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WO2017036418A1 - 智能工业化微通道连续反应器 - Google Patents

智能工业化微通道连续反应器 Download PDF

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Publication number
WO2017036418A1
WO2017036418A1 PCT/CN2016/098051 CN2016098051W WO2017036418A1 WO 2017036418 A1 WO2017036418 A1 WO 2017036418A1 CN 2016098051 W CN2016098051 W CN 2016098051W WO 2017036418 A1 WO2017036418 A1 WO 2017036418A1
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Prior art keywords
reaction
microchannel
reaction tube
tube
dimensional
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French (fr)
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张苏明
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Qingdao Ti-Ta-Nb-Zr Successive Reactor Co Ltd
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Qingdao Ti-Ta-Nb-Zr Successive Reactor Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus

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  • the invention relates to the technical field of reaction equipment used in petrochemical, fine chemical, pharmaceutical, plastic, synthetic rubber, paint, food processing and the like. More specifically, it relates to a smart industrialized microchannel that can partially replace the traditional batch production reactor and reactor, greatly reduce the land, workshop area and equipment investment, greatly improve safety and environmental performance, greatly save energy, and greatly improve production efficiency. Continuous reactor.
  • reaction heat energy of the reactor is difficult to be restricted by the structure, and the internal heat is not uniform, especially the dangerous processes such as nitrification, hydrogenation and oxidation, and the safety hazards contained in the pregnancy are more prominent. This is a major problem that has long been difficult to solve.
  • the large-diameter tubular static reactor is a continuous production reactor that uses a fixed, non-loaded or filled pipeline of different physical forms to react with different turbulence generated by the reaction liquid flowing therein.
  • the advantage is that there is basically no backmixing, and the cost is proportional to the flow, length, and space occupied. In order to be able to fully react, the longest tubular static reactor can be several kilometers long;
  • the loop reactor is a reaction liquid which reacts liquid/liquid, gas/liquid, gas/solid/liquid, and is sucked and mixed by a venturi ejector, and then sprayed under the liquid surface of the lower part of the reactor, and thoroughly mixed in the liquid surface.
  • the mixed liquid enters the external tube heat exchanger with the circulation pump at the bottom of the loop reactor for heat exchange, and then returns to the inlet end of the venturi injector, and is mixed with the initial reaction liquid to be recycled to form a loop reaction.
  • the latter part enters the post-processing process as a product, and the other part continues to participate in the cycle.
  • Such a reaction mode is currently applicable to rapid chemical reactions such as nitrification.
  • the advantage is that the heat exchange area of the external heat exchanger can be arbitrarily set, and its defects are also obvious, can not be completely reacted at one time, and form back mixing. Expensive;
  • Corning's high-throughput, microchannel continuous flow reactors have significant advantages over the above reactors: the corresponding flow of reaction liquid enters the reactor, mixing reactions in the internal heart-shaped channel modules, and the fluid undergoes turbulent fine mixing The process of almost no backmixing occurs. The reaction is rapid and thorough, and the solvent can be reduced or not used, so that the product conversion rate, purity, and yield are greatly improved. Due to the rectangular special structure of the "sandwich" sandwich form, the two sides of the reaction microcirculation channel are integrally attached to the heat carrier exchanger, and the heat of reaction is immediately removed. Therefore, this principle is relatively advanced in current chemical reactors.
  • microchannel reactors There are other forms of microchannel reactors at home and abroad, but mature industrial microchannel reactors that can scale up to thousands of tons per year are extremely rare.
  • the object of the invention is to add a three-dimensional microchannel fluid component in the reaction tube, cooperate with high-efficiency thermal energy conduction device, and corresponding peripheral devices such as front, rear and sensing, measurement and control, thereby becoming an efficient and practical intelligent industrialization.
  • Microchannel continuous reactor Liquid/liquid, gas/liquid, gas/solid/liquid homogeneous or heterogeneous reactants, when passing through the internal reaction tube, the liquid in the tube (either a powdered catalyst or a fine bubble) is taken into the tube.
  • the installed three-dimensional microchannel assembly is divided into small micro-channels, and in the micro-channel environment, a highly variable separation, polymerization, re-separation turbulence and mutual mixing are produced, which greatly reduces the mass transfer resistance between the reaction materials. .
  • the heat exchange exchange area between the fluid and the metal tube wall is greatly increased, so that the reaction heat energy can be quickly transmitted through the heat medium and the device, and the corresponding temperature required for each reaction can be precisely controlled.
  • the choice of reactor material can also be fully qualified.
  • the length of the reaction tube can be selected according to the length of the reaction time required in the reactor, and the diameter and the number of the reaction tubes in the reactor are selected according to the flow rate.
  • the present invention provides the following technical solutions:
  • An intelligent industrial microchannel continuous reactor comprising: a housing having a heat carrier inlet and a heat carrier outlet, a raw material inlet, a product outlet, a seal plugged at both ends of the housing, and a reaction for reacting the reaction material a tube, the reaction tube is disposed in the housing, the inner chamber of the reaction tube is a tube tube, the chamber between the shell and the reaction tube becomes a shell side, and the raw material inlet and the product outlet are connected to the tube path
  • the heat medium inlet and the heat medium outlet are in communication with the shell side, wherein the reaction tube is tightly inserted with a three-dimensional microchannel assembly, and the outer surface of the three-dimensional microchannel assembly and the inner surface of the reaction tube
  • microchannels of um/mm (micron or millimeter) that are always penetrated.
  • the three-dimensional microchannel assembly and the reaction tube are “tightly inserted”, which means any gap outside the micro-channel formed by the liquid reaction material not being recessed through the inner wall of the reaction tube and the surface of the three-dimensional microchannel assembly.
  • the microchannel is formed concavely on the outer surface of the three-dimensional microchannel assembly.
  • the micro-shaped channel is curved in any geometric pattern shape.
  • the microchannels are connected to each other.
  • the three-dimensional microchannel assembly is an inner column or an inner sleeve.
  • the reaction tube is an in-line reaction tube or a rotary reaction tube, and the overall shape of the three-dimensional microchannel assembly is matched with the reaction tube.
  • the intelligent industrialized microchannel continuous reactor has the following methods: the liquid/liquid, gas/liquid, gas/solid/liquid materials required for the reaction are intelligently mixed and mixed by the infusion pump and the metering pump of the corresponding pressure and head. After that, they enter the intelligent industrial microchannel continuous reactor. After entering the reaction tube 3 When passing through the three-dimensional microchannel assembly, the reaction material is divided into small (small cross section) by the microchannel 5 regardless of the flow rate, and the microchannel is turbulently entered into the microchannel 5, and is repeatedly mixed and separated again and again. Mix again.
  • the cross-section of the microchannel turbulent flow in the above reaction is extremely small, the flow pattern is converted very quickly, so the mass transfer resistance is extremely low; at the same time, the reaction generates heat energy or absorbs heat energy, even very intensely, and heat energy passes through the reaction tube wall and The heat carrier in the shell process exchanges instantly and quickly.
  • the temperature of the chemical reaction continuously in the tube can be precisely controlled.
  • the liquid phase reaction material passes through the path of the long microchannels 5 (generally 10 times longer than the length of the reaction tube) in the form of microchannel turbulent flow, is collected into the product outlet 9 of the reactor and flows out, and no reaction material is re-contacted. Backmixing of raw materials.
  • the three-dimensional microchannel assembly is an inner sleeve, and a heat medium is flowed in the inner cavity of the inner sleeve.
  • the intelligent industrialized microchannel continuous reactor provided by the invention effectively reduces the mass transfer resistance of the reaction material, shortens the reaction time and reduces the side reaction by inserting the three-dimensional microchannel assembly in the reaction tube; at the same time, passes through the reaction tube The three-dimensional microchannel assembly is inserted, so that the liquid reaction material forms a liquid film in the reaction tube, which is favorable for the reaction material to be thoroughly mixed and fully reacted; the heat generated or required during the reaction is immediately heated by the heat carrier and the reaction tube in the housing. Exchange, effectively improve heat transfer efficiency.
  • FIG. 1 is a schematic structural view of an intelligent industrialized microchannel continuous reactor according to an embodiment of the present invention
  • FIG. 2 is a partial cross-sectional structural view of a reaction tube of an intelligent industrial microchannel continuous reactor according to an embodiment of the present invention (a three-dimensional microchannel assembly is not cut);
  • FIG 3 is a schematic view showing another partial cross-sectional structure of a reaction tube of an intelligent industrial microchannel continuous reactor according to an embodiment of the present invention (the three-dimensional microchannel assembly is not cut);
  • the intelligent industrialized microchannel continuous reactor comprises: a casing having a heat carrier inlet 6 and a heat carrier outlet 7, a raw material inlet 8, and a product outlet 9. a sealing head 2 sealed at both ends of the casing and a reaction tube 3 for reacting the reaction material, the reaction tube is disposed in the casing, and the inner cavity of the reaction pipe 3 is a pipe process, and the casing
  • the cavity between the 1 and the reaction tube 3 becomes a shell side, and the raw material inlet 8 and the product outlet 9 are in communication with the tube path, and the heat carrier inlet 6 and the heat carrier outlet 7 are in communication with the shell side, and are characterized
  • the three-dimensional microchannel assembly 4 is tightly inserted into the reaction tube 3.
  • the outer surface of the three-dimensional microchannel assembly 4 and the inner wall surface of the reaction tube are formed with a plurality of um/mm steps (micrometer or millimeter level). ) The microchannel 5 .
  • the filler since the filler is discrete and amorphous, After long-term use, under the self-weight and other reasons, it will inevitably condense and block the reaction tube, causing the upper and lower airflow of the reaction tube to be impervious and blocked to form liquid flood, and the three-dimensional microchannel assembly 4 solves this problem well.
  • the casing 1 is made of corrosion-resistant material and is suitable for conduction of the required heat carrier; the shape of the casing may be a rectangular parallelepiped or a cylindrical shape, and a cylindrical shape is preferred; the reaction tube 3 can satisfy good thermal conductivity and corrosion resistance.
  • the pressure resistance is strong; the three-dimensional microchannel assembly 4 satisfies the corrosion resistance, and the microchannel 5 has a sufficient body surface area, has good liquid film fluidity, and can always keep the upper and lower airflows transparent.
  • the inner chamber of the reaction tube 3 is a tube process, the chamber between the shell 1 and the reaction tube 3 is a shell side, and the reaction tube 3 is reacted for the reaction material, that is, the reaction material flows through the tube, and the heat carrier flows through the shell side.
  • the diameter and the number of the reaction tubes 3 need to be designed according to actual needs.
  • the inner diameter of the reaction tube should be 6 mm to 16 mm, the number is generally tens to hundreds, and the wall thickness of the reaction tube is It should be 0.5-3.0 mm, but it is not limited to the above range.
  • the material of the reaction tube 3 can be various types of stainless steel, titanium, zirconium, hafnium or its alloys, some atmospheric reactors.
  • the reaction tube which is not required for the heat exchange can also be made of polytetrafluoroethylene, polypropylene, polyethylene, etc., which is not limited in the embodiment of the present invention.
  • the position and quantity of the heat medium inlet 6, the heat medium outlet 7, the raw material inlet 8 and the product outlet 9 are designed and determined according to actual needs.
  • the raw material inlet 8 is located in the housing.
  • the product outlet 9 is located at the top of the casing 1, but it does not mean that only this arrangement method, the material inlet 8 can also be located at the top of the casing 1, at which time the product outlet 9 is located at the bottom of the casing 1, so
  • the embodiments of the present invention are not limited thereto, and the scope of protection of the present application should not be limited by the specific embodiments.
  • the microchannel 5 is formed between the outer surface of the three-dimensional microchannel assembly 4 and the inner wall surface of the reaction tube, that is, the microchannel 5 can be formed on the outer surface of the three-dimensional microchannel assembly 4, or on the inner wall surface of the reaction tube 3. Formed, or in the outer surface of the three-dimensional microchannel assembly 4 and within the reaction tube 3 Processing is performed on the wall surface, but in order to facilitate processing, saving processing technology and processing cost, preferably, the micro-shaped channel is formed concavely on the outer surface of the three-dimensional microchannel assembly, such as by being on the outer surface of the three-dimensional microchannel assembly. The method of engraving is formed. Since the three-dimensional microchannel assembly is tightly coupled to the reaction tube 3, the liquid phase reaction material can only pass through the microchannel 5.
  • the intelligent industrialized microchannel continuous reactor has the following methods: the liquid/liquid, gas/liquid, gas/solid/liquid materials required for the reaction are intelligently controlled by the infusion pump and the metering pump corresponding to the pressure and the head. After mixing, they enter the intelligent industrial microchannel continuous reactor. After entering the reaction tube 3, when passing through the three-dimensional microchannel assembly, the reaction material is divided into small (small cross section) by the microchannel 5 regardless of the flow rate, and the microchannel turbulently enters the microchannel 5 and repeats each other. Mix well, separate again, and mix again.
  • the reaction temperature of the material in the reaction tube can be set by a heat carrier (such as a heat transfer oil) in the shell side.
  • the reactor can accurately control the reaction temperature in industrial production; the liquid phase reaction material passes through the path of the long micro-channel 5 (generally 10 times longer than the length of the reaction tube) in the form of microchannel turbulent flow, and is collected
  • the product exit 9 of the reactor flows out without any back-mixing of the reaction material and subsequent contact with the starting material. It should be noted that whether it is a liquid-liquid, gas-liquid or gas-solid reaction, when the reaction material enters the smart industrialized microchannel continuous reactor, the mixing and pretreatment methods are determined according to the specific conditions and requirements of the reaction.
  • the microchannel In order to extend the path of the microchannel 5, increase the chance of repeated mixing and the surface area of the body, it is preferred that the microchannel is curved in any geometric pattern shape, since the purpose is to satisfy the path of the extended microchannel 5 and to increase repeated separation and confluence. The opportunity is enough, so the micro channel 5 can be designed and processed. There are a myriad of patterns, so the embodiment of the present invention does not limit the specific form of the pattern.
  • the respective microchannels 5 communicate with each other. That is, the microchannels 5 are repeatedly separated and merged.
  • the meeting point may be one or more, and the meeting point may also be at any position in the longitudinal direction of the reaction tube 3, and the micro-shaped channels 5 may meet in a disorderly manner or may regularly meet, such as two or two. Convergence and so on.
  • the intelligent industrialized microchannel continuous reactor provided by the above embodiments preferentially selects a cylindrical intelligent industrialized microchannel continuous reactor for liquid-liquid phase reaction, gas-liquid phase reaction, gas-liquid solid phase reaction, and the cuboid intelligent industrialization
  • the channel continuous reactor is selected for horizontal installation.
  • the three-dimensional microchannel assembly is an inner column or an inner sleeve.
  • the reaction tube is an in-line reaction tube or a rotary reaction tube (ie, the reaction tube is not only a straight tube), and the overall shape of the three-dimensional microchannel assembly is matched with the reaction tube.
  • the material of the three-dimensional microchannel fluid component installed in the reaction tube and the reaction tube are preferably the same material, and the expansion coefficient is the same.
  • the diameter, the number of the reaction tube 3 and the type of the tube can be according to the equipment, the flow rate of the reaction material, the reaction heat conduction requirement, and the easy installation of the corresponding three-dimensional.
  • the microchannel component 4 and the like are determined.
  • the length of the reaction tube is substantially equal to the effective length of the reactor, depending on the time required for the completion of the reaction or the completion of the stage reaction. Therefore, some of the more gradual reactions require an increase in reactor length, or more than two reactors in series, or a rotary reaction tube. Even so, continuous, high efficiency, high yield, low emissions and lower investment and operating costs are superior to any conventional reactor.
  • the intelligent industrial microchannel continuous reactor can set various intelligent functions such as remote data monitoring, automatic sampling, and authorization level control.
  • different lines are processed on the outer wall surface of the reaction tube to increase its inner shell
  • the heat exchange specific surface area provides optimum heat exchange in a relatively compact shell-side space.
  • a heat carrier flows in the inner cavity of the inner sleeve, that is, the heat medium flows both in the shell side and in the inner chamber of the inner sleeve, which can be greatly enhanced. Heat exchange efficiency.
  • the connection between the inner cavity of the inner sleeve and the heat medium inlet 6 and the heat medium outlet 7 is not the essential point of the present application and can be easily realized by using some existing technical means, and thus will not be described.
  • the path lengths of all the micro-channels are the same, especially when the intelligent industrial micro-channel continuous reactor is installed vertically, the material in the tube-side is preferably entered from the bottom under the action of pressure, and is ejected from the top (ie, the raw material inlet 8) It is arranged at the bottom of the casing 1 and the product outlet 9 is arranged at the top of the casing 1 so that the material can be flushed in the pipe course, and simultaneously enters and exits, and the reaction is uniform. If the product gradually thickens as the reaction progresses, it is taken up or down, or horizontally.
  • the intelligent industrialized microchannel continuous reactors provided by the embodiments of the present invention may be used in series or in parallel, or combined and connected with other devices, and are not limited to being used alone.

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Abstract

一种大幅提高安全与环保性能，大幅节能，大幅提高生产效率的智能工业化微通道连续反应器。涉及石油化工、精细化学、制药、塑料、合成橡胶、涂料、食品加工等使用的反应设备技术领域，包括：壳体（1）、原料入口（8）、产物出口（9）、封头（2）和反应管（3），其特征在于：反应管中紧密插装有三维微通道组件（4），三维微通道组件（4）的外表面与反应管（3）内壁面之间形成有若干条始终贯通的um/mm级的微形通道（5）。它大幅降低了反应物料间的传质阻力，可及时迅速传导反应热能，缩短反应时间，减少返混与副反应，减少或免除溶剂使用，安全可靠性高，并可大幅节能减排，增加收率，提高生产效率。

Description

智能工业化微通道连续反应器 技术领域
本发明涉及石油化工、精细化学、制药、塑料、合成橡胶、涂料、食品加工等使用的反应设备技术领域。更具体地说，涉及一种可以部分取代传统间歇生产反应釜和反应器，大幅降低土地、车间使用面积和设备投资，大幅提高安全与环保性能，大幅节能，大幅提高生产效率的智能工业化微通道连续反应器。
背景技术
在石油化工、精细化工，制药、食品加工等生产领域中，对于液/液、气/液、气/固/液的均相、非均相常压，高压反应，聚合反应，通常要用到传统搅拌和反应釜进行反应。但搅拌器及反应釜由于先天结构原因，其传质阻力大，返混等现象难以克服，有时还需要增加溶剂使用量，造成整体反应时间过长，副产物增加，后处理分离困难及三废处理量加大等弊病；同时，反应釜的反应热能受结构限制传导困难，内部受热不均匀，特别是硝化、加氢、氧化等危险工艺其中孕含的安全隐患更为突出。这是一个长期以来难以解决的重大难题。
为此，长期以来国内外各种科研机构和企业进行了大量的理论探讨和实践研究。除了某些工艺可以用到的固定床、流化床、塔板式反应器之外，近些年来，国外公司逐步又推出了釜式串联、大口径管式静态反应器、回路反应器和高通量-微通道连续流反应器，逐步在将传统间歇反应向连续化生产工艺过渡和发展：
釜式串联，是将两个及两个以上反应釜串联使用，使反应液体在其转移过程中逐级搅拌完成反应，达到连续化生产的目的；此装置易于形成返混和局部放热、反应不全的致命缺陷，工程造价及车间占地面积不菲；
大口径管式静态反应器，是利用固定的，不装或者装填不同物理形态填料的管道，使反应液体在其中流动时产生的不同湍流而进行反应的连续化生产反应器。其优点是基本没有返混现象，而造价与流量、长度、占据空间成正比。为了能够充分反应，最长的管式静态反应器可长达数公里；
回路反应器是将液/液、气/液、气/固/液反应的反应液，通过文丘里喷射器将其吸入混合，再喷射于反应器下部液面下，在液面内充分混合，混合料液随着回路反应器底部循环泵进入外置式列管换热器进行热能交换，再返回到文丘里喷射器的入口端，与初始反应料液混合后进行再循环，形成环路反应。而后一部分做为产物进入后处理工序，另一部分继续参与循环。这样的反应方式目前可适用于硝化等快速化学反应。其优点是外接换热器的换热面积可以任意设置，而它的的缺陷也是显而易见，不能一次性反应完全，而且形成返混。造价昂贵；
康宁公司的高通量-微通道连续流反应器，比以上的反应器有显著的优点：相应流量的反应液进入反应器，在内部的心形通道模块中进行混合反应，流体经历湍流细致混合的过程，几乎没有返混现象发生。反应迅速、彻底，还可以减少甚至不使用溶剂，使产品转化率、纯度、收率大幅提高。由于其“三明治”夹层形态的矩形特殊结构，反应微循环通道两面整体贴合于热载体交换器，反应热会被即时移除。所以，该原理是目前化学反应器中较为先进的。但是，由于它采用特种玻璃、特种陶瓷或不锈钢等材质雕刻完成，加工工艺比较复杂，价格极为昂贵，加之原理所限而难以提高 的流量，其连接材料和结构所限还制约了它在高温、高压及中型以上规模工业化生产的普及和应用。
国内外还有其他形式的各种微通道反应器，但是成熟的，可以放大到数千吨/年流量以上的工业化微通道反应器极为罕见。
综上所述，在大型工业化生产中，如何减少化学反应时的传质阻力，及时迅速传导反应热能，缩短反应时间，减少混流与副反应，减少或免除溶剂使用，节能减排，增加收率，提高效率，安全可靠性高，环保清洁，大幅降低投资及运行成本，使用一种效果显著，切实可行，经济实用，易于推广的，能将传统间歇生产反应釜或老式反应器升级为智能工业化微通道连续反应器，是目前本领域技术和操作人员十分期待的。
发明内容
本发明的目的是通过在反应管内加装三维微通道流体组件，配合高效热能传导装置，以及相应的前置、后置及传感、测量、控制等外围设备，成为一种高效实用的智能工业化微通道连续反应器。液/液、气/液、气/固/液均相或非均相反应物，在通过其内部反应管时，管内液态(或是裹挟粉末催化剂，或是裹挟细微气泡)的物料，被管内加装的三维微通道组件分割为细小的微形通道，并在其中的微通道环境中产生强烈多变的分离、聚合、再分离的湍流和相互混合，大幅降低了反应物料间的传质阻力。又由于三维微通道流体组件，将流体与金属管壁间热传导交换面积大大增加，从而可以将反应热能通过载热体和装置迅速进行传导，精确控制各种反应所需相应温度。对于某些需要高压、超高压，高温、低温、超低温、强腐蚀条件下的特殊化学反应，也可以通过反应器材质的选择完全胜任。在实 际应用中，可根据具体反应在反应器内所需停留时间长短选择反应管长度，并根据流量选择反应器中反应管的直径和根数。
为了实现上述目的，本发明提供如下技术方案：
智能工业化微通道连续反应器，包括：具有载热体进口和载热体出口的壳体、原料入口、产物出口、封堵于壳体两端处的封头和用于供反应物料反应的反应管，所述反应管设置于壳体内，所述反应管的内腔为管程，所述壳体与反应管之间的腔体成为壳程，所述原料入口和产物出口与管程相连通，所述载热体进口和载热体出口与壳程相连通，其特征在于：所述反应管中紧密插装有三维微通道组件，所述三维微通道组件的外表面与反应管内壁面之间形成有若干条始终贯通的um/mm级(微米或毫米级)的微形通道。此处需要说明的是三维微通道组件与反应管“紧密插装”，是指液相反应物料无法通过反应管内壁与三维微通道组件表面凹陷形成的微形通道以外的任何缝隙。
在上述技术方案基础上，所述微形通道在三维微通道组件的外表面上凹陷地形成。
在上述技术方案基础上，所述微形通道为弯曲的任意几何图案形状。
在上述技术方案基础上，各微形通道之间相连通。
在上述技术方案基础上，所述三维微通道组件为内柱或内套管。
在上述技术方案基础上，所述反应管为直排反应管或回转反应管，所述三维微通道组件的整体形状与反应管相配适。
本发明提供的智能工业化微通道连续反应器的使用方法为：将反应所需液/液、气/液、气/固/液物料，用相应压力、扬程的输液泵、计量泵经智能控制混合后分别打入智能工业化微通道连续反应器。进入反应管3后在 通过三维微通道组件时，反应物料无论流量大小均会被微形通道5分割为细小的(横截面小)、剧烈地微通道湍流进入微形通道5中，并相互反复充分混合、再分离、再混合。由于上述反应中的微通道湍流横截面极小，流动形态转换很快，因此传质阻力极低；同时，反应会产生热能或者吸收热能，甚至是十分剧烈地，而热能会通过反应管壁与壳程内的热载体进行即时、迅速的交换。同时通过智能调整热载体温度、流量即可精确控制管程内连续进行的化学反应温度。液相反应物料以微通道湍流形态经过漫长的微形通道5的路径(一般为反应管长度的10倍以上)，汇集到反应器的产物出口9并流出，不会出现任何反应物料再接触初始原料的返混现象。
在上述技术方案基础上，所述三维微通道组件为内套管，内套管的内腔中流动有载热体。
在上述技术方案基础上，所有微形通道的路径长度相同。
本发明提供的智能工业化微通道连续反应器，通过在反应管内插装三维微通道组件，有效减小了反应物料的传质阻力，缩短了反应时间，减少了副反应；同时，通过在反应管内插装三维微通道组件，使得液相反应物料在反应管内形成液膜，有利于反应物料充分混合以及充分反应；反应过程中产生或所需的热量通过壳体内的热载体与反应管进行即时热交换，有效提高了传热效率。它具有如下优点：大幅降低了反应物料间的传质阻力，可及时迅速传导反应热能，缩短反应时间，减少返混与副反应，减少或免除溶剂使用，节能减排，增加收率，提高生产效率，安全可靠性高，环保清洁，能够大幅地降低投资及运行成本。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍。显而易见地，下面描述中的附图仅仅是本发明的一种实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据提供的附图引伸获得其它的实施附图。
图1为本发明实施例提供的一种智能工业化微通道连续反应器的结构示意图；
图2为本发明实施例提供的一种智能工业化微通道连续反应器的反应管的一种局部剖面结构示意图(三维微通道组件未剖切)；
图3为本发明实施例提供的一种智能工业化微通道连续反应器的反应管的另一种局部剖面结构示意图(三维微通道组件未剖切)；
具体实施方式
下面结合附图和实例对本发明作进一步说明：
如图1和图2所示智能工业化微通道连续反应器，智能工业化微通道连续反应器，包括：具有载热体进口6和载热体出口7的壳体1、原料入口8、产物出口9、封堵于壳体两端处的封头2和用于供反应物料反应的反应管3，所述反应管设置于壳体内，所述反应管3的内腔为管程，所述壳体1与反应管3之间的腔体成为壳程，所述原料入口8和产物出口9与管程相连通，所述载热体进口6和载热体出口7与壳程相连通，其特征在于：所述反应管3中紧密插装有三维微通道组件4，所述三维微通道组件4的外表面与反应管内壁面之间形成有若干条上下贯通的um/mm级(微米或毫米级)的微形通道5。相比在反应管3中加填料，由于填料是离散性的、不定形的， 长时间使用后，在自重等原因下势必会凝积阻塞反应管，造成反应管上下气流不通透、阻塞形成液泛，而三维微通道组件4很好地解决了此问题。
可以理解的是，壳体1为耐蚀材质，适用于所需载热体传导；壳体的形状可为长方体或圆柱体形等，宜选圆柱体形；反应管3能满足良好热传导性、耐蚀、耐压强等条件；三维微通道组件4满足耐蚀，微形通道5有充分的体表面积、具有良好液膜流动性、能始终保持上下气流通透。反应管3内腔为管程，壳体1与反应管3之间的腔体为壳程，反应管3供反应物料在内反应，即反应物料流经管程，载热体流经壳程。对于壳体1的大小、分级与否，反应管3的直径大小和数目需要根据实际需要进行设计，反应管内径宜取6mm～16mm，数量一般为数十至数百根，反应管的壁厚宜为0.5～3.0毫米，但不仅限于以上数量范围，根据反应料液的化学性质不同，反应管3的材质可为各类不锈钢、钛、锆、钽或其合金等材料，一些常压反应器及对热交换要求不高的反应管还可以使用聚四氟乙烯、聚丙烯、聚乙烯等，本发明实施例对此不做限定。
可以理解的是：载热体进口6、载热体出口7、原料入口8和产物出口9的位置、数量均是根据实际需要进行设计、确定的，如1所示，原料入口8位于壳体1的底部，产物出口9位于壳体1的顶部，但并不代表只有这一种布置方法，原料入口8亦可位于壳体1的顶部，此时产物出口9位于壳体1的底部，故本发明实施例对此不做限定，也不应以具体实施例来限制本申请的保护范围。
微形通道5形成于三维微通道组件4的外表面与反应管内壁面之间，即微形通道5可在三维微通道组件4的外表面上加工形成，也可在反应管3的内壁面上加工形成，抑或在三维微通道组件4的外表面及反应管3的内 壁面上均有加工，但为了方便加工，节约加工工艺和加工成本，优选的，所述微形通道在三维微通道组件的外表面上凹陷地形成，如通过在三维微通道组件的外表面上进行刻槽的方法形成。由于三维微通道组件与反应管3紧密结合，故液相反应物料仅可从微形通道5中通过。
本实施例提供的智能工业化微通道连续反应器的使用方法为：将反应所需液/液、气/液、气/固/液物料，用相应压力、扬程的输液泵、计量泵经智能控制混合后分别打入智能工业化微通道连续反应器。进入反应管3后在通过三维微通道组件时，反应物料无论流量大小均会被微形通道5分割为细小的(横截面小)、剧烈地微通道湍流进入微形通道5中，并相互反复充分混合、再分离、再混合。由于上述反应中的微通道湍流横截面极小，流动形态转换很快，因此传质阻力极低；同时，反应会产生热能，甚至是剧烈地放热，热能通过反应管壁可即时、迅速地传导至壳体内的热载体并被吸收交换。同时通过智能调整载热体温度、流量即可精确控制管程内连续进行的化学反应温度。如可以通过壳程中热载体(比如导热油)对反应管内的物料反应温度进行设定。由此，该反应器在工业化生产中可以做到精确控制反应温度；液相反应物料以微通道湍流形态经过漫长的微形通道5的路径(一般为反应管长度的10倍以上)，汇集到反应器的产物出口9处流出，不会出现任何反应物料再接触初始原料的返混现象。需要说明的是，无论是液液、气液或是气固液反应，反应物料在进入该智能工业化微通道连续反应器时，需要根据反应具体条件和要求决定混合和预处理方式。
为了延长微形通道5的路径、增加反复混合机会和体表面积，优选的，所述微形通道为弯曲的任意几何图案形状，由于目的是满足延长微形通道5的路径和增加反复分离和汇合的机会即可，故微形通道5可以设计加工出 无数种图案，故本发明实施例对图案的具体形态不做限定。
如图3所示，为了提高混合效率，优选的，各微形通道5之间彼此相连通。即微形通道5之间反复分离并汇合。可以理解的是汇合点可为一个也可为多个，汇合点也可在反应管3长度方向上任意位置处，微形通道5之间可杂乱地交汇也可有规律地交汇，如两两交汇等。
上述实施例提供的智能工业化微通道连续反应器，对于液液相反应、气液相反应、气液固相反应，优先选择将圆柱型智能工业化微通道连续反应器垂直安装，而长方体智能工业化微通道连续反应器选择水平安装。
优选的，所述三维微通道组件为内柱或内套管。
优选的，所述反应管为直排反应管或回转反应管(即反应管不仅仅为直管这一方式)，所述三维微通道组件的整体形状与反应管相配适。优选的，反应管内加装的三维微通道流体组件材质与反应管宜为相同材质，膨胀系数相同。上述实施例提供的智能工业化微通道连续反应器中，反应管3的直径、根数和管的类型(直排、回转)可根据设备、反应物料流量大小，反应热能传导需要以及易于安装相应三维微通道组件4等条件进行确定。而反应管的长度基本等于反应器的有效长度，取决于充分反应或阶段反应完成所需的时间。因此，某些较为和缓的反应需要增加反应器长度，或者串联2台以上反应器，或者使用回转反应管才能完成。即使这样，连续化、高效率、高收率，低排放和相比较低的投资、运营成本，比之任何一种传统反应器都要优越。
优选的，智能工业化微通道连续反应器可以设置远程数据监测、自动取样、授权级别操控等多种智能化功能。
优选的，反应管外壁面上可以加工有不同纹路，以增加其在壳程内的 热交换比表面积，在相对紧凑的壳程空间内，可达到最佳热交换效果。
当所述三维微通道组件为内套管时，内套管的内腔中流动有载热体，即载热体既在壳程内流动又在内套管的内腔中流动，可大大增强热交换效率。关于内套管的内腔与载热体进口6和载热体出口7间的连接方式非本申请的实质重点且运用现有的一些技术手段即可容易的实现，故不进行赘述。
宜使所有微形通道的路径长度相同，特别是在该智能工业化微通道连续反应器竖直安装时，管程内的物料宜在压力的作用下由底部进入，由顶部射出(即原料入口8设于壳体1的底部，产物出口9设于壳体1的顶部)，如此物料在管程内可齐平运动，同时进入同时导出，反应均匀。如果随着反应进行产物会逐渐增稠的反应，则采取上进下出，或水平安装的方式。
在实际应用过程中，可将本发明实施例提供的智能工业化微通道连续反应器串联或者并联使用，或者与其他设备组合、连接使用，并不局限于单独使用。
对所公开的实施例的上述说明，使本领域技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的原理或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。

Claims (8)

  1. 智能工业化微通道连续反应器，包括：具有载热体进口和载热体出口的壳体、原料入口、产物出口、封堵于壳体两端处的封头和用于供反应物料反应的反应管，所述反应管设置于壳体内，所述反应管的内腔为管程，所述壳体与反应管之间的腔体成为壳程，所述原料入口和产物出口与管程相连通，所述载热体进口和载热体出口与壳程相连通，其特征在于：所述反应管中紧密插装有三维微通道组件，所述三维微通道组件的外表面与反应管内壁面之间形成有若干条始终贯通的um/mm级(微米或毫米级)的微形通道。
  2. 根据权利要求1所述智能工业化微通道连续反应器，其特征在于：所述微形通道在三维微通道组件的外表面上凹陷地形成。
  3. 根据权利要求1或2所述智能工业化微通道连续反应器，其特征在于：所述微形通道为弯曲的任意几何图案形状。
  4. 根据权利要求1所述智能工业化微通道连续反应器，其特征在于：各微形通道之间相连通。
  5. 根据权利要求1所述智能工业化微通道连续反应器，其特征在于：所述三维微通道组件为内柱或内套管。
  6. 根据权利要求1所述智能工业化微通道连续反应器，其特征在于：所述反应管为直排反应管或回转反应管，所述三维微通道组件的整体形状与反应管相配适。
  7. 根据权利要求5所述智能工业化微通道连续反应器，其特征在于：所述三维微通道组件为内套管，内套管的内腔中流动有载热体。
  8. 根据权利要求1所述智能工业化微通道连续反应器，其特征在于：所有微形通道的路径长度相同。
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