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Chinese Journal of Chemical Engineering 2024年第4期68卷 76-82页

作者： Shaoyun Wu Zhuang Ma Zichi Yang Suying Zhao Caijin Zhou Huidong Zheng Fujian Engineering Research Center of Advanced Manufacturing Technology for Fine Chemicals College of Chemical EngineeringFuzhou UniversityFuzhou 350108China Qingyuan Innovation Laboratory Quanzhou362114China

Micromixing efficiency is an important parameter for evaluating the multiphase mass transfer performance and reaction efficiency of microreactors.In this work,the novel curved capillary reactor with different shapes was designed to generate Dean flow,which was used to enhance the liquideliquid micromixing performance.The VillermauxeDushman probe reaction was employed to characterize the micromixing performance in different curved capillary microreactors.The effects of experiment parameters such as liquid flow rate,inner diameter,tube length,and curve diameter on micromixing performance were systematically investigated.Under the optimal conditions,the minimum value of the segmentation factor XS was 0.008.It was worth noting that at the low Reynolds number(Remicroreactor can significantly improve the micromixing performance with XS reduced by 37.5%.Further,the correlations of segment index XS with dimensionless factor such as Reynolds number or Dean number were developed,which can be used to predict the liquide liquid micromixing performance in capillary microreactors.

关键词： microreactor Process intensification Micromixing performance Dean flow

Two-step continuous flow process of sodium tanshinone ⅡA sulfonate using a 3D circular cyclone-type microreactor

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Chinese Chemical Letters 2024年第1期35卷 290-294页

作者： Maolin Sun Chaoming Liang Liming Cao Yaguo Wang Jiasheng Yang Shiyu Hou Wei Yu Yueyue Ma Ruihua Cheng Jinxing Ye School of Biomedical and Pharmaceutical Sciences Guangdong University of TechnologyGuangzhou 510006China School of Pharmacy East China University of Science and TechnologyShanghai 200237China School of Chemical Engineering East China University of Science and TechnologyShanghai 200237China Shanghai No.1 Biochemical&Pharmaceutical Co. Ltd.Shanghai 200080China

A sustainable and practical process is presented for the direct synthesis of sodium tanshinone IIA sulfonate(STS).Our approach was inspired by the well-established and industrially applied batch synthetic route for STS production.We constructed a telescoped two-step continuous flow platform.This involved a continuous tanshinone IIA sulfonation and in-line salt formation.For the setup,we constructed a 3D circular cyclone-type microreactor using femtosecond laser micromachining.Compared to the 68%yield for 2 h in batch,the two-step continuous flow had an STS yield of 90%,achieved for a total residence time of<3.0 min under optimal conditions.The proposed continuous flow method vastly simplified the operation and improved procedural safety,while significantly reducing the required acid content and wastewater production.

关键词： Continuous flow Sodium tanshinone IIA sulfonate Cardiovascular microreactor Green chemistry

Layer-by-layer fabrication of montmorillonite coating immobilizing Cu_(2)O nanoparticles for continuously catalyzing glycerol to dihydroxyacetone

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Chinese Journal of Chemical Engineering 2024年第4期68卷 263-275页

作者： Kejin Li Jiahui Liu Dajian Li Xiaolan Chen Chunhui Zhou Research Group for Advanced Materials&Sustainable Catalysis(AMSC) State Key Laboratory Breeding Base of Green Chemistry-Synthesis TechnologyCollege of Chemical EngineeringZhejiang University of TechnologyHangzhou 310032China Qing Yang Institute for Industrial Minerals Qingyang 242804China Engineering Research Center of Non-metallic Minerals of Zhejiang Province Zhejiang Institute of Geology and Mineral ResourcesHangzhou 310007China

microreactors are increasingly used for green and safe chemical processes owing to their benefits of superior mass and heat transfer,increased yield,safety,and simplicity of control.However,immobilizing catalysts in microreactors remains challenging.In this investigation,a technique for creating Cu_(2)O/montmorillonite catalyst coating,using electrostatic attraction for layer-by-layer self-assembly,was proposed.The montmorillonite film's morphology and thickness could be efficiently regulated by adjusting the degree of exfoliation and surface charge of montmorillonite,alongside layer-by-layer coating times.The Cu_(2)O nanoparticles were immobilized using the flow deposition approach.The resulting Cu_(2)O@montmorillonite-film-coated capillary microreactor successfully transformed glycerol into dihydroxyacetone.The conversion of glycerol and product selectivity could be controlled by adjusting the molar ratio of reactants,temperature,residence time,and Cu_(2)O loading.The maximum glycerol conversion observed was 47.6%,with a 27%selectivity toward dihydroxyacetone.The study presents a technique for immobilizing montmorillonite-based catalyst coatings in capillary tubing,which can serve as a foundation for the future application of microreactors in glycerol conversion.

关键词： microreactor Coating Montmorillonite Glycerol Cu_(2)O

Assessing mixing uniformity in microreactors via in-line spectroscopy

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Chinese Journal of Chemical Engineering 2024年第2期66卷 119-124页

作者： Shusaku Asano Shinji Kudo Taisuke Maki Yosuke Muranaka Kazuhiro Mae Jun-ichiro Hayashi Institute for Materials Chemistry and Engineering Kyushu UniversityKasuga 816-8580Japan Department of Chemical Engineering Graduate School of EngineeringKyoto UniversityJapan

Mixing behavior is critical for enhancing the selectivity of fast chemical reactions in microreactors.A high Reynolds number(Re)improves the mixing rate and selectivity of the reactions,but some exceptions of increasing side product yield with the higher Re have been reported.This study investigated the mixing uniformity in microreactors with in-line UV-vis spectroscopy to clarify the relationship between reaction selectivity and chaotic mixing with the higher Re.A colorization experiment of thymolphthalein in an acidic solution was conducted with an excess acid amount to the base to indicate a non-uniformly mixed region.Non-uniformity significantly increased with Re.At the same time,the degree of mixing,which was measured by a usual decolorization experiment,showed that the mixing rate increased with Re.The in-line analysis of the Villermaux-Dushman reaction during the mixing clarified that side product yield significantly increased with Re at around 300 and then decreased at around 1100.These results suggest the compensation effect between the mixing uniformity and mixing rate on the selectivity of the mixing-sensitive reactions.Faster mixing,characterized by a larger Re,can disturb mixing uniformity and,in some cases,decrease reaction selectivity.

关键词： microreactor Villermaux-Dushman reaction In-line analysis Mixing Mass transfer Uniformity

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Continuous-flow enzymatic synthesis of chiral lactones in a three-dimensional microfluidic reactor

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Chinese Chemical Letters 2024年第3期35卷 299-303页

作者： Xuelei Deng Meng Fan Miao Wu Xiaoyan Zhang Ya Cheng Jianye Xia Yingping Zhuang Weiping Zhu Xuhong Qian Yunpeng Bai State Key Laboratory of Bioreactor Engineering Shanghai Collaborative Innovation Center for BiomanufacturingEast China University of Science and TechnologyShanghai 200237China The Extreme Optoelectromechanics Laboratory School of Physics and Materials ScienceEast China Normal UniversityShanghai 200241China Tianjin Institute of Industrial Biotechnology Chinese Academy of SciencesTianjin 300308China

A new continuous-flow process for the enzymatic synthesis of optically pureγ-lactones,which are used as flavors and fragrances in the food and cosmetic industries,was developed in a three-dimensional microfluidic reactor.The microchannels(175 mm in length,0.9 mm in depth,and 1.72 mL in volume)were carved precisely inside a single borosilicate glass(90 mm×75 mm×12 mm)with ultrafast femtosecond laser micromachining.The flow field analysis and reaction simulation showed that the mixing of substrates and enzymes was enhanced,allowing the adjustment of residence time in a wide window.SmCR_(V4),a carbonyl reductase with excellent catalytic activity and enantioselectivity towardγ/δ-keto acids,was employed for the asymmetric synthesis of various chiral lactones.30 mmol/L(R)-γ-decalactone(3g)can be obtained in 26 s with a space-time yield(STY)up to 16,877 g L^(-1)d^(-1),which is 14.4 times higher than the highest STY of batch reaction reported previously.This continuous-flow process was applied to the synthesis of 6 chiral lactones.In addition,the scaled-up synthesis of 3g was carried out in 6 cascade microreactors continuously for 6 h,demonstrating the feasibility and stability of the 3D continuous-flow process in enzymatic synthesis of optically pure compounds.

关键词： Continuous-flow Flow chemistry microreactor Biocatalysis Carbonyl reductase Asymmetric reduction

Micro/nano flow chemistry by Beyond Limits Manufacturing

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Chinese Chemical Letters 2024年第5期35卷 3-12页

作者： Peiwen Liu Fang Zhao Jing Zhang Yunpeng Bai Jinxing Ye Bo Bao Xinggui Zhou Li Zhang Changlu Zhou Xinhai Yu Peng Zuo Jianye Xia Lian Cen Yangyang Yang Guoyue Shi Lin Xu Weiping Zhu Yufang Xu Xuhong Qian State Key Laboratory of Bioreactor Engineering Shanghai Key Laboratory of Chemical BiologySchool of PharmacyEast China University of Science and TechnologyShanghai 200237China State Key Laboratory of Chemical Engineering School of Chemical EngineeringEast China University of Science and TechnologyShanghai 200237China State Key Laboratory of Bioreactor Engineering Shanghai Collaborative Innovation Center for BiomanufacturingEast China University of Science and TechnologyShanghai 200237China School of Biomedical and Pharmaceutical Sciences Guangdong University of TechnologyGuangzhou 510006China School of Mechanical and Power Engineering East China University of Science and TechnologyShanghai 200237China Shanghai Key Laboratory of Green Chemistry and Chemical Processes Department of ChemistrySchool of Chemistry and Molecular EngineeringEast China Normal UniversityShanghai 200241China

In September 2018,we proposed the cutting-edge concept of“Beyond Limits Manufacturing”(BLM).BLM technology is based on the three-dimensional inner engraving or precise outer engraving of ultra-fast laser,to invent micro/nano scale flow chips or devices,which makes it possible for the microform,integration,economy,safety,high efficiency,green and intelligence of research,development and manufacturing process,so as to realize transformational manufacturing in the era of Industry 4.0.In this paper,we reviewed the representative results we made in the field of micro/nano flow chemistry during the implementation of the BLM major project(December 2019 to August 2023),and discussed its application prospects in micro/nano flow chemistry.

关键词： Beyond Limits Manufacturing Flow chemistry Pharmaceutical manufacturing microreactor

microreactor platform for continuous synthesis of electronic doped quantum dots

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Nano Research 2022年第10期15卷 9647-9653页

作者： Yuxi Li Yanbin Li Xinyuan Li Tailei Hou Chen Qiao Yunpeng Tai Xiaole Gu Di Zhao Le Sang Jiatao Zhang Beijing Key Laboratory of Construction Tailorable Advanced Functional Materials and Green Applications Key Laboratory of Medical Molecule Science and Pharmaceutics EngineeringMOE Key Laboratory of Cluster ScienceSchool of Chemistry and Chemical EngineeringBeijing Institute of TechnologyBeijing 100081China State Key Laboratory of Organic-Inorganic Composites Beijing University of Chemical TechnologyBeijing 100029China School of Chemistry and Chemical Engineering Beijing Institute of TechnologyBeijing 102488China

Electronic doped quantum dots(Ed-QDs),by heterovalent cations doping,have held promise for future device concepts in optoelectronic and spin-based technologies due to their broadband Stokes-shifted luminescence,enhanced electrical transport and tailored magnetic behavior.Considering their scale-up requirement and the low yielding of several current colloidal synthesis methods,a stable and efficient bulk synthesis strategy must be developed.microreactors have long been recognized as an effective platform for producing nanomaterials and fabricating large-scale structures.Here,we chose microreactor platform for continuous synthesis of Ed-QDs in the air at low temperatures.By original reverse cation exchange reaction mechanism together with varying the kinetic conditions of microreactor platform,such as liquid flow rate,the Ag doped CdS(CdS:Ag)Ed-QDs with higher yield have been synthesized successfully due to the continuous synthesis advantages with a high degree of size selectivity.Enabled by microreactor engineering simulation,this research not only provides a new synthetic method towards scale-up production but also enables to improve chemical mass production of similar functional QDs for optical devices,bioimaging and innovative information processing applications.

关键词： quantum dots microreactor continuous synthesis scale-up

An efficient microreactor with continuous serially connected micromixers for the synthesis of superparamagnetic magnetite nanoparticles

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中国化学工程学报:英文版 2023年第7期59卷 85-91页

作者： Wenting Fan Fang Zhao Ming Chen Jian Li Xuhong Guo State Key Laboratory of Chemical Engineering School of Chemical EngineeringEast China University of Science and TechnologyShanghai 200237China International Joint Research Center of Green Energy Chemical Engineering Shanghai 200237China

A new microreactor with continuous serially connected micromixers(CSCM)was tailored for the coprecipitation process to synthesize Fe_(3)O_(4) nanoparticles.Numerical simulation reveals that the two types of CSCM microchannels(V-typed and U-typed)proposed in this work exhibited markedly better mixing performances than the Zigzag and capillary microchannels due to the promotion of Dean vortices.Complete mixing was achieved in the V-typed microchannel in 2.7 s at an inlet Reynolds number of 27.Fe_(3)O_(4) nanoparticles synthesized in a planar glass microreactor with the V-typed microchannel,possessing an average size of 9.3 nm and exhibiting superparamagnetism,had obviously better dispersity and uniformity and higher crystallinity than those obtained in the capillary microreactor.The new CSCM microreactor developed in this work can act as a potent device to intensify the synthesis of similar inorganic nanoparticles via multistep chemical precipitation processes.

关键词： microreactor Continuous serially connected micromixers Mixing Nanoparticles

Continuous deacylation of amides in a high-temperature and high-pressure microreactor

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Frontiers of Chemical Science and Engineering 2022年第12期16卷 1818-1825页

作者： Pengcheng Zou Kai Wang Guangsheng Luo State Key Lab of Chemical Engineering Department of Chemical EngineeringTsinghua UniversityBeijing 100084China

The deacylation of amides,which is widely employed in the pharmaceutical industry,is not a fast reaction under normal conditions.To intensify this reaction,a high-temperature and high-pressure continuous microreaction technology was developed,whose space-time yield was 49.4 times that of traditional batch reactions.Using the deacylation of acetanilide as a model reaction,the effects of the temperature,pressure,reaction time,molar ratio of reactants,and water composition on acetanilide conversion were carefully studied.Based on the rapid heating and cooling capabilities,the kinetics of acetanilide deacylation at high temperatures were investigated to determine the orders of reactants and activation energy.This microreaction technology was further applied to a variety of other amides to understand the influence of substituents and steric hindrance on the deacylation reaction.

关键词： amide deacylation microreactor flow chemistry reaction intensification

Hydrogenation Behavior of Hydrogen Peroxide in a microreactor

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China Petroleum Processing & Petrochemical Technology 2022年第4期24卷 29-35页

作者： Zhu Hongwei Sun Bing Jin Yan Feng Junjie Zhao Chenyang Yan Junjie Jiang Jie Xu Wei SINOPEC Research Institute of Safety Engineering Co. Ltd.Qingdao 266071 State Key Laboratory of Heavy Oil Processing China University of Petroleum Qingdao 266580

The hydrogenation of hydrogen peroxide is an unwanted side reaction in the direct synthesis of hydrogen peroxide and remains a problem to solve.The mechanism of this reaction has been studied with batch reactors but the slow heat and mass transfer in batch reactors hindered the understanding of its intrinsic kinetics.In this study,a microreactor is employed to investigate the parameters that influence the hydrogenation reaction,including flow rate,channel length,hydrogen pressure,solvent composition,and initial hydrogen peroxide concentration.The activity of different catalysts was compared and the hydrogenation law was confirmed,providing guiding information to better control the hydrogenation process.

关键词： hydrogenation hydrogen peroxide microreactor hydrogenation decomposition law catalyst passivation