CN106378021B - Parallel micro-impact flow mixing device and using method thereof - Google Patents
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Abstract
本发明公开了一种并列式微撞击流混合装置，包括微撞击流模块、前置进料模块、后置密封模块、连接装置；所述微撞击流模块内部设有相互平行的进样通道，与进样通道垂直设有撞击通道，撞击通道为T型结构，底部设有渐扩形出料口；所述前置进料模块出口端连接微撞击流模块入口端，微撞击流模块的末端处通过后置密封模块密封；前置进料模块、微撞击流模块和后置密封模块通过连接装置连接紧固。该装置主要针对液‑液快速反应体系，既可用作旋转填料床的预混合与分布装置，也可单独用作液‑液快速反应的反应器，制备超细/纳米功能材料；通过并列式的撞击流混合，解决了微撞击流混合器放大的难题，实现了RPB微观混合性能的进一步提升。
The invention discloses a parallel micro-impact flow mixing device, which comprises a micro-impact flow module, a pre-feeding module, a rear-mounted sealing module and a connection device; the micro-impact flow module is internally provided with mutually parallel sampling channels, which are parallel to each other. The injection channel is vertically provided with an impact channel, the impact channel is a T-shaped structure, and the bottom is provided with a gradually expanding discharge port; the outlet end of the pre-feeding module is connected to the inlet end of the micro-impact flow module, and the end of the micro-impact flow module is at the end. It is sealed by the rear sealing module; the front feeding module, the micro-impact flow module and the rear sealing module are connected and fastened by the connecting device. The device is mainly aimed at the liquid-liquid rapid reaction system. It can be used as a pre-mixing and distribution device for a rotating packed bed, and can also be used alone as a liquid-liquid rapid reaction reactor to prepare ultrafine/nano functional materials; The impinging flow mixing of the micro impingement flow mixer solves the problem of amplification of the micro impinging flow mixer, and further improves the micro-mixing performance of the RPB.
Description
技术领域technical field
本发明涉及一种并列式微撞击流混合装置及其使用方法，属于化工过程强化技术领域。The invention relates to a parallel micro-impact flow mixing device and a method for using the same, belonging to the technical field of chemical process strengthening.
背景技术Background technique
分子尺度的微观混合是反应能够进行的前提，强化微观混合能极大地改善反应状况，进而获得高质量的产物。常见的过程强化技术有撞击流、超重力、微通道技术等。Molecular-scale micro-mixing is the premise for the reaction to proceed. Strengthening the micro-mixing can greatly improve the reaction conditions and obtain high-quality products. Common process enhancement technologies include impinging flow, hypergravity, and microchannel technology.
撞击流(Impinging Stream)是一类重要的流体混合强化技术，对扩散控制的化工过程尤其有效。经过多年发展，撞击流的连续相由气相扩展到了液相，由此更加突出撞击流强化液相微观混合的优势。对于液相撞击流装置的微观混合研究，国外主要集中在自由式撞击流(FIS)和受限式撞击流(CIS)两类结构，国内则以伍沅提出的浸没式结构为主(CN1463789A、CN2455353Y)。自由式和受限式撞击流装置的停留时间极短，且两者都可以进行连续操作，其中受限式撞击流的微观混合效果明显优于自由式撞击流；浸没式撞击流装置的主要特点是停留时间长，但主要适用于间歇操作，且微观混合效果弱于FIS与CIS装置。相比于传统釜式反应器，撞击流装置结构简单、混合效率高，因此撞击流技术在粉体干燥、超细/纳米功能材料制备以及乳化等领域发挥了重要作用。Impinging Stream is an important fluid mixing enhancement technology, especially effective for diffusion-controlled chemical processes. After years of development, the continuous phase of the impinging flow has expanded from the gas phase to the liquid phase, which highlights the advantages of the impinging flow in enhancing the micro-mixing of the liquid phase. For the micro-mixing research of liquid-phase impinging flow devices, foreign countries mainly focus on two types of structures, free impinging flow (FIS) and confined impinging flow (CIS), while domestically, the submerged structure proposed by Wu Yuan is the main (CN1463789A, CN2455353Y). The residence time of the free and confined impinging flow devices is extremely short, and both can be operated continuously. The micro-mixing effect of the confined impinging flow is obviously better than that of the free impinging flow; the main features of the submerged impinging flow device It has a long residence time, but it is mainly suitable for intermittent operation, and the micro-mixing effect is weaker than that of FIS and CIS devices. Compared with the traditional tank reactor, the impinging flow device has a simple structure and high mixing efficiency, so the impinging flow technology has played an important role in the fields of powder drying, ultrafine/nano functional material preparation and emulsification.
超重力是另一类重要的过程强化技术，其核心设备为旋转填料床。在旋转填料床内，流体受到离心力作用而被撕裂成液滴、液丝、液膜，进而极大地强化受传质扩散控制的反应过程。有关超重力装置已公开，详见中国专利ZL95215430.7等。超重力技术已经成功应用于分离、解析、有机合成、超细粉体制备等领域。超重力旋转填料床(RPB)的微观混合性能明显优于其它过程强化设备，其微观混合时间为0.01-0.1ms。然而，传统的超重力旋转填料床存在以下问题：(1)物料不经过预混直接注入旋转填料，导致部分反应物尚未接触就已排出，降低了物料的利用率；(2)流体在旋转填料床的轴向分布状况较差，导致其填料的利用率普遍偏低。Hypergravity is another important process intensification technology, and its core equipment is a rotating packed bed. In the rotating packed bed, the fluid is torn into droplets, liquid filaments and liquid films under the action of centrifugal force, which greatly strengthens the reaction process controlled by mass transfer and diffusion. The supergravity device has been disclosed, see Chinese patent ZL95215430.7 and so on. Hypergravity technology has been successfully used in separation, analysis, organic synthesis, ultrafine powder preparation and other fields. The micro-mixing performance of the supergravity rotating packed bed (RPB) is significantly better than other process intensification equipment, and its micro-mixing time is 0.01-0.1ms. However, the traditional supergravity rotating packed bed has the following problems: (1) the material is directly injected into the rotating packing without premixing, so that part of the reactants are discharged without contact, which reduces the utilization rate of the material; (2) the fluid is in the rotating packing The axial distribution of the bed is poor, resulting in a generally low utilization rate of its packing.
针对上述问题，中国专利(CN1425493A)公开了一种撞击流-旋转填料床(IS-RPB)，在转鼓腔体中心位置安装自由撞击流装置，使物料首先进行预混，同时流体撞击产生了大量的分散液滴，这些液滴会被旋转填料捕获，进一步混合、反应。该实用新型突破了旋转填料床的技术难题，提高了旋转填料床的微观混合性能。然而，产物混合效果受到液滴的捕集率的影响；最重要的是，自由撞击流的微观混合性能明显弱于受限式撞击流，且撞击面易受流体扰动的影响，设备运行的稳定性较差。同时，应用于工业放大装置时，多级并行的自由撞击流间会产生相互干扰，不利于提高产物质量。此外，自由撞击产生的液滴飞溅，容易对管件及壳体造成严重污染，增加了装置的清理、维护难度。In view of the above problems, Chinese patent (CN1425493A) discloses an impinging flow-rotating packed bed (IS-RPB), in which a free impinging flow device is installed at the center of the drum cavity, so that the materials are first premixed, and at the same time the fluid impingement produces a A large number of dispersed droplets, which are captured by the rotating packing, are further mixed and reacted. The utility model breaks through the technical difficulties of the rotating packed bed and improves the micro-mixing performance of the rotating packed bed. However, the product mixing effect is affected by the capture rate of the droplets; most importantly, the micro-mixing performance of the free impinging flow is significantly weaker than that of the confined impinging flow, and the impinging surface is easily affected by fluid disturbance, and the equipment operates stably Poor sex. At the same time, when applied to an industrial amplifying device, the multi-stage parallel free impingement flows will interfere with each other, which is not conducive to improving the product quality. In addition, the splash of droplets generated by free impact is easy to cause serious pollution to the pipe fittings and the casing, which increases the difficulty of cleaning and maintenance of the device.
发明内容SUMMARY OF THE INVENTION
本发明旨在提供一种并列式微撞击流装置，采用多组受限式撞击流模块前后衔接，形成多级并列式混合装置，解决了IS-RPB放大应用的难题；该装置能进一步提升RPB的微观混合性能，提高设备运行的稳定性，并降低设备的清理、维护难度。本发明还提供了该装置的使用方法。The invention aims to provide a parallel micro impingement flow device, which adopts multiple groups of restricted impinging flow modules to connect back and forth to form a multi-stage parallel mixing device, which solves the problem of the amplification and application of IS-RPB; the device can further improve the RPB performance. Micro-mixing performance improves the stability of equipment operation and reduces the difficulty of cleaning and maintenance of equipment. The present invention also provides a method of using the device.
本发明提供了一种并列式微撞击流混合装置，包括微撞击流模块、前置进料模块、后置密封模块、连接装置；The invention provides a parallel micro-impact flow mixing device, comprising a micro-impact flow module, a pre-feeding module, a rear sealing module and a connecting device;
所述微撞击流模块为长方体结构，内部设有相互平行的进样通道，在长方体中心处与进样通道垂直设有撞击通道，撞击通道为T型结构，底部连接出料口；The micro-impact flow module is of a rectangular parallelepiped structure, and is provided with mutually parallel sample injection channels inside, and an impact channel is perpendicular to the sample injection channel at the center of the rectangular parallelepiped.
所述前置进料模块的入口为塔式或螺纹结构，内部为直通孔，前置进料模块出口端微撞击流模块入口端，微撞击流模块的末端处通过后置密封模块密封；后置密封模块为矩形板；The inlet of the pre-feeding module is a tower or threaded structure, the interior is a straight hole, the outlet end of the pre-feeding module impacts the inlet end of the flow module, and the end of the micro-impact flow module is sealed by the rear sealing module; Set the sealing module as a rectangular plate;
所述连接装置包括连杆和螺母；前置进料模块、微撞击流模块和后置密封模块通过连接装置依次连接紧固，模块衔接处采用垫圈密封。The connecting device includes a connecting rod and a nut; the front feeding module, the micro-impact flow module and the rear sealing module are connected and fastened in sequence through the connecting device, and the joints of the modules are sealed with gaskets.
上述装置中，微撞击流模块是该装置的核心部件，该模块的进样通道相互平行，通道内径D＝8.0～10.0mm，长度为10.0～20.0mm，通道间距为I＝6.0～10.0mm；“T”型撞击通道是流体进行混合/反应的场所，其所在平面与进样通道所在的平面相互垂直，撞击通道为等径三通，通径d＝1.0～2.0mm，较小的通道尺度促进了微区效应的形成，极大地强化了流体的微观混合，撞击通道的长度为6.0～10.0mm；位于撞击通道结构下方的是流体出料口，所述出料口为渐扩的锥形，其上端与撞击通道底部连接，内径为1.0～2.0mm，出口处的内径为3.3～5.3mm，锥角α＝30～45°，主要用于均匀分布液体。In the above device, the micro-impact flow module is the core component of the device, the sample injection channels of the module are parallel to each other, the inner diameter of the channel is D=8.0～10.0mm, the length is 10.0～20.0mm, and the channel spacing is I=6.0～10.0mm; The "T"-shaped impact channel is a place where fluids are mixed/reacted. The plane where it is located is perpendicular to the plane where the injection channel is located. The impact channel is an equal-diameter tee with a diameter of d=1.0-2.0mm, and the smaller channel size It promotes the formation of micro-area effect and greatly strengthens the micro-mixing of fluids. The length of the impact channel is 6.0-10.0mm; the fluid outlet is located below the impact channel structure, and the outlet is a gradually expanding cone. , its upper end is connected to the bottom of the impact channel, the inner diameter is 1.0-2.0mm, the inner diameter at the outlet is 3.3-5.3mm, and the cone angle α=30-45°, which is mainly used for evenly distributing the liquid.
上述装置中，所述前置进料模块的入口段设计为塔式或螺纹结构，便于管路连接，其内径为8.0～10.0mm，厚度为2.0mm，长度为50～100mm。入口段长管除了用于进料外，还可以起到调整装置在反应系统(如：旋转填料床)内的空间位置。后置密封模块与前置模块配合，用于密封整个装置，通过螺栓、连杆以及凹槽实现高度密封，防止流体泄露。In the above device, the inlet section of the pre-feeding module is designed as a tower or threaded structure, which is convenient for pipeline connection. In addition to being used for feeding, the long pipe in the inlet section can also be used to adjust the spatial position of the device in the reaction system (eg, rotating packed bed). The rear sealing module cooperates with the front module to seal the entire device, and achieves a high degree of sealing through bolts, connecting rods and grooves to prevent fluid leakage.
前置进料模块的入口段需要与管路连接，塔式结构多用于连接软管，也可以采用其它常用连接方式，例如螺纹或法兰，因此将前置进料模块的入口段设计为塔式或螺纹结构。The inlet section of the pre-feed module needs to be connected to the pipeline. The tower structure is mostly used to connect hoses, and other common connection methods, such as threads or flanges, can also be used. Therefore, the inlet section of the pre-feed module is designed as a tower. type or threaded construction.
上述装置中，所述微撞击流模块前、后端面的四个角上分别设有孔，所述前置进料模块和后置密封模块的四个角上与微撞击流模块对应处分别设有相同的孔，连杆从上述孔中穿过，通过螺母固定。In the above device, the four corners of the front and rear surfaces of the micro-impact flow module are respectively provided with holes, and the four corners of the front feeding module and the rear sealing module are respectively provided with the corresponding positions of the micro-impact flow module. There are the same holes through which the connecting rods pass and are held in place by nuts.
上述装置中，所述前置进料模块与微撞击流模块，或后置密封模块与微撞击流模块，或两个微撞击流模块的衔接处，通过垫圈密封；在每种模块的进料通道端部设有环形凹槽，出口端设有凸起结构，凸起与凹槽依次配合连接，垫圈设置在该凹槽内。In the above device, the pre-feeding module and the micro-impact flow module, or the rear sealing module and the micro-impact flow module, or the junction of the two micro-impact flow modules, are sealed by gaskets; The end of the channel is provided with an annular groove, the outlet end is provided with a convex structure, the convex and the groove are matched and connected in sequence, and the gasket is arranged in the groove.
本发明中，所述模块采用不锈钢、聚四氟乙烯或聚甲基丙烯酸甲酯等材料制备，模块之间采用螺栓连接密封。In the present invention, the modules are made of materials such as stainless steel, polytetrafluoroethylene or polymethyl methacrylate, and bolts are used to seal the modules.
本发明提供了一种并列式微撞击流混合装置的使用方法，包括以下任一种：The present invention provides a method for using a parallel micro-impact flow mixing device, including any of the following:
(1)使用一组或多组微撞击流模块，形成单级或多级结构，用作混合器或反应器；(1) Use one or more groups of micro-impact flow modules to form a single-stage or multi-stage structure for use as a mixer or reactor;
(2)使用一组或并列连接多组微撞击流模块，形成单级或多级的撞击流结构，与旋转填料床耦合，用于工业化生产。(2) One group or multiple groups of micro-impact flow modules are connected in parallel to form a single-stage or multi-stage impingement flow structure, which is coupled with the rotating packed bed for industrial production.
所述多级的撞击流结构，出料方向与旋转轴垂直；各组模块之间通过环形凹槽与凸起结构相互衔接，凹槽位于每个模块进料端，凹槽宽度为1.0mm，模块的组数根据实际情况进行调节。In the multi-stage impact flow structure, the discharge direction is perpendicular to the rotation axis; each group of modules is connected to each other through annular grooves and raised structures, the grooves are located at the feeding end of each module, and the groove width is 1.0mm. The number of groups of modules is adjusted according to the actual situation.
多级的撞击流结构中，当多组微撞击流模块与旋转填料床耦合时，出口处与填料内缘的距离K以及填料厚度δ满足以下关系：In the multi-stage impinging flow structure, when multiple groups of micro impinging flow modules are coupled with the rotating packed bed, the distance K between the outlet and the inner edge of the packing and the packing thickness δ satisfy the following relationship:
δ＝N·W(N＝1,2,3……) (2)δ=N·W (N=1,2,3...) (2)
式中，H为微撞击流模块主体高度；L微撞击流模块主体长度；W为微撞击流模块主体宽度；d为撞击通道的通径；I为进料通道间距；α为微撞击流模块出料口的角度；K为出料口末端与填料内缘的距离；δ为填料厚度；N为微撞击流模块组数。In the formula, H is the height of the main body of the micro-impact flow module; L is the length of the main body of the micro-impact flow module; W is the width of the main body of the micro-impact flow module; d is the diameter of the impact channel; I is the distance between the feed channels; The angle of the discharge port; K is the distance between the end of the discharge port and the inner edge of the filler; δ is the thickness of the filler; N is the number of micro-impact flow modules.
多组微撞击流模块组成的装置主要采用连续操作方式。The device composed of multiple groups of micro-impact flow modules mainly adopts the continuous operation mode.
本发明提供了一种化工混合/反应装置，主要针对液-液快速反应体系，既可与旋转填料床耦合用作预混合及分布器，亦可单独用作规模化制备功能材料的反应器。本发明带来的有益效果：The invention provides a chemical mixing/reaction device, which is mainly aimed at a liquid-liquid rapid reaction system, which can be used as a premixer and distributor by being coupled with a rotating packed bed, and can also be used alone as a reactor for large-scale preparation of functional materials. Beneficial effects brought by the present invention:
(1)撞击通道的有限空间内形成微撞击流，微观混合效果显著提升，与旋转填料床联用后，能进一步提升设备的微观混合性能；(1) The micro-impact flow is formed in the limited space of the impact channel, and the micro-mixing effect is significantly improved. After being used in combination with the rotating packed bed, the micro-mixing performance of the equipment can be further improved;
(2)流体的微小波动不会影响设备的运行状况，设备的稳定性提高，同时液滴飞溅腐蚀程度降低，设备清理、维护便利；(2) The slight fluctuation of the fluid will not affect the operation of the equipment, the stability of the equipment is improved, and the degree of droplet splashing corrosion is reduced, and the equipment is easy to clean and maintain;
(3)装置结构简单，容易实现并行放大，单独用作混合、反应设备时，可制备超细/纳米功能材料。(3) The structure of the device is simple, and it is easy to realize parallel amplification. When used alone as a mixing and reaction equipment, ultra-fine/nano functional materials can be prepared.
附图说明Description of drawings
图1为本发明并列式微撞击流混合装置结构的立体结构图；Fig. 1 is the three-dimensional structure diagram of the structure of the parallel micro-impingement flow mixing device of the present invention;
图2为本发明微撞击流模块的立体结构图；Fig. 2 is the three-dimensional structure diagram of the micro-impact flow module of the present invention;
图3为本发明微撞击流模块的结构示意图；3 is a schematic structural diagram of a micro-impact flow module of the present invention;
图4为图3中沿A-A线的剖面图；Fig. 4 is a sectional view along line A-A in Fig. 3;
图5为实施例1并列式微撞击流混合装置与旋转填料床组合使用的示意图；5 is a schematic diagram of the combined use of a parallel micro-impingement flow mixing device and a rotating packed bed in Example 1;
图6为实施例1并列式微撞击流-旋转填料床(PMIS-RPB)微观混合性能实验流程图；Fig. 6 is the experimental flow chart of the micro-mixing performance of the parallel micro-impact flow-rotating packed bed (PMIS-RPB) in Example 1;
图7为单级微撞击流(MIS)装置的三维结构图；FIG. 7 is a three-dimensional structural diagram of a single-stage micro impinging flow (MIS) device;
图8为自由撞击流(IS)装置的三维结构图；8 is a three-dimensional structural diagram of a free impinging flow (IS) device;
图9为单级MIS-RPB设备与IS-RPB设备微观混合性能对比图；Figure 9 is a comparison chart of micro-mixing performance between single-stage MIS-RPB equipment and IS-RPB equipment;
图10为实施例3并列式微撞击流反应器(PMISR)制备超细粉体流程图。FIG. 10 is the flow chart of the preparation of ultrafine powder by the parallel micro-impact flow reactor (PMISR) in Example 3. FIG.
图中：1为前置进料模块；2为一级微撞击流模块；3为二级微撞击流模块；4为后置密封模块；5为连杆，6为螺母，7为凹槽，8为进样通道，9为撞击通道，10为出料口，11为第一储液槽，12为泵Ⅰ，13为第一流量调节阀，14为第一流量计，15为产物收集器，16为并列式微撞击流-旋转填料床，17为第二储液槽，18为泵Ⅱ，19为第二流量调节阀，20为第二流量计，21为并列式微撞击流反应器。In the figure: 1 is the pre-feeding module; 2 is the first-level micro-impact flow module; 3 is the second-level micro-impact flow module; 4 is the rear sealing module; 5 is the connecting rod, 6 is the nut, and 7 is the groove, 8 is the injection channel, 9 is the impact channel, 10 is the discharge port, 11 is the first liquid storage tank, 12 is the pump I, 13 is the first flow regulating valve, 14 is the first flow meter, and 15 is the product collector , 16 is the parallel micro-impact flow-rotating packed bed, 17 is the second liquid storage tank, 18 is the pump II, 19 is the second flow regulating valve, 20 is the second flow meter, and 21 is the parallel micro-impact flow reactor.
具体实施方式Detailed ways
下面通过实施例来进一步说明本发明，但不局限于以下实施例。The present invention is further illustrated by the following examples, but is not limited to the following examples.
首先对本发明的结构进行说明，如图1～4所示，一种并列式微撞击流混合装置，包括微撞击流模块2和3、前置进料模块1、后置密封模块4、连接装置；First, the structure of the present invention will be described. As shown in Figures 1 to 4, a parallel micro-impact flow mixing device includes
图1中包括两级微撞击流模块，包括一级微撞击流模块2和二级微撞击流模块3；所述微撞击流模块为长方体结构，内部设有相互平行的进样通道8，在长方体中心处与进样通道8垂直设有撞击通道9，撞击通道9为T型结构，底部连接出料口10；Figure 1 includes a two-stage micro-impact flow module, including a first-stage
所述前置进料模块1的入口为塔式或螺纹结构，内部为直通孔，前置进料模块1出口端连接微撞击流模块入口端，微撞击流模块的末端处通过后置密封模块4密封；后置密封模块4为矩形板；The inlet of the
所述连接装置包括连杆5和螺母6；前置进料模块、微撞击流模块和后置密封模块通过连接装置连接紧固。The connecting device includes a connecting
所述进样通道8的内径为8.0～10.0mm；长度为10.0～20.0mm，通道间距为6.0～10.0mm；所述撞击通道的通径为1.0～2.0mm，撞击通道的长度为6.0～10.0mm。The inner diameter of the
所述前置进料模块1的内径为8.0～10.0mm，长度为50～100mm，入口长管能调节装置在旋转填料床内的空间位置。The inner diameter of the
所述出料口10为渐扩的锥形，其上端与撞击通道9底部连接，内径为1.0～2.0mm，出口处的内径为3.3～5.3mm，锥角为30～45°。The discharge port 10 is a gradually expanding cone, the upper end of which is connected to the bottom of the impact channel 9, the inner diameter is 1.0-2.0 mm, the inner diameter at the outlet is 3.3-5.3 mm, and the cone angle is 30-45°.
所述微撞击流模块前、后端面的四个角上分别设有孔，所述前置进料模块1和后置密封模块4的四个角上与微撞击流模块对应处分别设有相同的孔，连杆5从上述孔中穿过，通过螺母6固定。The four corners of the front and rear surfaces of the micro-impact flow module are respectively provided with holes, and the four corners of the
所述模块采用不锈钢、聚四氟乙烯或聚甲基丙烯酸甲酯中的一种材料制备而成。The module is made of stainless steel, polytetrafluoroethylene or polymethyl methacrylate.
所述前置进料模块与微撞击流模块的衔接处，或两个微撞击流模块的衔接处，通过垫圈密封；在每个模块的进料通道端部设有环形凹槽，出口端出设有凸起结构，凸起与凹槽依次配合连接，垫圈设置在该凹槽内。The joint of the pre-feeding module and the micro-impact flow module, or the joint of the two micro-impact flow modules, is sealed by a gasket; an annular groove is provided at the end of the feeding channel of each module, and the outlet end exits. A convex structure is provided, the convex and the groove are matched and connected in sequence, and the washer is arranged in the groove.
下面通过具体实施例对本发明的实施情况进行说明：Embodiments of the present invention will be described below by specific examples:
实施例1：单级MIS-RPB设备与IS-RPB设备微观混合性能实验研究。Example 1: Experimental study on micro-mixing performance of single-stage MIS-RPB equipment and IS-RPB equipment.
图5示出了本实施例并列式微撞击流混合装置与旋转填料床组合使用的示意图；图5汇总可以看出，所述撞击流模块的出料方向与旋转轴垂直。Fig. 5 shows a schematic diagram of the combined use of the parallel micro-impingement flow mixing device and the rotating packed bed in this embodiment; it can be seen from the summary of Fig. 5 that the discharge direction of the impinging flow module is perpendicular to the rotation axis.
图6示出了本实施例并列式微撞击流-旋转填料床(PMIS-RPB)微观混合性能实验流程图；液体A从第一储液槽11经由泵Ⅰ12、第一流量调节阀13、第一流量计14进入并列式微撞击流-旋转填料床16；液体B从第二储液槽17经由泵Ⅱ18、第二流量调节阀19、第二流量计20进入并列式微撞击流-旋转填料床16；二者在并列式微撞击流-旋转填料床16中实现碰撞、混合、反应。并列式微撞击流-旋转填料床16由电机和变频器控制。Fig. 6 shows the experimental flow chart of the micro-mixing performance of the parallel micro-impingement flow-rotating packed bed (PMIS-RPB) in this embodiment; The
图7为单级MIS装置的三维结构图；7 is a three-dimensional structural diagram of a single-stage MIS device;
图8为IS装置的三维结构图；8 is a three-dimensional structural diagram of an IS device;
本实施例所采用单级MIS与IS装置的特征尺寸相同，区别在于后者的流体撞击区不受壁面约束(见图8)。The feature size of the single-stage MIS used in this embodiment is the same as that of the IS device, the difference is that the fluid impingement zone of the latter is not constrained by the wall (see FIG. 8 ).
具体的操作步骤为：配制碘化物混合液A：取11.241g H3BO3和3.636g NaOH配制成H3BO3/NaOH缓冲液。然后将0.6560g KI加入到缓冲液中，混匀后再加入0.7062g KIO3，用1L的容量瓶定容后得到澄清的A溶液。配制硫酸溶液B：准确称取98％的浓硫酸12.5g，用去离子水分别稀释至氢离子浓度为0.05mol/L的溶液B。混合液A和酸溶液B分别经泵输运到研究设备内，溶液在强烈的撞击作用下进行预混合及分布，后经旋转填料床进一步强化反应过程。设备运行稳定后，收集产物并采用分光光度计测量其在353nm波长处的吸光度，依据Lambert-Beer定律换算获求得离集指数XS值。The specific operation steps are: prepare iodide mixture A: take 11.241g H 3 BO 3 and 3.636g NaOH to prepare H 3 BO 3 /NaOH buffer solution. Then, 0.6560g of KI was added to the buffer solution, and 0.7062g of KIO 3 was added after mixing, and a 1L volumetric flask was used to obtain a clear A solution. Preparation of sulfuric acid solution B: Accurately weigh 12.5 g of 98% concentrated sulfuric acid, and dilute with deionized water to solution B with a hydrogen ion concentration of 0.05 mol/L. Mixed solution A and acid solution B were transported to the research equipment by pump respectively. The solutions were pre-mixed and distributed under the action of strong impact, and then the reaction process was further strengthened by the rotating packed bed. After the equipment was running stably, the product was collected and its absorbance at a wavelength of 353 nm was measured with a spectrophotometer, and the segregation index X S value was obtained by conversion according to the Lambert-Beer law.
如图9，相比于IS-RPB设备，单级MIS-RPB设备在相同Re条件下，XS的值较小，表明其微观混合性能有显著提高。因此，本发明采用了微撞击流进行混合过程的强化。As shown in Figure 9, compared with the IS -RPB device, the single-stage MIS-RPB device has a smaller value of XS under the same Re condition, indicating that its micro-mixing performance is significantly improved. Therefore, the present invention adopts the micro-impact flow to enhance the mixing process.
实施例2：单级微撞击流反应器制备超细掺铁二氧化锰。Example 2: Preparation of ultrafine iron-doped manganese dioxide in a single-stage microimpact flow reactor.
本实施例以单级MIS装置为例进行超细功能材料的制备。In this example, a single-stage MIS device is used as an example to prepare ultra-fine functional materials.
选取FeCl3为掺杂源，配制50mL 0.1mol·L-1含Fe3+离子的KMnO4溶液A，溶液中锰铁配比Mn2+:Fe3+＝20:1；配制50mL 0.15mol·L-1MnSO4溶液B。将两股溶液以1:1的体积流量比，经泵引入到MIS反应器内进行混合、反应，实验条件为常温(25±1℃)，入口体积流量为80L/h。用烧杯收集产物，在磁力搅拌器中继续搅拌30min，真空抽滤、洗涤后，在烘箱中80℃烘干12h。相比于传统搅拌反应器，采用单级微撞击流制备的样品粒径分布更加均匀，平均粒径约为120nm，比传统搅拌方法制备的产物比容量提高15％，循环1000次后比容量衰减10％。Select FeCl 3 as the doping source, prepare 50 mL of 0.1 mol·L -1 KMnO 4 solution A containing Fe 3+ ions, and the ratio of manganese to iron in the solution is Mn 2+ :Fe 3+ =20:1; L - 1 MnSO4 solution B. The two solutions were introduced into the MIS reactor through a pump at a volume flow ratio of 1:1 for mixing and reaction. The experimental conditions were normal temperature (25±1°C), and the inlet volume flow was 80L/h. The product was collected in a beaker, stirred in a magnetic stirrer for 30 min, vacuum filtered, washed, and dried in an oven at 80° C. for 12 h. Compared with the traditional stirring reactor, the particle size distribution of the sample prepared by the single-stage micro-impact flow is more uniform, the average particle size is about 120nm, and the specific capacity of the product prepared by the traditional stirring method is increased by 15%, and the specific capacity decreases after 1000 cycles. 10%.
实施例3：多级微撞击流反应器规模化制备超细掺铁二氧化锰。Example 3: Large-scale preparation of ultrafine iron-doped manganese dioxide in a multi-stage microimpact flow reactor.
本实施例采用多级MIS装置为例进行超细功能材料的制备，流程如图10所示。液体A从第一储液槽11经由泵Ⅰ12、第一流量调节阀13、第一流量计14进入并列式微撞击流反应器21；液体B从第二储液槽17经由泵Ⅱ18、第二流量调节阀19、第二流量计20进入并列式微撞击流反应器21；二者在并列式微撞击流反应器21中实现碰撞、混合、反应。In this embodiment, a multi-stage MIS device is used as an example to prepare ultra-fine functional materials, and the process is shown in FIG. 10 . Liquid A enters the parallel
在实施例2的基础上，采用相同的反应体系以及溶液浓度，将多级MIS装置代替单级MIS装置，通过连续操作的模式，在保证原有材料性能的前提下，扩大超细材料的制备规模，实现功能材料的工业化生产。On the basis of Example 2, using the same reaction system and solution concentration, the multi-stage MIS device was replaced by the single-stage MIS device, and the preparation of ultra-fine materials was expanded under the premise of ensuring the performance of the original material through the continuous operation mode. Scale to achieve industrialized production of functional materials.
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