyl ammonium bromide (CTAB), while the shape of LTNR can be controlled by the concentration of glycerol and CTAB. Besides, there is a good linear relationship between the size and the activation energy. This illustrates that the LTNR particles with smaller size are more stable and have higher heat release. This study demonstrated the power of micro-segmented flow for generation of LTNR micro-particles with high quality and for tuning of particle properties.

CAS / MDL: 629-59-4
研究领域: 化学工程 · 材料科学
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CHEMICAL ENGINEERING JOURNAL · 2021 · IF 13.273

Tuning the gas-liquid-solid segmented flow for enhanced heterogeneous photosynthesis of Azo- compounds

Yuhang Chen,Yaheng Zhang,Hongwei Zou,Minglei Li,Gang Wang,Min Peng,Jie Zhang,Zhiyong Tang

Difficult handling the solid catalysts remains one of the pain points in the continuous flow photochemistry. In this work, the gas–liquid-solid segmented flow was employed in the photocatalytic production of azo- compounds (azoxybenzene and azobenzene) from nitrobenzene using graphitic carbon nitride (g-C 3 N 4 ) as solid catalyst. Compared with the batch reactor, the photocatalytic reaction rate was greatly improved in the microreactor, and the reaction time was shortened from 180 min of the batch to 7.5 min for near-full conversion of nitrobenzene. The effects of various reaction parameters (temperature, light source power, catalyst content) in the continuous system were examined, and the reaction kinetic was found in first order. The photocatalytic reaction performance was very sensitive to the gas–liquid-solid segmented flow conditions, which needed to be carefully tuned. With the help of high-speed camera and micro particle image velocimetry (µ-PIV) techniques, it was identified that the increasing inert gas fraction resulted in more stable segmented flow with shorter liquid segments, favoring the reaction rate. With a high gas fraction, the intensity of recirculation in the liquid segments was strengthened by the increasing total flow rate, enhancing the local mass transfer, thereby benefiting the photocatalytic reaction. Overall, the continuous microreactor reached 5.6 times higher productivity per volume (26.1 mmol/h*L) of azo- compounds than the batch reactor under the same conditions. The successful photosynthesis of azo- compounds demonstrated the great potential of the presented gas–liquid-solid segmented flow, and the findings of this work provide useful guidance on its future application in other heterogeneously catalyzed reactions.

研究领域: 化学工程 · 环境科学 · 材料科学
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PROPELLANTS EXPLOSIVES PYROTECHNICS · 2016 ·Vol. 41 ·期 5 ·899-905 · IF 1.578

Microfluidic Synthesis of Size-Controlled and Morphologically Homogeneous Lead Trinitroresorcinate Produced by Segmented Flow

Nan Zhou,Peng Zhu,Yi Rong,Huanming Xia,Ruiqi Shen,Yinghua Ye,Shenglin Lv

Size-controlled and morphologically homogeneous lead trinitroresorcinate (LTNR) particles were synthesized in aqueous solutions using segmented flow. The experimental setup consisted of syringe pumps connected with silicone tubing to a segmented flow microfluidic platform made of polymethyl methacrylate (PMMA) containing silicone-based microchannels immersed in a thermostatted bath. As a starting point for the optimization of the experimental conditions, LTNR particles were first synthesized through conventional batch synthesis. The optimized batch conditions were adapted to segmented flow arrangements. Characterization studies on LTNR formed through batch and segmented flow methods were carried out, and it was found that in the latter LTNR particles exhibited superior particle morphology and narrower particle size distribution. In addition, the heat release of LTNR prepared by segmented flow increased by 353.52 J g −1 in comparison to that formed through batch synthesis. Finally, it was found demonstrated that segmented flow methods result in a 13 % increase in yield for the synthesis of LTNR. This study demonstrated the feasibility of synthesising primary explosives using a segmented flow microfluidic platform.

CAS / MDL: 629-59-4
研究领域: 化学工程 · 材料科学 · 炸药科学
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TALANTA · 2025 · IF 6.1

Inter-droplet gas diffusion in segmented-flow analysis for ammonium determination

Xiaodi Yan,Yiyu Jiang,Jin Zhang,Xuejia Chen,Wenshan Liang,Hui Zeng,Min Zhang

Gas diffusion enables ammonium determination by converting it to ammonia gas under alkaline conditions. Ammonia is typically transferred across membranes or air gaps and absorbed by an acceptor phase, inducing measurable changes. This study presents a novel donor-oil-acceptor system for ammonium determination. Immiscible fluorinated oils, such as FC-40, which dissolve ammonia, are used to efficiently segment donor and acceptor droplets within a single flow stream. These oils act as liquid membranes, facilitating ammonia transfer from the donor phase to the acceptor phase through both diffusion and inner droplet circulation. An automated flow-through analyzer, incorporating peristaltic micro-pumps, was developed to generate multiple paired donor-acceptor droplets, enabling concurrent gas diffusion and enhancing sample throughput. Bromothymol blue (BTB) was used as a pH indicator for absorbance-based detection, while o-phthalaldehyde (OPA)-sulfite reagent served as a selective reagent for fluorescence-based detection. The limits of detection were determined to be 14 μmol L -1 for the absorbance method and 2 μmol L -1 for the fluorescence method. Interference studies revealed that precipitation from alkaline earth metals had minimal effect on recovery, while amines exhibited significantly higher transfer efficiency through the oil phase. To address this, the OPA-sulfite reagent in the acceptor phase effectively mitigated interference from amines. The proposed droplet-based system provides an innovative and versatile platform for analyzing volatile compounds in complex sample matrices.

研究领域: 分析化学 · 流动分析 · 微流控技术 · 环境分析 · 化学传感器
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