CN103060559A - Microfluid extraction method for extracting and separating In, Fe and Zn - Google Patents

Microfluid extraction method for extracting and separating In, Fe and Zn Download PDF

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CN103060559A
CN103060559A CN2013100347915A CN201310034791A CN103060559A CN 103060559 A CN103060559 A CN 103060559A CN 2013100347915 A CN2013100347915 A CN 2013100347915A CN 201310034791 A CN201310034791 A CN 201310034791A CN 103060559 A CN103060559 A CN 103060559A
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zinc
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extracting
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巨少华
魏亚乾
彭金辉
张利波
代林琴
张利华
郭战永
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Kunming University of Science and Technology
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Abstract

本发明提供一种萃取分离In和Fe、Zn的微流体萃取方法,将含铟、铁、锌的硫酸体系溶液作为水相、经溶剂油稀释的P204萃取剂作为有机相分别通入两台流量泵内,流量泵的出口端连接微反应器入口;同时通过光学显微镜观察微通道内形成的两相层流相界面,使两相平行流动至微通道出口的Y型岔口处时开始分离,从各自出口流出微反应器,并对两相分别收集,铟被萃取进入有机相,而铁和锌留着水相中,实现了铟与铁、锌的分离。In萃取率可达到90%以上,而Fe和Zn离子则完全不被萃取,而且未出现乳化现象,反应所需时间大大缩短,能减少萃取剂的用量和耗量,条件可控性强,安全性高,避免了萃取有机溶剂暴露在空气中。

Figure 201310034791

The invention provides a microfluidic extraction method for extracting and separating In, Fe, and Zn. The sulfuric acid system solution containing indium, iron, and zinc is used as the water phase, and the P204 extraction agent diluted with solvent oil is used as the organic phase. In the pump, the outlet end of the flow pump is connected to the inlet of the microreactor; at the same time, the two-phase laminar flow interface formed in the microchannel is observed through an optical microscope, and the two phases start to separate when they flow in parallel to the Y-shaped fork at the outlet of the microchannel, from Each outlet flows out of the microreactor, and the two phases are collected separately. Indium is extracted into the organic phase, while iron and zinc remain in the water phase, realizing the separation of indium from iron and zinc. The extraction rate of In can reach more than 90%, while Fe and Zn ions are not extracted at all, and there is no emulsification phenomenon, the reaction time is greatly shortened, the amount and consumption of extraction agent can be reduced, and the conditions are controllable and safe. High resistance, to avoid the extraction of organic solvents exposed to the air.

Figure 201310034791

Description

一种萃取分离In和Fe、Zn的微流体萃取方法A microfluidic extraction method for extracting and separating In, Fe, and Zn

技术领域 technical field

本发明涉及一种利用微反应器系统对有价金属进行萃取的方法,属于微流体技术领域。 The invention relates to a method for extracting valuable metals by using a microreactor system, which belongs to the field of microfluid technology.

背景技术 Background technique

湿法冶金的萃取分离过程可以直接从溶液中将多种金属离子进行分离提纯,避免了沉淀、结晶或还原等分离过程产生废渣、以及溶液到渣再到溶液的繁多工序,是冶金溶液体系分离净化的关键手段。但传统萃取过程仍然存在一些需要解决的关键问题: The extraction and separation process of hydrometallurgy can directly separate and purify a variety of metal ions from the solution, avoiding the waste residue generated during the separation process such as precipitation, crystallization or reduction, and the numerous processes from solution to slag and then to solution. key means of purification. However, there are still some key problems that need to be solved in the traditional extraction process:

a、萃取剂耗量大 a. Large consumption of extractant

由于萃取、反萃时间相对较长,往往需要多级甚至十多级萃取,为了适应萃取传质要求,萃取剂用量大。另外,萃取剂与空气接触面积大,受环境温度的影响大,挥发严重,高能搅拌过程的剪切力可能会破坏萃取剂分子结构和引起温升等问题。 Due to the relatively long extraction and stripping time, multi-stage or even more than ten stages of extraction are often required. In order to meet the requirements of extraction and mass transfer, a large amount of extractant is used. In addition, the extractant has a large contact area with the air, is greatly affected by the ambient temperature, and volatilizes severely. The shear force during the high-energy stirring process may destroy the molecular structure of the extractant and cause problems such as temperature rise.

b、共萃严重,萃取效率低 b. Serious co-extraction and low extraction efficiency

在强混合条件下,主金属离子和杂质金属离子的共萃严重,萃取的选择性差,导致萃取之后还需多级洗涤和反萃。如用P204萃取分离Ni、Co过程中由于存在萃Co时Fe、Zn、Mn和Cu的共萃,而使整个萃取级数达到18级以上,再如用P204萃取分离In过程中由于出现Fe、Zn、Sb、Bi和Cl等的共萃问题,使得整个萃取级数达到14级以上。这大大增加了投资成本,降低了萃取效率。 Under strong mixing conditions, the co-extraction of main metal ions and impurity metal ions is severe, and the selectivity of extraction is poor, resulting in the need for multi-stage washing and stripping after extraction. For example, in the process of extracting and separating Ni and Co with P204, due to the co-extraction of Fe, Zn, Mn and Cu during the extraction of Co, the entire extraction stage can reach more than 18 levels. The co-extraction problem of Zn, Sb, Bi and Cl, etc. makes the whole extraction stages reach more than 14 stages. This greatly increases the investment cost and reduces the extraction efficiency.

c、易出现乳化现象 c, prone to emulsification

关于铟萃取过程中产生乳化的机理,目前国内外都进行了深入的研究,并提出了很多预防措施。但到目前为止,乳化现象并不能很好的避免。究其原因,是由于对于存在有颗粒、某种金属离子或是包含表面活性剂的复杂溶液体系,由于常规萃取的高能混合使得萃取过程进行的很充分和迅速,但在相分离过程中,由于稳定性粒子(如颗粒胶体)吸附在乳化液颗粒的液-液界面上成为稳定的保护层,使得两相液滴聚结速率变得非常缓慢甚至完全停止,而从界面上移开一个颗粒所需的能量是很大的。这也就是破乳困难和需要输入大量能量的根本原因。 Regarding the mechanism of emulsification during the extraction of indium, in-depth research has been carried out at home and abroad, and many preventive measures have been proposed. But so far, the emulsification phenomenon cannot be well avoided. The reason is that for complex solution systems with particles, certain metal ions, or surfactants, the high-energy mixing of conventional extraction makes the extraction process very sufficient and rapid, but in the phase separation process, due to Stable particles (such as particle colloids) are adsorbed on the liquid-liquid interface of emulsion particles to become a stable protective layer, making the coalescence rate of two-phase droplets very slow or even completely stopped, and removing a particle from the interface The energy required is great. This is the root cause of difficulty in demulsification and the need to input a large amount of energy.

d、火灾隐患大 d. Big fire hazard

由于萃取过程时间较长,需要建成体积较大的搅拌槽和澄清池,整个萃取过程要占据很大的地方。而且有机相大面积暴露在空气中,使得火灾隐患较大。近年来,我国大型冶炼厂就发生了多起萃取车间失火事故,一些小型的冶炼厂的萃取工序也频发火灾事故。 Since the extraction process takes a long time, it is necessary to build a large volume of stirring tank and clarification tank, and the entire extraction process will occupy a large area. Moreover, a large area of the organic phase is exposed to the air, so that the fire hazard is relatively large. In recent years, there have been many fire accidents in the extraction workshops of large-scale smelters in my country, and frequent fire accidents in the extraction process of some small smelters.

因此,常规萃取的这些局限性亟待解决,而密闭、高效的萃取设备的开发是解决这一问题的关键所在。 Therefore, these limitations of conventional extraction need to be solved urgently, and the development of airtight and efficient extraction equipment is the key to solve this problem.

利用微反应器系统的高效、低耗、安全等特点来改造传统冶金产业的低效高耗单元过程如萃取、换热和混合等,有可能开发出新的节能工艺过程,从而推动冶金行业的产业升级。 Using the characteristics of high efficiency, low consumption and safety of the microreactor system to transform the low-efficiency and high-consumption unit processes of the traditional metallurgical industry such as extraction, heat exchange and mixing, it is possible to develop new energy-saving processes, thereby promoting the development of the metallurgical industry Industrial upgrading.

由于微反应器的有效通道或腔室的物理尺寸缩小到微米甚至纳米级别,使得流体物理量如温度、压力、浓度和密度等的梯度急剧增加,导致传热传质推动力的大大增加,可使传热系数提高一个数量级而传质反应时间降低一个数量级。由此带来的优势还表现在:由于反应速度的提高,反应设备以及反应体系可大大缩减,使得反应过程的安全性大大提高,用地投资大大节约,材料消耗大大减少;对于原料、反应过程或产物存在毒性的反应,可通过采用分区域小型的分布式生产方式,从而避免有毒有害原料产品运输的风险;其处理能力可以通过增加功能单元的数目(Numbering-up)来提高,而不需要逐级放大反应设备。目前先进的微制造技术正在促进微反应器的快速发展,这一领域中的焦点都大量集中在不相溶的液-液两相萃取分离的扩散传质的研究。 Since the physical size of the effective channel or chamber of the microreactor is reduced to the micron or even nanometer level, the gradient of fluid physical quantities such as temperature, pressure, concentration and density increases sharply, resulting in a great increase in the driving force of heat and mass transfer, which can make The heat transfer coefficient increases by an order of magnitude while the mass transfer reaction time decreases by an order of magnitude. The resulting advantages are also manifested in: due to the increase of reaction speed, the reaction equipment and reaction system can be greatly reduced, which greatly improves the safety of the reaction process, greatly saves land investment, and greatly reduces material consumption; for raw materials, reaction processes or Toxic reactions in the product can avoid the risk of transportation of toxic and harmful raw materials by adopting small-scale distributed production methods in different regions; its processing capacity can be improved by increasing the number of functional units (Numbering-up) instead of step by step Level amplification reaction equipment. At present, the advanced micro-manufacturing technology is promoting the rapid development of micro-reactors. The focus in this field is largely on the study of diffusion and mass transfer of immiscible liquid-liquid two-phase extraction separation.

在微流体领域,溶剂萃取是非常高效的,因为它具有能提供很高的比表面积和短的扩散距离的特征。有利于降低扩散的路径长度及增加两相界面的传质速率,从而提高化学反应速率。此外,层流控制下的相传质可以避免乳化发生。通过“数量叠加”Numbering-up(例如并行处理)技术为微流体工艺过程产量的增加提供了一种新的可能。这也使得批量操作(混合/反应/分离)能够连续进行。因此,在微量化学体系下,可以同时达到简化工艺流程防止乳化产生和缩短反应时间的目标。 In the field of microfluidics, solvent extraction is very efficient because of its high specific surface area and short diffusion distance. It is beneficial to reduce the diffusion path length and increase the mass transfer rate of the two-phase interface, thereby increasing the chemical reaction rate. In addition, phase mass transfer under laminar flow control can avoid emulsification. Through the "number superposition" Numbering-up (such as parallel processing) technology provides a new possibility for the increase of the output of the microfluidic process. This also enables batch operations (mixing/reaction/separation) to be performed continuously. Therefore, under the microchemical system, the goals of simplifying the process flow, preventing emulsification and shortening the reaction time can be achieved at the same time.

发明内容 Contents of the invention

本发明所要解决的技术问题在于克服传统溶剂萃取铟的萃取效率低、溶液易乳化、铟与铁、锌等杂质分离困难,对环境污染严重,危险性高等缺点,提供一种萃取分离In和Fe、Zn的微流体萃取方法,是一种高效、安全、无污染、分离率高的新方法。 The technical problem to be solved by the present invention is to overcome the shortcomings of traditional solvent extraction of indium, such as low extraction efficiency, easy emulsification of the solution, difficulty in separating indium from impurities such as iron and zinc, serious environmental pollution, and high risk, and provides a method for extracting and separating In and Fe , The microfluidic extraction method of Zn is a new method with high efficiency, safety, no pollution and high separation rate.

本发明通过下列技术方案实现:一种萃取分离In和Fe、Zn的微流体萃取方法,经过下列各步骤: The present invention is realized through the following technical solutions: a microfluidic extraction method for extracting and separating In, Fe, and Zn, through the following steps:

(1)将含铟、铁、锌的硫酸体系溶液作为水相、经溶剂油稀释的P204萃取剂作为有机相分别通入两台流量泵内,流量泵的出口端连接微反应器入口; (1) The sulfuric acid system solution containing indium, iron, and zinc is used as the water phase, and the P204 extractant diluted with solvent oil is used as the organic phase to pass into two flow pumps respectively, and the outlet end of the flow pump is connected to the inlet of the microreactor;

(2)先开启有机相流量泵,待有机相进入微反应器的微通道后,再按有机相流量的0.65倍设定并开启水相流量泵,同时通过光学显微镜观察微通道内形成的两相层流相界面(显微镜俯视观察能看到水相和有机相在微通道中呈左右平行前进,两相层流相界面即为水相和有机相的接触面),期间调节两相的流量,使两相平行流动; (2) Turn on the flow pump of the organic phase first. After the organic phase enters the microchannel of the microreactor, set the flow rate of the organic phase at 0.65 times and turn on the flow pump of the water phase. Phase laminar flow phase interface (observation with a microscope can see that the water phase and the organic phase are moving in parallel in the microchannel, and the two-phase laminar flow phase interface is the contact surface between the water phase and the organic phase), during which the flow of the two phases is adjusted , so that the two phases flow in parallel;

(3)两相流至微通道出口的Y型岔口处时开始分离,从各自出口流出微反应器,并对两相分别收集,铟被萃取进入有机相,而铁和锌留着水相中,实现了铟与铁、锌的分离。 (3) When the two phases flow to the Y-shaped fork at the outlet of the microchannel, they begin to separate, and flow out of the microreactor from their respective outlets, and collect the two phases separately. Indium is extracted into the organic phase, while iron and zinc remain in the water phase , realized the separation of indium, iron and zinc.

所述含铟、铁、锌的硫酸体系溶液是湿法冶炼锌过程中的浸出液。 The sulfuric acid system solution containing indium, iron and zinc is the leaching solution in the zinc hydrometallurgy process.

所述溶剂油是常规溶剂油,如260号溶剂油。 Described solvent oil is conventional solvent oil, such as No. 260 solvent oil.

所述微通道的特征尺寸为160~800μm(内径),长度为80~480mm。 The characteristic size of the microchannel is 160-800 μm (inner diameter), and the length is 80-480 mm.

所述两相在微通道中的接触时间为0.01~10s。 The contact time of the two phases in the microchannel is 0.01-10s.

发明原理:由于微反应器内两相界面积与两相传质深度之比,两相中目标元素浓度梯度很大,致使萃取推动力大大提高,传质效率往往比传统操作提高一个数量级。所以互不相溶的两相可以在微通道内,通过短时间的层流流动接触的情况下进行快速传质。它的特点是强化了冶金操作单元过程,提高效率、降低能耗。 Invention principle: Due to the ratio of the area of the two-phase interface in the microreactor to the mass transfer depth of the two phases, the concentration gradient of the target element in the two phases is very large, resulting in a greatly improved extraction driving force, and the mass transfer efficiency is often an order of magnitude higher than that of traditional operations. Therefore, the immiscible two phases can undergo rapid mass transfer in the microchannel under the condition of short-time laminar flow contact. It is characterized by strengthening the metallurgical operation unit process, improving efficiency and reducing energy consumption.

微流体技术是在微观尺寸下控制、操作和检测复杂流体的技术,是在微化工、微机械、生物工程和纳米技术基础上发展起来的一门全新交叉学科。近年来微流体技术的快速发展,已经在化学、医药及生命科学等领域上造成革命性的冲击。目前,在化学和化工领域,如气体处理、化学合成及颗粒合成等,微流体技术已经能够达到年产数吨的产能。因此,把微流体技术应用于湿法冶金领域,可能在改善湿法冶金溶剂萃取过程的乳化现象、降低萃取剂用量和提高萃取操作的安全性等方面,发挥重要作用。 Microfluidic technology is a technology for controlling, manipulating and detecting complex fluids at a microscopic scale. It is a new interdisciplinary subject developed on the basis of microchemical engineering, micromechanics, bioengineering and nanotechnology. The rapid development of microfluidic technology in recent years has caused revolutionary impacts in the fields of chemistry, medicine and life sciences. At present, in the field of chemistry and chemical engineering, such as gas treatment, chemical synthesis and particle synthesis, microfluidic technology has been able to achieve an annual production capacity of several tons. Therefore, the application of microfluidic technology in the field of hydrometallurgy may play an important role in improving the emulsification phenomenon in the hydrometallurgical solvent extraction process, reducing the amount of extractant and improving the safety of extraction operations.

本发明使用微流体技术,使两相液体在微通道内保持层流流动,通过Y型出口快速分离,In萃取率可达到90%以上,而Fe和Zn离子则完全不被萃取,而且未出现乳化现象,从而避免了传统萃取含In、Fe和Zn溶液的一系列问题。具有以下效果和优点: The present invention uses microfluidic technology to keep the two-phase liquid in the microchannel to maintain laminar flow, and quickly separates through the Y-shaped outlet. The extraction rate of In can reach more than 90%, while Fe and Zn ions are not extracted at all, and there is no Emulsification phenomenon, thereby avoiding a series of problems in the traditional extraction of solutions containing In, Fe and Zn. It has the following effects and advantages:

1、本发明针对湿法炼锌浸出液中的In金属,采用微流体溶剂萃取技术回收,回收效率高,且反应所需时间大大缩短。 1. The present invention adopts microfluidic solvent extraction technology to recover In metal in the zinc hydrometallurgy leaching solution, the recovery efficiency is high, and the time required for the reaction is greatly shortened.

2、本发明由于萃取过程耗时短,通过提高循环次数,可大大减少萃取剂的用量和耗量。 2. Since the extraction process of the present invention is short in time, the amount and consumption of the extractant can be greatly reduced by increasing the number of cycles.

3、本发明采用微流体层流条件下进行选择性萃取,可避免萃取过程出现乳化现象。 3. The present invention uses microfluidic laminar flow conditions for selective extraction, which can avoid emulsification during the extraction process.

4、本发明使得In与Fe和Zn等杂质金属高效分离,萃取选择性非常优越。 4. The present invention enables efficient separation of In from impurity metals such as Fe and Zn, and the extraction selectivity is very superior.

5、本发明在保证反应在封闭体系中进行,条件可控性强,安全性高,避免了萃取有机溶剂暴露在空气中,产生挥发和火灾的危险。 5. The present invention ensures that the reaction is carried out in a closed system, the conditions are highly controllable, and the safety is high, avoiding the risk of volatilization and fire caused by the extraction of organic solvents exposed to the air.

附图说明 Description of drawings

图1为本发明微反应器的装置示意图; Fig. 1 is the device schematic diagram of microreactor of the present invention;

图2为实施例1微通道的截面示意图。 Figure 2 is a schematic cross-sectional view of the microchannel of Example 1.

具体实施方式 Detailed ways

下面通过实施例对本发明做进一步说明。 The present invention will be further described below by embodiment.

实施例1 Example 1

(1)将含铟4.52g/L、铁、锌的硫酸体系溶液(湿法冶炼锌过程中的浸出液)作为水相、经260号溶剂油稀释的P204萃取剂(30%体积分数P204+70%体积分数溶剂油)作为有机相分别通入两台流量泵内,流量泵的出口端连接微反应器入口; (1) The sulfuric acid system solution containing 4.52g/L indium, iron, and zinc (leaching solution in the process of hydrometallurgy of zinc) is used as the water phase, and the P204 extraction agent diluted with No. 260 solvent oil (30% volume fraction P204+70 %volume fraction solvent oil) as the organic phase respectively into the two flow pumps, the outlet end of the flow pump is connected to the inlet of the microreactor;

(2)先开启有机相流量泵,待有机相进入微反应器的微通道(特征尺寸为160μm、长度为380mm)后,再按有机相流量的0.65倍设定并开启水相流量泵,同时通过光学显微镜观察微通道内形成的两相层流相界面(显微镜俯视观察能看到水相和有机相在微通道中呈左右平行前进,两相层流相界面即为水相和有机相的接触面),期间调节两相的流量,使两相平行流动,两相在微通道中的接触时间为1.49s; (2) Turn on the organic phase flow pump first, and after the organic phase enters the microchannel of the microreactor (with a characteristic size of 160 μm and a length of 380 mm), set and turn on the water phase flow pump at 0.65 times the flow rate of the organic phase, and at the same time The two-phase laminar flow interface formed in the microchannel is observed through an optical microscope (observation with a microscope can see that the water phase and the organic phase are moving in parallel from left to right in the microchannel, and the two-phase laminar flow interface is the water phase and the organic phase. contact surface), during which the flow of the two phases is adjusted so that the two phases flow in parallel, and the contact time of the two phases in the microchannel is 1.49s;

(3)两相流至微通道出口的Y型岔口处时开始分离,从各自出口流出微反应器,并对两相分别收集,铟被萃取进入有机相,而铁和锌留着水相中,实现了铟与铁、锌的分离。检测得到92.50%的In萃取率,体系无乳化现象。 (3) When the two phases flow to the Y-shaped fork at the outlet of the microchannel, they begin to separate, and flow out of the microreactor from their respective outlets, and collect the two phases separately. Indium is extracted into the organic phase, while iron and zinc remain in the water phase , realized the separation of indium, iron and zinc. The In extraction rate of 92.50% was detected, and the system had no emulsification phenomenon.

实施例2 Example 2

(1)将含铟3.17g/L、铁3.42g/L、锌52.82g/L的硫酸体系溶液(湿法冶炼锌过程中的浸出液)作为水相、经常规溶剂油稀释的P204萃取剂(30%体积分数P204+70%体积分数溶剂油)作为有机相分别通入两台流量泵内,流量泵的出口端连接微反应器入口; (1) The sulfuric acid system solution containing 3.17g/L of indium, 3.42g/L of iron, and 52.82g/L of zinc (leaching solution in the process of hydrometallurgy of zinc) is used as the water phase, P204 extractant diluted with conventional solvent oil ( 30% volume fraction P204+70% volume fraction solvent oil) as the organic phase respectively passed into two flow pumps, and the outlet end of the flow pump was connected to the inlet of the microreactor;

(2)先开启有机相流量泵,待有机相进入微反应器的微通道(特征尺寸为200μm、长度为80mm)后,再按有机相流量的0.65倍设定并开启水相流量泵,同时通过光学显微镜观察微通道内形成的两相层流相界面(显微镜俯视观察能看到水相和有机相在微通道中呈左右平行前进,两相层流相界面即为水相和有机相的接触面),期间调节两相的流量,使两相平行流动,两相在微通道中的接触时间为0.69s; (2) Turn on the flow pump of the organic phase first, and after the organic phase enters the microchannel of the microreactor (with a characteristic size of 200 μm and a length of 80 mm), set the flow rate of the organic phase to 0.65 times and turn on the flow pump of the water phase, and at the same time The two-phase laminar flow interface formed in the microchannel is observed through an optical microscope (observation with a microscope can see that the water phase and the organic phase are moving in parallel from left to right in the microchannel, and the two-phase laminar flow interface is the water phase and the organic phase. contact surface), during which the flow of the two phases is adjusted so that the two phases flow in parallel, and the contact time of the two phases in the microchannel is 0.69s;

(3)两相流至微通道出口的Y型岔口处时开始分离,从各自出口流出微反应器,并对两相分别收集,铟被萃取进入有机相,而铁和锌留着水相中,实现了铟与铁、锌的分离。检测得到90.80%的In萃取率,而Fe、Zn的萃取率均为0,体系无乳化现象。 (3) When the two phases flow to the Y-shaped fork at the outlet of the microchannel, they begin to separate, and flow out of the microreactor from their respective outlets, and collect the two phases separately. Indium is extracted into the organic phase, while iron and zinc remain in the water phase , realized the separation of indium, iron and zinc. It was detected that the extraction rate of In was 90.80%, while the extraction rates of Fe and Zn were both 0, and the system had no emulsification phenomenon.

实施例3 Example 3

(1)将含铟4.12g/L、铁、锌的硫酸体系溶液(湿法冶炼锌过程中的浸出液)作为水相、经常规溶剂油稀释的P204萃取剂作为有机相分别通入两台流量泵内,流量泵的出口端连接微反应器入口; (1) The sulfuric acid system solution containing 4.12g/L indium, iron and zinc (leaching solution in the process of hydrometallurgy of zinc) is used as the water phase, and the P204 extractant diluted with conventional solvent oil is used as the organic phase to pass into two flow In the pump, the outlet end of the flow pump is connected to the inlet of the microreactor;

(2)先开启有机相流量泵,待有机相进入微反应器的微通道(特征尺寸为800μm、长度为90mm)后,再按有机相流量的0.65倍设定并开启水相流量泵,同时通过光学显微镜观察微通道内形成的两相层流相界面(显微镜俯视观察能看到水相和有机相在微通道中呈左右平行前进,两相层流相界面即为水相和有机相的接触面),期间调节两相的流量,使两相平行流动,两相在微通道中的接触时间为0.01s; (2) Turn on the flow pump of the organic phase first, and after the organic phase enters the microchannel of the microreactor (the characteristic size is 800 μm, the length is 90 mm), then set and turn on the flow pump of the water phase at 0.65 times the flow rate of the organic phase, and at the same time The two-phase laminar flow interface formed in the microchannel is observed through an optical microscope (observation with a microscope can see that the water phase and the organic phase are moving in parallel from left to right in the microchannel, and the two-phase laminar flow interface is the water phase and the organic phase. contact surface), during which the flow of the two phases is adjusted so that the two phases flow in parallel, and the contact time of the two phases in the microchannel is 0.01s;

(3)两相流至微通道出口的Y型岔口处时开始分离,从各自出口流出微反应器,并对两相分别收集,铟被萃取进入有机相,而铁和锌留着水相中,实现了铟与铁、锌的分离。检测得到92.10%的In萃取率,体系无乳化现象。 (3) When the two phases flow to the Y-shaped fork at the outlet of the microchannel, they begin to separate, and flow out of the microreactor from their respective outlets, and collect the two phases separately. Indium is extracted into the organic phase, while iron and zinc remain in the water phase , realized the separation of indium, iron and zinc. The In extraction rate of 92.10% was detected, and the system had no emulsification phenomenon.

实施例4 Example 4

(1)将含铟3.92g/L、铁、锌的硫酸体系溶液(湿法冶炼锌过程中的浸出液)作为水相、经260号溶剂油稀释的P204萃取剂作为有机相分别通入两台流量泵内,流量泵的出口端连接微反应器入口; (1) The sulfuric acid system solution containing 3.92g/L indium, iron and zinc (leaching solution in the process of hydrometallurgy of zinc) is used as the water phase, and the P204 extractant diluted with No. 260 solvent oil is used as the organic phase to pass into two sets In the flow pump, the outlet of the flow pump is connected to the inlet of the microreactor;

(2)先开启有机相流量泵,待有机相进入微反应器的微通道(特征尺寸为700μm、长度为480mm后,再按有机相流量的0.65倍设定并开启水相流量泵,同时通过光学显微镜观察微通道内形成的两相层流相界面(显微镜俯视观察能看到水相和有机相在微通道中呈左右平行前进,两相层流相界面即为水相和有机相的接触面),期间调节两相的流量,使两相平行流动,两相在微通道中的接触时间为10s; (2) Turn on the organic phase flow pump first, wait for the organic phase to enter the microchannel of the microreactor (with a characteristic size of 700 μm and a length of 480 mm, then set and turn on the water phase flow pump at 0.65 times the flow rate of the organic phase, and simultaneously pass The two-phase laminar flow interface formed in the microchannel is observed by an optical microscope (the water phase and the organic phase can be seen to move in parallel in the microchannel when viewed from the top of the microscope, and the two-phase laminar flow interface is the contact between the water phase and the organic phase surface), during which the flow rate of the two phases is adjusted so that the two phases flow in parallel, and the contact time of the two phases in the microchannel is 10s;

(3)两相流至微通道出口的Y型岔口处时开始分离,从各自出口流出微反应器,并对两相分别收集,铟被萃取进入有机相,而铁和锌留着水相中,实现了铟与铁、锌的分离。检测得到91.86%的In萃取率,体系无乳化现象。 (3) When the two phases flow to the Y-shaped fork at the outlet of the microchannel, they begin to separate, and flow out of the microreactor from their respective outlets, and collect the two phases separately. Indium is extracted into the organic phase, while iron and zinc remain in the water phase , realized the separation of indium, iron and zinc. The In extraction rate of 91.86% was detected, and the system had no emulsification phenomenon.

Claims (5)

1. the microfluid extracting process of an extracting and separating In and Fe, Zn is characterized in that through following each step:
The sulfuric acid system solution that (1) will contain indium, iron, zinc is as water, pass into respectively as organic phase in two flow pumps through the P204 extraction agent of solvent oil dilution, and the exit end of flow pump connects the microreactor entrance;
(2) open first organic phase flow pump, enter the microchannel of microreactor until organic phase after, pressing 0.65 times of the organic phase flow sets and open water phase flow rate pump again, pass through simultaneously the two-phase laminar flow phase interface of formation in the observation by light microscope microchannel, regulate during this time the flow of two-phase, make the two-phase split flow;
Begin to separate when (3) two phase flow is to the place, Y type fork of microchannel outlet, flow out microreactor from outlet separately, and two-phase is collected respectively, indium is extracted and enters organic phase, and iron and zinc are kept aqueous phase, has realized separating of indium and iron, zinc.
2. the microfluid extracting process of extracting and separating In according to claim 1 and Fe, Zn, it is characterized in that: the described sulfuric acid system solution that contains indium, iron, zinc is the leach liquor in the hydrometallurgy zinc process.
3. the microfluid extracting process of extracting and separating In according to claim 1 and Fe, Zn, it is characterized in that: described solvent oil is conventional solvent oil.
4. the microfluid extracting process of extracting and separating In according to claim 1 and Fe, Zn, it is characterized in that: the characteristic dimension of described microchannel is 160~800 μ m, and length is 80~480mm.
5. the microfluid extracting process of extracting and separating In according to claim 1 and Fe, Zn is characterized in that: the duration of contact of described two-phase in the microchannel is 0.01~10s.
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