微通道反应器连续法合成硝酸异辛酯

以硝硫混酸作为硝化剂,与异辛醇在微通道反应器中经硝化反应得到硝酸异辛酯。考察了反应温度、混酸配比、硝酸浓度、停留时间、反应物配比对产品收率的影响,优化出微通道反应器中合成硝酸异辛酯的适宜工艺条件,硝酸异辛酯的收率97.8%,纯度达99.5%。微通道反应器连续法合成硝酸异辛酯具有操作简单、反应时间短、收率高、安全可靠等优点,具有工业化应用前景。     

大连化学物理研究所科研成果介绍微反应技术硝化合成硝酸异辛酯

正电话:0411-84379031传真:0411-84379327Email:gwchen@dicp.ac.cn学科领域:精细化工项目阶段:中试放大项目简介及应用领域异辛醇混酸硝化生产的硝酸异辛酯作为柴油十六烷值改进剂,对柴油油品升级起着重要作用。按典型的0.1%的添加量计,每万吨硝酸异辛酯可以调和1000万吨符合国V排放标准的优质柴油。随着油品的升级换代,硝酸异辛酯产品的市场需求量势必增加。由于硝酸异辛酯生产比较危险,技术主要由法国SNPE、瑞士BIAZZI等少数军工企业掌握。国内,西安万德能源化学公司采用微管式生产工艺,每年产能为1万吨,但数十条线并行生产工艺弊端明显。本项目采用微通道反应器技术,在反应热力学和反应动力学研究结果的基础上,创新性开发了微反应技术硝化合成硝酸异辛酯工艺,该工艺的主要特点是:异辛醇和混酸在并行多通道微混合器中接触反应,混合器内体积微小、物料混合均匀,反应时间短,传热速率快,产物和酸可实现连续自动分离。技术指标包括:原料转化率高于99.9%,产品纯度高于99.5%,水分小于0.05%,酸度小于3mg KOH/100ml。本项目同时揭示了反应过程中的爆炸机制,因而这项技术具有无可比拟的先进     

微反应技术合成不敏感硝酸酯增塑剂TMETN和PGDN

利用微反应技术,分别以1,2-丙二醇、三羟甲基乙烷为原料,硝硫混酸为硝化剂,合成了1,2-丙二醇二硝酸酯(PGDN)和三羟甲基乙烷三硝酸酯(TMETN);采用红外光谱、核磁共振等对其结构进行了表征,同时优化了微反应器硝化反应条件。结果表明,TMETN和PGDN结构与间歇式合成产物一致,合成TMETN的较佳硝化温度为17~20℃,硝酸与三羟甲基乙烷的最佳摩尔比为5.6∶1.0,收率达90.0%以上,纯度达98.5%;合成PGDN的较佳反应温度为20~22℃,硝酸与1,2-丙二醇的摩尔比为2.7∶1.0。该工艺具有反应温度范围宽、硝酸用量少和收率高等优点。     

陶瓷基微反应器制备的研究进展

微反应器中亚毫米级的流体通道具有高效的传质传热效应,使其能够强化反应过程。随着微细加工技术的发展,制备出了耐高温耐腐蚀的陶瓷基微反应器,适用于更严苛的反应条件,然而陶瓷基微反应器的制备存在微结构成型工艺复杂、密封难度较大等问题。本文主要介绍不同陶瓷材料微反应器的制备工艺,重点论述陶瓷基微反应器制备过程中常规微加工技术的优化和新型微加工技术的引入,对比这些技术对微结构成型的改善效果。列举常用的陶瓷微通道密封连接方法,概述其特点和适用范围。并提出在陶瓷基微反应器制备的后续研究过程中,应注重陶瓷基微反应器制备的成功率和新技术的开发,完善陶瓷基微反应器的性能,将陶瓷基微反应器引入到更广泛的应用体系中。     

间硝基苯乙酮在微通道反应器中的连续流合成研究

在碳化硅材质微通道反应器中,以苯乙酮为原料、硝酸为硝化剂、浓硫酸为溶剂合成间硝基苯乙酮。考察反应物料摩尔比、混酸摩尔比、反应温度、反应停留时间等工艺参数对反应的影响并对其进行优化。结果表明,当n(苯乙酮)∶n(硝酸)∶n(硫酸)=1∶1.5∶2、反应体系温度为10℃、停留时间为110 s时,反应效果最佳。该工艺充分利用了微通道反应器优良的传质传热特点,有利于对反应的精确控制和降低能耗,并减少副反应的发生。     

微反应器在化工行业中的应用

微反应器工艺技术应用在化工行业中是未来的—个重要发展趋势,微流体技术的出现为化工工艺的发展提供了策略。微反应器同普通的反应器相比具有过程强化、安全性提高、产品性能提高、易实现工业化生产等优势。纳米材料与微反应器技术相结合为进一步研究新型的纳米材料和新型反应器提供了巨大的机会和推动力。本文概述了微反应器的优点,并重点对微反应器在化工行业中制备纳米颗粒物质的应用进行了综述。     

微通道反应器内氯苯硝化反应研究

在微通道反应器内对氯苯硝化反应进行了研究,考察了氯苯与硝酸的摩尔比、体积流速、反应温度等对单程转化率及选择性的影响。实验选择了较优工艺参数组合:n(氯苯)∶n(硝酸)=1∶1.3,n(硝酸)∶n(硫酸)=1∶3,氯苯体积流速0.5 mL/min,反应温度80℃,氯苯单程转化率达74.8%,n(邻硝基氯苯)∶n(对硝基氯苯)=0.56∶1,时空转化率(STC)达4.07×109mol/(m3.h)。微通道反应器内,时空转化率是常规反应器的3.08×104倍。     

邻二氯苯合成3,4-二氯硝基苯的连续流工艺研究

以邻二氯苯为原料、硝酸为硝化剂、浓硫酸为溶剂,研究了在脉冲混合结构微通道反应器中合成3,4-二氯硝基苯的连续流工艺,考察了反应物料摩尔比、硝硫混酸摩尔比、反应温度、反应停留时间等工艺条件。结果表明,当n(邻二氯苯)∶n(硝酸)∶n(硫酸)=1∶2∶4、反应体系温度为60℃、停留时间为135 s时,反应效果最佳。该工艺充分利用了微通道反应器优良的传质传热特点,缩短了反应时间,扩大了工艺条件选择区间,实现了对反应过程的有效控制,增加了安全系数。     

惠安公司与德国IMM合作研发微化工工艺

西安惠安化工集团有限公司与德国美因茨微技术研究所(IMM)最近在西安签订了合作研发协议。双方将在精细化学品，特殊化学品及日用化学品方面应用微反应工艺进行合作研究。双方的合作将从硝酸甘油酯产品的中试生产开始。合作开发的硝酸甘油酯整条生产线将实现全部自动化安全操作，整个过程因应用先进废水处理及封闭式循环系统．将有效避免环境污染。     

微通道连续硝化制备2-硝基-4,5-二甲基乙酰苯胺的工艺研究

本论文开发了在微通道反应器中以3,4-二甲基乙酰苯胺为原料,进行连续硝化反应制备2-硝基-4,5-二甲基乙酰苯胺的新工艺,考察了硝酸浓度、停留时间、反应温度、混酸配比和硝化比等参数对反应的影响,并通过优化工艺参数得到最佳工艺条件。结果表明：最佳的工艺条件为以95%的硝酸和冰乙酸配成的混酸(混酸重量比：硝酸30%、冰乙酸70%)作为硝化试剂,硝化比为2,反应温度40℃,停留时间14.7 min,此条件下原料转化率为100%,目标产物的收率可达68%。与间歇式硝化反应相比,微通道反应器具有安全系数高、副反应少、可实现连续化生产等优点。     

离子液体的非常规制备技术研究进展

离子液体的大规模应用有赖于其制备技术的不断进步。然而,常规制备方法反应时间长、产品纯化繁琐、不宜规模化等问题,制约着离子液体的工业化应用进程。针对离子液体制备过程的关键环节,综述了目前离子液体非常规制备技术的研究进展,重点介绍了微波、超声波、微波-超声、微反应和STT过程强化制备离子液体的技术研究现状,指出现阶段虽然非常规制备技术取得了重要进展,但是仍然需要通过深入细致的研究,建立完善的理论指导体系,同时还要加快功能化离子液体和绿色化制备技术开发。     

Experimental Investigation and Modeling Approach of the Phenylacetonitrile Alkylation Process in a Microreactor

The application of microreaction technology has the potential to intensify chemical processes. It is therefore of great interest to investigate the operating efficiency of a multiphase process such as the alkylation of phenylacetonitrile in a microreactor and to compare the performance to a batch reactor. The undeniable advantages of continuous microreactor systems for this process were demonstrated. Furthermore, the influence of the organic to aqueous phase ratio in the microreactor was investigated. A model of the reaction course was formulated based on experimental data. This model was used in the analysis and modeling of the alkylation process in a microreactor and found to be adequate. The optimal microreactor performance conditions were determined using the numerical optimization technique (Harrington's desirability function) and confirmed by experiments.     

声化学微反应器——超声和微反应器协同强化

微反应器和声化学技术都是化工过程强化的重要手段,但都有优缺点。阐释了“声化学微反应器”的理念--微反应器和声化学技术相互集成,利用超声强化微通道内的混合、传质和预防堵塞等,同样借助微反应器实现声场和气泡场的有效调控并解决声空化过程的放大难题,实现协调强化的目的。同时,深入剖析了声化学微反应器内的声空化行为、声场和气泡场调控规律,以及多相流动体系中的混合与传质强化机制。最后展望了该领域的发展方向,并指出超声空化过程中表界面时空尺度现象和理论是实现并优化超声强化的基础。     

Facile Preparation of an Enzyme‐Immobilized Microreactor using a Cross‐Linking Enzyme Membrane on a Microchannel Surface

The enzyme microreactor has considerable potential for use in biotechnological syntheses and analytical studies. Simplifying the procedure of enzyme immobilization in a microreactor is attractive, and it is achievable by utilizing enzyme immobilization techniques and taking advantage of the characteristics of microfluidics. We previously developed a facile and inexpensive preparation method for an enzyme‐immobilized microreactor. The immobilization of enzymes can be achieved by the formation of an enzyme‐polymeric membrane on the inner wall of the microchannel through cross‐linking polymerization in a laminar flow. However, this method is unsuitable for use in conjunction with electronegative enzymes. Therefore, a novel preparation method using poly‐L ‐lysine [poly(Lys)] as a booster and an adjunct for the effective polymerization of electronegative enzymes was developed in this study. Using aminoacylase as a model for an electronegative enzyme, the reaction conditions for the enzyme‐cross‐linked aggregation were optimized. On the basis of the determined conditions, an acylase‐immobilized tubing microreactor was successfully prepared by cross‐linking polymerization in a concentric laminar flow. The resulting microreactor showed a higher stability against heat and organic solvents compared to those of the free enzyme. The developed method using poly(Lys) was applicable to various enzymes with low isoelectric points, suggesting that this microreactor preparation utilizing a cross‐linked enzyme in a laminar flow could be expanded to microreactors in which a broad range of functional proteins are employed.     

Microreactor technology and process miniaturization for catalytic reactions—A perspective on recent developments and emerging technologies

Recent developments in microreactor technology (MRT) are reviewed within the context of discovery, development and commercialization of catalytic systems. Emerging trends and drivers for development of pilot plants and scale-up methods for the next generation of multiphase catalytic processes are presented. Developments in microreactor scale-out, materials of construction, fabrication techniques, and the potential effect of materials of construction on performance are highlighted. Key issues that impact the adoption and implementation of MRT for research, development, and small-scale commercial applications, including safety, potential performance enhancement, environmental impact, distributed production, scale-up, and computer-aided design tools are also analyzed. The role of MRT in portable power systems is given as an example of a potential commercial application.     

A novel fluidized and induction heated microreactor for catalyst testing

The jiggled bed reactor (JBR) is a state‐of‐the‐art batch fluidized microreactor designed and developed to test catalysts for endothermic reactions. The solid particles in the microreactor are mechanically fluidized by agitating the reactor using a linear pneumatic actuator. An external induction field heats up vertical metal wires installed inside the reactor bed to generate heat rapidly and uniformly within the bed of solid particles, while eliminating hot spots and large temperature gradients. Image and signal processing techniques were utilized to investigate how the fluidization dynamics of the solid particles are affected by the amplitude and frequency of the vibrations, and the size distribution and the mass of the particles. The results show that the microreactor is very flexible: operating conditions can be optimized to successfully fluidize any type of catalyst. Heat‐transfer coefficients between heating surfaces and the bed are similar to the coefficients that could be obtained in a well‐bubbling fluidized bed. This confirms the excellent quality of the fluidization achieved with the new JBR. © 2014 American Institute of Chemical Engineers AIChE J, 60: 3107–3122, 2014     

Gas-liquid flow mass transfer in a T-shape microreactor stimulated with 1.7 MHz ultrasound waves

This paper describes the application of ultrasound waves on hydrodynamics and mass transfer characteristics in the gas-liquid flow in a T-shape microreactor with a diameter of 800 μm.A 1.7 MHz piezoelectric transducer (PZT) was employed to induce the vibration in this microreactor.Liquid side volumetric mass transfer coefficients were measured by physical and chemical methods of CO2 absorption into water and NaOH solution.The approach of absorption of CO2 into a 1 mol· L-1 NaOH solution was used for analysis of interfacial areas.With the help of a photography system,the fluid flow patterns inside the microreactor were analyzed.The effects of superficial liquid velocity,initial concentration of NaOH,superficial CO2 gas velocity and length of microreactor on the mass transfer rate were investigated.The comparison between sonicated and plain microreactors (microreactor with and without ultrasound) shows that the ultrasound wave irradiation has a significant effect on kLa and interfacial area at various operational conditions.For the microreactor length of 12 cm,ultrasound waves improved kLa and interfacial area about 21％ and 22％,respectively.From this study,it can be concluded that ultrasound wave irradiation in microreactor has a great effect on the mass transfer rate.This study suggests a new enhancement technique to establish high interfacial area and kLa in microreactors.     

硝酸铵改性表征技术进展

文章介绍了硝酸铵的物理化学性质,说明了硝酸铵改性效果表征的重要性,综合了国内外硝酸铵改性表征技术研究历史和现状,分析了各种表征技术的特点,展望了表征技术的发展趋势。     

Effect of Hydrodynamic Conditions on Micromixing in Impinging-Jets Microreactors

Theoretical Foundations of Chemical Engineering - Micromixing was experimentally studied by the iodide–iodate technique in a free impinging-jets microreactor (FIJMR) with differentiated...     

微反应器在化学化工领域中的应用

微反应器是微型化学反应系统,具有换热和传质效率高、严格控制反应时间、易于放大、安全性能好等特点。和传统搅拌反应器相比,这些特点使得微反应器在缩短反应时间、大幅度提高化学反应的转化率和产品收率等方面展现出一定的优势。但微反应器也存在易堵塞,催化剂负载、微通道的设计与制造难度大等问题。本文介绍了近年来快速发展的微反应器技术,回顾了微反应器的特点,重点探讨微反应器在化学化工领域的应用以及微反应器在精细化工和制药工业、生物化工领域的应用实例,讨论了微反应器目前存在的诸多挑战。微反应器目前是化学和化工学科的前沿和热点方向,分析表明微反应器仍然有很大的发展空间,有潜力改变化学化工前景。提出应进一步深入系统地认识微反应器内化学反应以及微通道设计的基本规律和机理,将微反应器技术引入更广泛的反应体系中,加强微反应器的集成化水平。