WO2017036418A1

WO2017036418A1 - Smart industrial micro-channel flow reactor

Info

Publication number: WO2017036418A1
Application number: PCT/CN2016/098051
Authority: WO
Inventors: 张苏明
Original assignee: 青岛钛钽铌锆连续化反应器有限公司
Priority date: 2015-09-06
Filing date: 2016-09-05
Publication date: 2017-03-09
Also published as: CN105107442A; CN105107442B

Abstract

An smart industrial micro-channel flow reactor that greatly improves the safety and environmental protection performance, saves a lot of energy, and significantly increases production efficiency relates to the technical field of reactor devices used in the petrochemical industry, fine chemistry, pharmacy, plastics, synthetic rubbers, coatings, food processing, and the like, and comprises: a housing (1), a raw material inlet (8), a product outlet (9), a seal head (2), and a reaction tube (3), wherein a three-dimensional micro-channel component (4) is tightly inserted in the reaction tube, and several constantly cut-through micrometer/millimeter-grade micro-channels (5) are formed between the outer surface of the three-dimensional micro-channel component (4) and the inner wall surface of the reaction tube (3). The smart industrial micro-channel flow reactor greatly reduces the mass transfer resistance between reaction mass, can quickly transfer reaction thermal energy in time, reduce the reaction time, reduce backmixing and side reactions, and reduce or avoid use of a solvent, is safe and highly reliable, and can save a lot of energy and significantly reduce emission, increase the yield, and improve the production efficiency.

Description

Intelligent industrial microchannel continuous reactor

Technical field

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.

Background technique

In the fields of petrochemical, fine chemical, pharmaceutical, food processing, etc., for liquid/liquid, gas/liquid, gas/solid/liquid homogeneous, heterogeneous atmospheric pressure, high pressure reaction, polymerization reaction, usually used The reaction is carried out by a conventional stirring and a reaction kettle. However, due to the innate structure of the agitator and the reactor, the mass transfer resistance is large, and the phenomenon of back mixing is difficult to overcome. Sometimes the solvent usage is increased, resulting in an excessive reaction time, increased by-products, difficulty in post-treatment separation, and treatment of three wastes. At the same time, the 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.

To this end, a large number of theoretical research and practical research have been carried out by various scientific research institutions and enterprises at home and abroad for a long time. In addition to fixed-bed, fluidized bed and tray reactors that can be used in some processes, in recent years, foreign companies have gradually introduced tank-type series, large-diameter tubular static reactors, loop reactors and Qualcomm. Volume-microchannel continuous flow reactors, gradually transitioning and developing traditional batch reactions to continuous production processes:

In the tank type, two or more reactors are used in series, so that the reaction liquid is stirred step by step during the transfer process to achieve the purpose of continuous production; the device is easy to form back mixing and local exotherm, and the reaction is incomplete. Fatal defects, project cost and workshop area are very high;

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. However, because it is finished with special glass, special ceramics or stainless steel, the processing technology is more complicated, the price is extremely expensive, and the principle is limited and it is difficult to improve. The flow rate, its connection materials and structure limits also limit its popularity and application in industrial production at high temperature, high pressure and medium scale.

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.

In summary, in large-scale industrial production, how to reduce the mass transfer resistance during chemical reaction, timely transfer reaction heat energy, shorten reaction time, reduce mixed flow and side reactions, reduce or eliminate solvent use, save energy and reduce emissions, increase yield Improve efficiency, safety and reliability, environmental protection and cleanliness, significantly reduce investment and operating costs, use a significant, practical, economical and easy to promote, can upgrade traditional batch production reactor or old-fashioned reactor to intelligent industrialization Microchannel continuous reactors are currently highly anticipated by those skilled in the art and operators.

Summary of the invention

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. . Moreover, due to the three-dimensional microchannel fluid component, 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. For some special chemical reactions that require high pressure, ultra high pressure, high temperature, low temperature, ultra low temperature and strong corrosion conditions, the choice of reactor material can also be fully qualified. In reality In the application, 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.

In order to achieve the above object, 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 There are a number of microchannels of um/mm (micron or millimeter) that are always penetrated. It should be noted here that 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.

Based on the above technical solution, the microchannel is formed concavely on the outer surface of the three-dimensional microchannel assembly.

Based on the above technical solution, the micro-shaped channel is curved in any geometric pattern shape.

Based on the above technical solutions, the microchannels are connected to each other.

Based on the above technical solution, the three-dimensional microchannel assembly is an inner column or an inner sleeve.

Based on the above technical solution, 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 provided by the invention 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. Since 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. At the same time, by precisely adjusting the temperature and flow rate of the heat carrier, 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.

Based on the above technical solution, the three-dimensional microchannel assembly is an inner sleeve, and a heat medium is flowed in the inner cavity of the inner sleeve.

Based on the above technical solutions, the path lengths of all the micro channels are the same.

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. It has the following advantages: it greatly reduces the mass transfer resistance between the reaction materials, can quickly transfer the reaction heat energy, shorten the reaction time, reduce back mixing and side reactions, reduce or eliminate solvent use, save energy and reduce emissions, increase yield, and improve production. Efficiency, safety and reliability, environmentally friendly and clean, can significantly reduce investment and operating costs.

DRAWINGS

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art description will be briefly described below. Obviously, the drawings in the following description are only one embodiment of the present invention, and those skilled in the art can obtain other implementations according to the drawings provided without any creative work. Figure.

1 is a schematic structural view of an intelligent industrialized microchannel continuous reactor according to an embodiment of the present invention;

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);

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);

detailed description

The present invention will be further described below in conjunction with the accompanying drawings and examples:

As shown in FIG. 1 and FIG. 2, the intelligent industrialized microchannel continuous reactor, 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 . Compared to the addition of the filler in the reaction tube 3, 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.

It can be understood that 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. For the size and grading of the casing 1, 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. According to the chemical nature of the reaction liquid, 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.

It can be understood that 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. As shown in FIG. 1, the raw material inlet 8 is located in the housing. At the bottom of 1, 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 provided by the embodiment 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. Since 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, even a violent exotherm, and the heat energy can be instantaneously and rapidly passed through the reaction tube wall. The heat carrier that is conducted into the housing is absorbed and exchanged. At the same time, by precisely adjusting the temperature and flow rate of the heat carrier, the temperature of the chemical reaction continuously in the tube can be precisely controlled. For example, 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. Thus, 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.

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.

As shown in FIG. 3, in order to improve the mixing efficiency, it is preferable that the respective microchannels 5 communicate with each other. That is, the microchannels 5 are repeatedly separated and merged. It can be understood that 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.

Preferably, the three-dimensional microchannel assembly is an inner column or an inner sleeve.

Preferably, 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. Preferably, 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. In the intelligent industrialized microchannel continuous reactor provided by the above embodiment, the diameter, the number of the reaction tube 3 and the type of the tube (straight row, rotation) 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.

Preferably, the intelligent industrial microchannel continuous reactor can set various intelligent functions such as remote data monitoring, automatic sampling, and authorization level control.

Preferably, 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.

When the three-dimensional microchannel assembly is an inner sleeve, 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.

It is preferred that 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.

In an actual application process, 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.

The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments are obvious to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the present invention is not to be limited to the embodiments shown herein, but the scope of the invention is to be accorded

Claims

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 There are a number of microchannels of um/mm (micron or millimeter) that are always penetrated.
The intelligent industrial microchannel continuous reactor of claim 1 wherein said microchannels are recessedly formed on an outer surface of the three dimensional microchannel assembly.
The intelligent industrial microchannel continuous reactor according to claim 1 or 2, wherein the microchannel is curved in any geometric pattern shape.
The intelligent industrial microchannel continuous reactor according to claim 1, wherein each of the microchannels is in communication with each other.
The intelligent industrial microchannel continuous reactor according to claim 1, wherein the three-dimensional microchannel assembly is an inner column or an inner tube.
The intelligent industrialized microchannel continuous reactor according to claim 1, wherein 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 industrial microchannel continuous reactor according to claim 5, wherein the three-dimensional microchannel assembly is an inner sleeve, and a heat carrier is flowed in the inner cavity of the inner sleeve.
The intelligent industrial microchannel continuous reactor of claim 1 wherein all of the microchannels have the same path length.