套管膜式微反应器内高效安全的气液传质-反应过程研究进展

doi:10.11949/0438-1157.20240070

化工学报 ›› 2024, Vol. 75 ›› Issue (9): 3011-3027.DOI: 10.11949/0438-1157.20240070

套管膜式微反应器内高效安全的气液传质-反应过程研究进展

杨子驰¹(), 谢冰琪²(), 石瑞莘¹, 雷虹¹, 陈晨¹, 周才金¹^,²(), 张吉松²()

^1.福州大学化工学院，福建福州 350108
^2.清华大学化学工程系，化学工程联合国家重点实验室，北京 100084

收稿日期:2024-01-15 修回日期:2024-03-24 出版日期:2024-09-25 发布日期:2024-10-10
通讯作者: 周才金,张吉松
作者简介:杨子驰（1999—），男，硕士研究生，1943478473@qq.com
谢冰琪（1996—），男，博士研究生，992352738@qq.com
基金资助:
国家自然科学基金项目(22308057);福州大学引进人才科研启动基金项目(0040-511175);福州大学贵重仪器设备开放测试基金项目(2023T003)

Research progress on efficient and safe gas-liquid mass transfer and reaction processes in tube-in-tube reactor

Zichi YANG¹(), Bingqi XIE²(), Ruixin SHI¹, Hong LEI¹, Chen CHEN¹, Caijin ZHOU¹^,²(), Jisong ZHANG²()

^1.College of Chemical Engineering, Fuzhou University, Fuzhou 350108, Fujian, China
^2.State Key Laboratory of Chemical Engineering, Department of Chemical Engineering, Tsinghua University, Beijing 100084, China

Received:2024-01-15 Revised:2024-03-24 Online:2024-09-25 Published:2024-10-10
Contact: Caijin ZHOU, Jisong ZHANG

摘要/Abstract

摘要：

近年来，套管膜式微反应器由于具有传质距离短、气液接触面积大和高透气性等优点，极大地提高了气液传质和反应速度，被视为加快气液传质和流动反应过程的强大工具。目前，套管膜式微反应器已被应用于建立快速准确的气液体系基本参数流动测量平台、实现高效安全的气液反应过程和强化气体介导的生物酶催化反应过程。详细介绍了套管膜式微反应器的构造、组装和操作方式，重点概述了该反应器在不同气液传质-反应过程中的最新研究进展。最后，结合当前的研究热点，展望了套管膜式微反应器的进一步开发方向和未来潜在的应用领域。

关键词: 微反应器, 传质, 多相反应, 生物合成

Abstract:

In recent years, tube-in-tube membrane microreactors have greatly improved gas-liquid mass transfer and reaction rates due to their advantages such as short mass transfer distance, large gas-liquid contact area and high gas permeability. They are regarded as a powerful tool to accelerate the study of gas-liquid mass transfer and flow reaction processes. At present, the tube-in-tube reactor has been widely used to establish a fast and accurate flow measurement platform for gas-liquid physical parameters, achieve efficient and safe gas-liquid reaction processes, and enhance gas-mediated biological enzyme catalytic reaction processes. In this review, a detailed description and construction method, and the recent advancements in this reactor are provided. Finally, based on current research hotspots, a perspective on future potential applications filed of such flow reactor is discussed.

Key words: microreactor, mass transfer, multiphase reaction, biosynthetic process

中图分类号:

TQ 021.1

杨子驰, 谢冰琪, 石瑞莘, 雷虹, 陈晨, 周才金, 张吉松. 套管膜式微反应器内高效安全的气液传质-反应过程研究进展[J]. 化工学报, 2024, 75(9): 3011-3027.

Zichi YANG, Bingqi XIE, Ruixin SHI, Hong LEI, Chen CHEN, Caijin ZHOU, Jisong ZHANG. Research progress on efficient and safe gas-liquid mass transfer and reaction processes in tube-in-tube reactor[J]. CIESC Journal, 2024, 75(9): 3011-3027.

图/表 18

图1 常见的用于强化气液传质的反应器：(a)微通道反应器[15]；(b)降膜反应器[16]；(c)微填充床反应器[17]

Fig.1 The common microreactors used to enhance gas-liquid mass transfer: (a) microchannel reactor[15]; (b) falling film reactor[16]; (c) micropacked bed reactor[17]

图2 常见的套管膜式微反应器装置：(a)聚四氟乙烯外管；(b)不锈钢外管[32, 36]

Fig.2 The two typical configures of the tube-in-tube reactor: (a) polytetrafluoroethylene material outer tube; (b) stainless steel outer tube[32, 36]

图3 套管膜式微反应器内常见的气液两相流动形式：(a)气体在外管流动和液体在内管流动；(b)气体在内管流动和液体在外管流动[40]

Fig.3 The common gas-liquid two-phase flow pattern in tube-in-tube microreactors: (a) gas flows in the outer tube and liquid flows in the inner tube; (b) gas flows in the inner tube and liquid flows in the outer tube[40]

表1 不同反应器比表面积和气液传质系数的比较

Table 1 Comparison of specific surface area and gas-liquid mass transfer coefficient of different reactors

反应器类型	a/(m²/m³)	k_La×10²/s^-1
套管膜式反应器^[41]	3000~10000	10~100
鼓泡塔反应器^[42]	50~600	0.5~24
填充柱反应器^[43]	10~1700	0.04~102
管式反应器^[44]	10~1000	0.5~100
Taylor-Couette反应器^[45]	50~2000	3~21
冲击射流吸收器^[46]	200~1200	2.5~122
喷雾柱设备^[43]	75~170	1.5~2.2
搅拌釜式反应器^[47]	10~2000	0.5~20
静态混合器^[48]	100~1000	10~250
降膜微反应器^[49]	3400~9000	30~2100
微填充床反应器	1945~5464	1.2~50
Y型微通道反应器^[49-50]	9000	0.3~21

图4 微反应器的放大过程[51]

Fig.4 Schematic diagram of the amplification process of the microreactor[51]

图5 用于气-液光催化反应的微反应器放大原理概述[53]

Fig.5 The amplification process of a microreactor for gas-liquid photocatalytic reaction[53]

图6 周期性心形结构反应器的放大图：(a)反应器内混合单元的前视图；(b)心形结构反应器图；(c)单个流动反应器的横截面图[56]

Fig.6 The amplification process diagram of periodic heart-shaped structure reactor: (a) front view of the mixing unit inside the reactor; (b) diagram of heart-shaped reactor; (c) cross section view of a single flow reactor[56]

图7 基于套管膜式微反应器在线测量气体溶解度平台：(a)利用傅里叶变换红外技术在线监测溶剂中溶解的CO气体浓度变化的装置[63]；(b)气泡计数法在线测定溶剂中H2气体浓度[64]（1 bar=0.1 MPa)

Fig.7 An online gas solubility measurement platform based on a tube-in-tube microreactor: (a) a device for monitoring the concentration change of dissolved CO gas using Fourier transform infrared technology[63]; (b) online determination of H2 gas concentration in solvents using bubble counting method[64]

图8 套管膜式膜反应器内在线滴定法测量气体溶解度装置：(a)在线比色滴定技术测定溶剂中NH3气体浓度装置[66]；(b)不同pH下反应器出口的溶液颜色变化[66]；(c)比色滴定技术检测有机溶剂中CO2气体浓度[68]；(d)溶液中CO2气体的滴定曲线[68]

Fig.8 The device for measuring gas solubility using online titration method in a tube-in-tube microreactor： (a) device for measuring NH3 gas concentration in solvents using online colorimetric titration technology[66]; (b) color change of the solution with different pH at the reactor outlet[66]; (c) colorimetric titration technology for detecting the concentration of CO2 gas in organic solvents[68]; (d) titration curve of CO2 gas in solution[68]

图9 套管膜式反应器内测量气体溶解度[62]：(a)实验装置；(b)液体流量和气体流量随时间的变化关系（STP表示标准状况）

Fig.9 Measurement of gas solubility in a tube-in-tube reactor[62]: (a) experimental setup; (b) the variation of liquid flow rate and gas flow rate over time (STP stands for standard temperature and pressure)

表2 套管膜式反应器内气体溶解度测量值与文献值的比较

Table 2 Comparison of gas solubility measurement values in tube-in-tube reactor with literature values

气体	液体	温度/℃	K_H测量值/（mol/（m²·bar））	K_H文献值/（mol/（m²·bar））	相对误差/%
H₂	甲醇	23	3.83±0.02^[62]	3.88^[70]	1.3
H₂	甲醇	40	4.24±0.02^[62]	4.26^[70]	0.5
H₂	甲醇	60	4.70±0.02^[62]	4.62^[70]	1.7
H₂	庚烷	23	4.51±0.02^[62]	4.60^[71]	2.0
H₂	甲基苯乙烯	23	2.51±0.01^[62]	2.56^[72]	1.9
N₂	甲醇	23	6.46±0.03^[69]	6.60^[73]	2.0
O₂	甲醇	23	9.87±0.05^[69]	9.72^[74]	1.6
CO₂	甲醇	23	99.8±0.5^[69]	98.7^[75]	1.1

图10 套管膜式反应器用于测量气体在液体中的扩散系数：(a)反应器内气体扩散过程示意图；(b)Ramping过程中液体流速随气体流速的变化；(c)溶解气体浓度随停留时间的变化[76]

Fig.10 Measuring the diffusion coefficient of gas in liquid with tube-in-tube reactor: (a) schematic diagram of gas diffusion process in the reactor; (b) the variation of liquid flow rate with gas flow rate in the Ramping process; (c) the variation of dissolved gas concentration with residence time[76]

表3 不同Ramping时间下CO2气体在水中扩散系数D的测量值［76］

Table 3 Measurement values of CO2 gas diffusion coefficient in water under different Ramping time［76］

Ramping时间/min	Ramping速度/ (ml/min)	气体扩散稀释/ （10^-9 m²/s）	误差/%
90	0.014	1.97	0
60	0.022	2.00	1.5
40	0.033	1.91	3.0
30	0.043	2.18	10.7
20	0.065	2.69	36.5
10	0.130	6. 00	204.6

图11 套管膜式膜反应器内反应动力学测量概述：(a)气液反应动力学常数测定平台装置；(b)液膜内气体浓度的分布

Fig.11 Overview of reaction kinetics measurement in a tube-in-tube microreactor: (a) platform for measuring the kinetic constants of gas-liquid reactions; (b) the distribution of gas concentration in the liquid film

图12 套管膜式膜反应器内测定酶催化反应动力学的实验装置平台[84]

Fig.12 Experimental setup platform for measuring enzyme catalytic reaction kinetics in a tube-in-tube microreactor[84]

图13 基于微反应器的无细胞蛋白合成装置：(a)基于微芯片反应器开发的无细胞蛋白合成平台装置[93]；(b)高透气性纳米膜微通道反应器用于蛋白质合成[87]；(c)基于套管膜式微反应器的无细胞蛋白合成平台[95]

Fig.13 A cell free protein synthesis device based on a microreactor: (a) device of a developed cell-free protein synthesis platform based on a microchip reactor[93]; (b) a microchannel reactor with highly breathable nanofilms for protein synthesis[87]; (c) cell-free protein synthesis platform based on tube-in-tube microreactor[95]

图14 套管膜式微反应器用于生物氧化过程：(a)酶催化氧化合成邻苯二酚的反应机理；(b)套管膜式微反应器内水、有机两相液体分段流动示意图；(c)连续分段流套管膜式反应器装置[96]

Fig.14 Tube-in-tube microreactor for biological oxidation process: (a) the reaction mechanism of enzymatic oxidation to synthesize catechol; (b) diagram of segmented flow of water and organic two-phase liquids in a tube in tube membrane reactor; (c) device of continuous segmented flow tube-in-tube reactor[96]

图15 基于套管膜式反应器的高效安全的气液反应平台：(a)套管膜式反应器用于加氢反应[66]；(b)套管膜式反应器内利用CO2气体进行羧基化反应装置[101]；(c)套管膜式微反应器用于甲酸/硫酸羰基化反应[102]；(d)用于三氟甲基化的流动化学平台装置示意图[103]（1 psi=6894.757 Pa)

Fig.15 Efficient and safe gas-liquid reaction platform based on tube-in-tube reactor: (a) a tube-in-tube microreactor for hydrogenation reaction[66]; (b) a tube-in-tube reactor was used for carboxylation reaction with CO2 gas[101]; (c) a tube-in-tube microreactor for formic acid/sulfuric acid carbonylation reaction[102]; (d) schematic diagram of a flow chemistry platform for trifluoromethylation[103]（1 psi=6894.757 Pa)

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套管膜式微反应器内高效安全的气液传质-反应过程研究进展

Research progress on efficient and safe gas-liquid mass transfer and reaction processes in tube-in-tube reactor

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