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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

continuous-flow synthesis and crystal modification of Pigment Red 53

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中国化学快报:英文版 2023年第8期34卷 153-157页

作者： Yuxin Mao Changlu Zhou Chaoying Wang Zhong Xin Shanghai Key Laboratory of Multiphase Materials Chemical Engineering School of Chemical EngineeringEast China University of Science and TechnologyShanghai 200237China State Key Laboratory of Chemical Engineering School of Chemical EngineeringEast China University of Science and TechnologyShanghai 200237China

In this study,a continuous-flow procedure containing four steps has been developed to synthesize Pigment Red 53 and modify its crystal structure.This process avoided the problems of conveying highly insoluble reaction intermediates by removing intermediate operating steps.After optimization,the overall yield of Pigment Red 53:1 reached 97.1%in the total residence time of 80 s by this diazotizationcoupling-laking-crystal transition process.From batch to continuous flow,the purity of products increased from 97.1%to 98.2%and the median diameter of pigment particles decreased from 14μm to 1.9μm.This process achieved a similar crystal transition effect in 18 s as in batch,producingα,δandνcrystals of Pigment Red 53:2 as expected.In conclusion,this continuous-flow procedure displays advantages in both synthesis and crystal transition,indicating another potential use for industrial application.

关键词： C.I.Pigment Red 53 continuous synthesis Process optimization Crystal modification

continuous synthesis for zirconium metal-organic frameworks with high quality and productivity via microdroplet flow reaction

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Chinese Chemical Letters 2018年第6期29卷 849-853页

作者： Ying Wang Liangjun Li Liting Yan Lei Cao Pengcheng Dai Xin Gu Xuebo Zhao Research Center of New Energy Science and Technology Research Institute of Unconventional Oil & Gas and Renewable Energy China University of Petroleum (East China) College of Science China University of Petroleum (East China)

Zirconium metal-organic frameworks（Zr-MOFs） represent the most promising candidates among MOFs for industrial utilizations owing to their high porosity and excellent stability. However, the efficient synthesis of Zr-MOFs combining with continuous production, high productivity and good product quality still remains a critical issue for practical applications. Herein, we report an efficient method of synthesizing a series of Zr-MOFs through a microdroplet flow reaction, which is more accommodate the requirements of industrial production. Four types of Zr-based MOFs with different ligands and topologies（MOF-801, MOF-804, DUT-67 and MOF-808） were produced as a pure phase of high quality crystalline with uniform morphologies. Furthermore, this series of Zr-MOFs were obtained in a continuous way and at a space-time yield（STY） highly up to 367.2 kg m-3 d-1. These MOFs exhibit the similar pore structure and thermal stability with that prepared from conventional solvothermal synthesis. CO2 sorption studies on these MOFs demonstrate that the hydroxyl groups on ligand can render MOFs with high CO2/N2 selectivity.

关键词： Zirconium metal-organic frameworks Microdroplet flow reaction continuous synthesis Space-time yield CO2 adsorption

High-efficiency and safe synthesis of tonalid via two Friedel-Crafts reactions in continuous-flow microreactors

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Chinese Journal of Chemical Engineering 2022年第12期52卷 126-135页

作者： Yang Han Yuanyuan Liu Shiwei Wang Xuehui Ge Xiaoda Wang Ting Qiu Engineering Research Center of Reactive Distillation Fujian Province Higher Education InstitutesCollege of Chemical EngineeringFuzhou UniversityFuzhou 350108China Qingyuan Innovation Laboratory Quanzhou 362801China

Tonalid,an important fragrance ingredient with widespread applicatio n,was synthesized via two FriedelCrafts reactions,which were catalyzed by AlCl_(3).The traditional tonalid production was conducted in batch stirring tank reactors,suffering from low production capacity and the safety hazard of temperature runaway.To solve these problems,the continuous-flow technologies were developed for the highefficiency and intrinsically safe synthesis of tonalid in microreactors.Catalyst AlCl_(3)was neatly homogenized in proper solvents by forming complex with reactant,which was a necessary step for the continuous synthesis in microreactors.Several reaction conditions,including reactant molar ratio,catalyst concentration,temperature,and microchannel hydrodynamic diameter,were investigated for the two Friedel-Crafts reactions in micro reactors.At optimized conditions,the yields of the two Friedel-Crafts reactions were 44.15%and 97.55%,respectively.In comparison with the batch reactors,the reaction times of these two reactions could both be reduced by nearly two thirds in microreactors at the similar yield.

关键词： Microreactor continuous synthesis Process intensification Tonalid Friedel-Crafts reaction

continuous, homogeneous and rapid synthesis of 4-bromo-3-methylanisole in a modular microreaction system

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Chinese Journal of Chemical Engineering 2020年第8期28卷 2092-2098页

作者： Pei Xie Kai Wang Jian Deng Guangsheng Luo The State Key Laboratory of Chemical Engineering Department of Chemical EngineeringTsinghua UniversityBeijing 100084China

4-Bromo-3-methylanisole is mainly used to synthesize black fluorane dye(2-anilino-3-methyl-6-dibutylaminofluorane, ODB-2), which is one of the most important heat and pressure-sensitive dyes in the manufacture of thermal papers. Compared to the industrial heterogeneous batch process, a continuous homogeneous bromination technology in a modular microreaction system has been developed, and 4-bromo-3-methylanisole has been successfully prepared through high-selective mono-bromination of 3-methylanisole with Br2 solution in CHCl3. In optimal conditions, the content of bis-brominated byproducts can be controlled less than 0.5%,which is superior to the industrial standard with 99.5% 3-methylanisole conversion at very short residence time and mild reaction temperature.

关键词： 4-bromo-3-methylanisole bromination continuous synthesis modular microreaction system mixing enhancement

A safe and efficient process for the preparation of difluoromethane in continuous flow

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Chinese Journal of Chemical Engineering 2020年第7期28卷 1860-1865页

作者： Tao Shen Xin Ge Hengjun Zhao Zhixiong Xu Shaofeng Tong Shaodong Zhou Chao Qian Xinzhi Chen College of Chemical and Biological Engineering Zhejiang UniversityZhejiang Provincial Key Laboratory of Advanced Chemical Engineering Manufacture TechnologyHangzhou 310027China School of Chemical and Material Engineering Jiangnan UniversityWuxi 214122China Jiangsu Sanmei Chemical Co. Ltd.Nantong 226461China

Difluoromethane is typically produced vialiquid-phase fluorination as performed in a batch reactor.However,this process suffers from some problems,e.g.,severe corrosion of the reactor,high safety risk,and the regeneration of the catalyst.In this paper,a flow process as performed in the tubular reactor was designed.The optimum conditions for continuous synthesis of difluoromethane were obtained as follows:the reaction temperature was 100℃,the molar ratio of dichloromethane to hydrogen fluoride was 1.6:1 and the reaction time was 300 s.The operation of the cyclic process was stable for 24 h with the conversion per pass of hydrogen fluoride up to 16.2%.The unreacted raw materials were easily reused.The deactivation of the common catalyst,antimony pentachloride,was investigated by catalyst concentration curve and XPS analysis.The approach proposed in this work is proven to be safe,efficient and low amount of catalyst.

关键词： Tubular reactor continuous synthesis Difluoromethane Catalyst