CN111434377B - Coil microreactor and microreactor system - Google Patents
Coil microreactor and microreactor system Download PDFInfo
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- CN111434377B CN111434377B CN201910027865.XA CN201910027865A CN111434377B CN 111434377 B CN111434377 B CN 111434377B CN 201910027865 A CN201910027865 A CN 201910027865A CN 111434377 B CN111434377 B CN 111434377B
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Abstract
The invention relates to the field of microreactors, and discloses a coil microreactor and a microreactor system, wherein the coil microreactor comprises a support tube (31) and a microchannel (32) arranged around the support tube (31), at least two fluid redistribution members (341) are arranged in the microchannel (32), one of the fluid redistribution members (341) is arranged at an inlet (36) of the microchannel (32), and the fluid redistribution members (341) are of a cone structure which enables fluid to flow out of the tip of the cone and enter the downstream of the microchannel (32). The invention can prolong the residence time of reactants in a limited reactor volume while ensuring the homogeneous or multiphase raw material mixing effect in the coil pipe microreactor, thereby simultaneously improving the selectivity of products and the conversion rate of raw materials.
Description
Technical Field
The invention relates to the field of microreactors, in particular to a coil microreactor and a microreactor system.
Background
The micro-reactor has obvious advantages in many aspects due to small characteristic size on space, such as large specific surface area, excellent mixing and mass and heat transfer effects, capability of accurately controlling conditions such as reaction time, temperature and the like, green, safe and efficient production and the like.
The micro-reactor is already applied to various petrochemical systems, such as PAO synthesis, liquefied gas desulfurization, Fischer-Tropsch synthesis and hydrogenation processes, has unique advantages in the process of strengthening reaction, and has great industrialization potential.
One fundamental limitation of the development of new technologies using microreactors is that the reaction time must be controlled within a certain range. The micro-reactor is difficult to process and often has higher equipment investment cost, the liquid holdup of the micro-reactor is generally very small, and meanwhile, the feeding speed of reaction raw materials is relatively high, so that the process adopting the micro-reactor generally requires higher reaction speed, otherwise, large-scale production or overhigh investment cost is difficult to realize. And the coil reactor is an effective means for solving the above problems in a limited space.
CN204768602U discloses a microchannel coil reactor, which comprises a temperature adjusting pipe, a microchannel coil and a light source, wherein a first drainage port is arranged on the upper surface of the temperature adjusting pipe, a second drainage port is arranged on the lower surface of the temperature adjusting pipe, the first drainage port is connected with a first drainage pipe, the second drainage port is connected with a second drainage pipe, and a group of annular groove microchannel coils are arranged on the outer wall of the temperature adjusting pipe, embedded in the annular groove and surrounded on the outer wall of the temperature adjusting pipe; the light source is arranged in the central position of the interior of the temperature adjusting pipe. The temperature and illumination of the device are convenient and flexible to adjust, the process can be simplified, the selectivity is improved, the synthesis cost is reduced, and the pollutant emission is reduced. The reactor is suitable for homogeneous reaction process, and for heterogeneous reaction system, especially for gas-liquid phase reaction system, the two phases may not reach good mixing effect.
CN101733056A discloses an impinging stream microchannel reactor, wherein at least two microchannels with equivalent hydraulic diameter of 0.1-2mm are engraved on a flat plate material, and are coaxial or in a certain angle and collide with each other, and an impinging region with width (or collision distance) of 0.5-10mm is formed in the middle of the colliding channel. The technology is suitable for instantly finished reaction process or reaction precipitation process, such as gas-liquid and liquid-liquid rapid reaction for generating liquid or solid (ultrafine powder or nano material and the like). The difficulty of the technology implementation is to uniformly disperse gas-phase and liquid-phase fluids into the colliding microchannels, and a dendritic layer-by-layer grading technical method is adopted to solve the problem, but the processing difficulty of the design is high, and pressure fluctuation at different positions in an impact area is transmitted to each colliding microchannel, so that the fluid distribution in each channel is not uniform.
CN205731200U discloses a Fischer-Tropsch synthesis micro-reactor, which comprises a gas phase inlet, a reaction micro-channel, a heat exchange micro-channel and a product outlet, and adopts a flat-plate micro-channel integration method to solve the problem of gas-liquid phase average distribution in the micro-channel. However, the reactor is more suitable for a Fischer-Tropsch system, the reaction raw material is gas, and when the reactants have two or more gas phases or dispersed phases of liquid phases, the mixing effect is limited.
Disclosure of Invention
One of the objectives of the present invention is to provide a coiled-tube microreactor which can prolong the residence time of reactants in a limited reactor volume while ensuring the homogeneous or multiphase raw material mixing effect in the coiled-tube microreactor, thereby simultaneously improving the selectivity of products and the conversion rate of raw materials.
The invention also aims to provide a micro-reactor system for improving the mixing quality of the multi-phase fluid.
In order to achieve the above object, a first aspect of the present invention provides a coiled-tube microreactor comprising a support tube and a microchannel disposed around the support tube, wherein the microchannel has at least two fluid redistribution means disposed therein, and wherein one of the fluid redistribution means is disposed at an inlet of the microchannel, and the fluid redistribution means is a pyramidal structure which allows a fluid to flow out from a pyramidal tip and into a downstream of the microchannel.
The coil pipe micro-reactor provided by the invention is suitable for effectively mixing multiple strands of miscible or immiscible multiphase raw material mixed solutions and carrying out long-time chemical reaction.
The invention enables the residence time of the fluid in the coiled tube microreactor to be adjusted accordingly by adjusting the length of the microchannel and/or support tube.
According to the invention, the fluid redistribution component is arranged in the microchannel, so that the fluid can be mixed more uniformly, or bubbles and a dispersed liquid phase in the fluid are refined and dispersed in the main phase fluid again.
Preferably, the microchannels are arranged around the support tube in a spiral manner.
The supporting tube can be a hollow structure, a solid structure, a frame structure or a combined structure of one or more of the hollow structure, the solid structure and the frame structure.
Preferably, the tip of the cone of the fluid redistribution means is further provided with a connecting tube, such that the fluid from the tip of the cone enters the connecting tube and then enters the downstream of the microchannel.
Preferably, the cone angle of the cone structure is 10-170 °.
Preferably, the ratio of the inner diameter of the connecting pipe to the inner diameter of the microchannel is 1: (2-50); more preferably 1: (5-20).
The present invention has no special requirements for the specific dimensions of the microchannels in the coiled microreactors, and those skilled in the art can obtain suitable microchannel dimensions according to the actual reaction requirements, for example, the inside diameter of the microchannel can be 0.1-3mm, and the inside diameter of the microchannel is twice the distance from the center of the microchannel to the inner wall, or the diameter of the circular cross section if the inside cross section of the microchannel is circular.
Preferably, the ratio of the inner diameter to the length of the connecting pipe is 1: (0.01-100); more preferably 1: (0.1-10).
The inner diameter of the connection pipe of the present invention may be, for example, 0.05 to 0.5 mm.
Preferably, the support tube is arranged such that there is or is not a height difference between two adjacent microchannel rings formed by microchannels which are wound around a circumference of the support tube.
In order to distribute the redistributed discrete phases (gas-liquid or liquid) in the microchannels more uniformly and to suppress coalescence of the discrete phases, according to a preferred embodiment, the number of the support tubes is at least two, and the arrangement of two adjacent support tubes is such that there is a height difference between the microchannel ring sets on the two adjacent support tubes, which represent a general term for the microchannel rings on the same support tube.
Preferably, the distance between two adjacent microchannel rings formed on the support tube is equal or unequal.
In order to provide the same mixing strength on each section of the support tube and to facilitate the overall design of the process technology, according to a preferred embodiment the distance between two adjacent microchannel rings formed on said support tube is equal.
Preferably, the ratio of the distance between two adjacent microchannel rings to the outer diameter of the support tube supporting the microchannel rings is each independently 1: (1-1000); more preferably 1: (5-200).
According to a preferred embodiment, the number of segments of support tubes is two or more, and the angle between two adjacent segments of support tubes is independently 0-180 °, more preferably 45-135 °. The stay time and the flow of the logistics can be adjusted by adjusting the length and the number of the supporting tubes. Furthermore, the inventor finds that the axial back mixing of the fluid can be reduced and the radial mixing strength can be enhanced simultaneously by making the angle between the adjacent two sections of the supporting tubes be 45-135 degrees and more preferably 80-100 degrees, respectively, so as to improve the selectivity of the target product.
According to a particularly preferred embodiment, each section of support tube is vertically spaced from the other section of support tube.
Preferably, the number of said fluid redistribution elements is such that there is at least one fluid redistribution element in said microchannel surrounding each section of said support tube.
Preferably, at least one outlet is provided on the microchannel to enable fluid to flow out of the coil microreactor.
According to a preferred embodiment, the number of inlets and outlets on the microchannels is such that there is at least one inlet and at least one outlet on each segment of the microchannel surrounding the support tube, and that in the coil microreactor, fluid exiting from an outlet on an upstream microchannel can re-enter a microchannel from an inlet on an adjacent downstream microchannel. The inlet and the outlet of the micro-channel are respectively arranged on each section of the supporting tube, so that the micro-channel on each section of the supporting tube can be selectively connected, and the residence time of the fluid in the micro-channel can be adjusted.
For clarity, the invention defines the most upstream inlet in the coil microreactor as the inlet of the coil microreactor and the most downstream outlet in the coil microreactor as the outlet of the coil microreactor. And the inlet and the outlet of each rest section of the supporting pipe are respectively defined as a product introduction inlet and a product introduction outlet.
Preferably, the microchannel is wound on the outside of the support tube, or the microchannel is a groove embedded in the outer wall of the support tube.
Preferably, the microchannel has an internal cross section of a circle, a regular triangle, a square, a regular pentagon or a regular hexagon.
The coil microreactor can be immersed in a water bath or an oil bath to maintain an isothermal environment, and the supporting tube can also be set as a hollow tube and is used for passing a constant-temperature liquid through the hollow tube to exchange heat with fluid in a microchannel.
A preferred embodiment is provided below using the coiled-tube microreactor of the present invention:
the coil pipe micro-reactor comprises more than two sections of supporting tubes and micro-channels arranged around the supporting tubes, wherein the adjacent two sections of supporting tubes are vertically distributed, a primary reaction product as a raw material enters the micro-channel on the first section of supporting tube through an inlet of the micro-channel, and is led out from a product leading outlet, the direction is changed, then the primary reaction product enters the micro-channel on the second section of supporting tube from the product leading inlet, then the primary reaction product is led out from a product leading outlet of the micro-channel on the second section of supporting tube, the steps are repeated until a reaction product is obtained from an outlet of the micro-channel of the coil pipe micro-reactor, a fluid redistribution component with a cone structure is arranged at the inlet (or the product leading inlet) of the micro-channel on each section of supporting tube, and the cone structure enables fluid to flow out from the tip of the cone and enter the downstream of the micro-channel. The supporting tube and the micro-channel surrounding the supporting tube are arranged inside the shell of the coil micro-reactor, and an internal space formed by the shell of the coil micro-reactor is filled with a material capable of exchanging heat with fluid in the micro-channel.
The coil pipe micro-reactor provided by the invention has the following specific advantages:
1. the device can provide longer residence time for a micro-reactor system, and simultaneously ensure the mixing intensity of multiphase reactants;
2. the coil pipe micro-reactor can replace a conventional reactor, has low liquid storage capacity, and reduces safety risk.
In a second aspect of the present invention, a micro-reactor system is provided, which comprises a two-phase microchannel reactor and a coil micro-reactor, which are sequentially connected, wherein the coil micro-reactor is the coil micro-reactor of the first aspect of the present invention.
The inventor finds that the micro-reactor system provided by the invention can improve the mixing quality of the multi-phase fluid and is easy to be industrially amplified.
According to a preferred embodiment, the two-phase microchannel reactor is provided with a first inlet channel and a fluid distribution member connected to the first inlet channel, the fluid distribution member being arranged in the distribution chamber such that the first material introduced by the first inlet channel can pass through the fluid distribution member into the distribution chamber to contact the second material entering by the first material flow collection chamber, and the distribution chamber communicates with the crude product collection chamber through the reaction microchannels, and the crude product collection chamber communicates with the inlet of the microreactor coil.
The fluid distribution member facilitates the material entering the distribution chamber to be broken up directly into small bubbles or droplets as it passes through the fluid distribution member, thereby facilitating the reaction to proceed more fully. The fluid distribution member may be a sheet of foamed metal or sintered metal.
The present invention has no particular requirement on the cross-sectional area of the reaction microchannel, and those skilled in the art can determine the cross-sectional area of the reaction microchannel suitable for the reaction requirement, and the cross-sectional area of the reaction microchannel of the present invention may be, for example, 0.01 to 90mm2. When the number of reaction microchannels is two or more, the distance between two adjacent reaction microchannels may be, for example, 0.5 to 19 mm.
Preferably, a raw product outlet channel is further arranged in the two-phase microchannel reactor, and the raw product collecting chamber is communicated with the inlet of the coil micro-reactor through the raw product outlet channel.
Preferably, in the two-phase microchannel reactor, the number of the fluid distribution members is at least two, and the adjacent first fluid distribution member and the second fluid distribution member are connected through a connecting piece.
Preferably, a two-phase microchannel reactor shell is further arranged on the two-phase microchannel reactor, and a two-phase microchannel reactor heat exchange fluid inlet channel and a two-phase microchannel reactor heat exchange fluid outlet channel which are respectively used for introducing and leading out heat exchange fluid are arranged on the two-phase microchannel reactor shell.
According to a preferred embodiment, the microreactor system further comprises an impinging stream microchannel mixer disposed upstream of and in communication with the two-phase microchannel reactor.
In the invention, after the material flow is premixed in the impinging stream microchannel mixer, the mixed solution is effectively mixed (homogeneous mixing or heterogeneous mixing) with another material flow (gas phase and/or liquid phase) in the two-phase microchannel reactor and reacts; and the primary product of the reaction flows out of the two-phase microchannel reactor and then enters a subsequent coil pipe micro-reactor for further reaction.
According to a preferred embodiment, the impinging stream microchannel mixer is provided with at least two material conveying units and at least two material flow impinging units, each material conveying unit is communicated with the material flow impinging unit so that the materials in each material conveying unit can enter the material flow impinging unit to be mixed, each material conveying unit comprises a raw material inlet channel, a raw material liquid collecting chamber and a raw material impinging microchannel which are sequentially communicated, so that the raw materials can sequentially flow through the raw material liquid collecting chamber and the raw material impinging microchannel to enter the material flow impinging unit after entering from the raw material inlet channel, and an outlet of the material flow impinging unit is communicated with an inlet of the two-phase microchannel reactor.
Preferably, the raw material liquid collecting chamber is provided with a fluid distribution inner member, and the fluid distribution inner member can enable fluid to uniformly enter the raw material impact micro-channel. The fluid distribution inner member can be provided with a structure such as sieve holes, slits and the like, and can also be made of foam metal or sintered metal.
Preferably, in the impinging-stream microchannel mixer, the ratio of the feed impinging microchannels to the internal diameter of the stream impinging unit is 1: (2-50); more preferably 1: (5-20).
Preferably, in the impinging stream microchannel mixer, the number of the raw material impinging microchannels is one or more.
Preferably, in said impinging stream microchannel mixer, the angle between each of said feed impinging microchannels and said stream impinging unit is independently from 15 to 165 °.
Preferably, the coil pipe microreactor is further provided with a coil pipe microreactor shell, and the coil pipe microreactor shell is provided with a coil pipe microreactor heat exchange fluid inlet and a coil pipe microreactor heat exchange fluid outlet which are respectively used for leading in and leading out heat exchange fluid.
A preferred embodiment is provided below using the microreactor system of the present invention:
the micro-reactor system comprises an impinging stream micro-channel mixer, a two-phase micro-channel reactor and a coil micro-reactor which are sequentially communicated, wherein a plurality of strands of miscible or immiscible liquid-phase raw materials are premixed in the impinging stream micro-channel mixer, the mixed solution is effectively mixed with a gas-phase raw material in the two-phase micro-channel reactor and reacts with the gas-phase raw material, and a primary reaction product obtained by the reaction flows out of the two-phase micro-channel reactor and then enters the subsequent coil micro-reactor for further reaction.
The impinging stream microchannel mixer comprises two material conveying units, namely a first material conveying unit and a second material conveying unit, wherein the first raw material and the second raw material respectively enter the impinging stream microchannel mixer from the first material conveying unit and the second material conveying unit, and are in contact mixing in a material flow impinging unit; in the first material conveying unit and the second material conveying unit, a first raw material and a second raw material respectively and sequentially pass through a raw material inlet channel, a raw material liquid collecting chamber and a raw material impact micro-channel, then enter the material flow impact unit, and obtain a mixed liquid by the material flow impact unit and enter a subsequent two-phase micro-channel reactor.
In the two-phase microchannel reactor, a first material (such as a gas-phase raw material) is introduced into the two-phase microchannel reactor from a first inlet channel, uniformly enters a distribution chamber through a fluid distribution member, and is contacted with a second material (such as a mixed solution obtained by the material flow impacting unit) entering from a first material flow collecting chamber, a reactant flow enters a reaction microchannel from the distribution chamber to react to obtain a primary reaction product, and the primary reaction product then enters a crude product collecting chamber and is led out from a crude product outlet channel to enter a subsequent coil microreactor to further react.
With respect to the specific flow scheme in a coiled-tube microreactor, as described in the detailed description of the first aspect of the present invention, the present invention is not repeated here.
In the microreactor system of the present invention, the impinging stream microchannel mixer is selected depending on whether or not there is a discrete phase of liquid present in the reaction system itself.
The micro-reactor system is suitable for the synthesis process of the poly-alpha-olefin base oil, the process of liquefied gas desulfurization and the like.
The microreactor system of the present invention has the following specific advantages:
1. the micro reactor system is an organic combination of an impinging stream micro-channel mixer, a two-phase micro-channel reactor and a coil micro reactor, is suitable for homogeneous reaction, gas-liquid phase reaction, liquid-liquid phase reaction and gas-liquid multi-phase reaction with reaction gas volume reduced along with time, and strengthens the processes of interphase mass transfer and heat transfer. Through the coupling use of the coil pipe micro-reactor, the reaction time and the reactant feeding speed can be flexibly controlled, and the method is suitable for a system with rapid reaction and relatively low reaction speed.
2. The micro-reactor system has compact structure and small occupied area, can save a large amount of early investment and reduce the operation cost.
3. The micro-reactor system has low liquid storage amount, and reduces safety risk.
Drawings
FIG. 1 is a schematic structural view of a preferred embodiment of a coiled tube microreactor and an enlarged schematic structural view of a fluid redistribution means therein;
FIG. 2 is a schematic diagram of a preferred embodiment microreactor system;
FIG. 3 is a schematic diagram of a preferred embodiment impinging stream microchannel mixer configuration;
FIG. 4 is a schematic diagram of a two-phase microchannel reactor according to a preferred embodiment.
Description of the reference numerals
1. Impinging stream microchannel mixer 2 and two-phase microchannel reactor
3. Coil pipe micro-reactor 11, raw material inlet channel
12. Raw material liquid collecting chamber 13 and raw material impact micro-channel
14. Logistics impact unit 21, first inlet channel
22. First material flow collecting chamber 23, first fluid distribution member
24. Second fluid distribution member 25, reaction microchannel
26. Coarse product collection chamber 27, coarse product outlet channel
281. Heat exchange fluid inlet channel of two-phase microchannel reactor
282. Two-phase microchannel reactor shell
283. Heat exchange fluid outlet channel of two-phase microchannel reactor
29. Connecting piece 291, distribution chamber
31. Support tube 32, microchannel
33. Product inlet outlet 34 and product outlet inlet
341. Fluid redistribution member 35, outlet
36. Inlet 37, coil microreactor housing
38. Coil pipe micro-reactor heat exchange fluid inlet
39. Coil micro-reactor heat exchange fluid outlet
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and these ranges or values should be understood to encompass values close to these ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The structure of a particularly preferred embodiment of a coiled tube microreactor and a microreactor system of the present invention is illustrated below in connection with the schematic structural illustrations provided in FIGS. 1-4.
As mentioned above, the present invention provides a coiled tube microreactor comprising a support tube 31 and a microchannel 32 arranged around said support tube 31, said microchannel 32 being internally provided with at least two fluid redistribution means 341, and one of said fluid redistribution means 341 being arranged at an inlet 36 of said microchannel 32, said fluid redistribution means 341 being of a conical structure which allows fluid to flow out of the tip of the conical structure and into the downstream of said microchannel 32.
Preferably, the tip of the cone of the fluid redistribution member 341 is further provided with a connecting tube 342, so that the fluid enters the connecting tube 342 from the tip of the cone and then enters the downstream of the micro-channel 32.
Preferably, the cone angle of the cone structure is 10-170 °.
Preferably, the ratio of the inner diameter of the connecting pipe 342 to the inner diameter of the microchannel 32 is 1: (2-50); more preferably 1: (5-20).
Preferably, the ratio of the inner diameter to the length of the connecting pipe 342 is 1: (0.01-100); more preferably 1: (0.1-10).
Preferably, the support tube 31 is arranged such that there is or is not a height difference between two adjacent microchannel rings formed by the microchannels 32 that encircle the circumference of the support tube 31.
Preferably, the distance between two adjacent microchannel rings formed on the support tube 31 is equal or unequal.
According to a preferred embodiment, the distance between two adjacent microchannel rings formed on the support tube 31 is equal.
Preferably, the ratio of the distance between two adjacent microchannel rings to the outer diameter of the support tube 31 supporting the microchannel rings is each independently 1: (1-1000); more preferably 1: (5-200).
Preferably, the number of the segments of the support tubes 31 is two or more, and the angles between two adjacent segments of the support tubes 31 are each independently 0 to 180 °, more preferably 45 to 135 °, and still more preferably 15 to 75 °.
Particularly preferably, the number of the fluid redistribution elements 341 is such that at least one fluid redistribution element 341 is present in the microchannels 32 surrounding each section of the support tube 31.
Preferably, the microchannel 32 is provided with at least one outlet 35 to allow fluid to flow out of the coil microreactor.
Preferably, the number of inlets and outlets on the microchannels 32 is such that each section of the microchannels 32 surrounding the support tube 31 has at least one inlet and at least one outlet, and that in the coiled microreactor, the fluid exiting from the outlet on the upstream microchannel 32 can re-enter the microchannel 32 from the inlet on the adjacent downstream microchannel 32.
For clarity, the present invention defines the most upstream inlet in the coil microreactor, i.e., the inlet that is connected to the outlet of a two-phase microchannel reactor, as the inlet of the coil microreactor (i.e., as indicated at 36 in fig. 1), and the most downstream outlet in the coil microreactor as the outlet of the coil microreactor (i.e., as indicated at 35 in fig. 1). The inlet and outlet of the remaining support tube 31 are defined as a product inlet 34 and a product outlet 33, respectively.
Preferably, the micro channel 32 is wound around the outside of the support tube 31, or the micro channel 32 is a groove embedded in the outer wall of the support tube 31.
Preferably, the microchannel 32 has an internal cross-section of a circle, a regular triangle, a square, a regular pentagon or a regular hexagon.
A preferred embodiment of a coiled-tube microreactor to which the present invention may be applied is provided below in conjunction with fig. 1:
the coil pipe micro-reactor comprises more than two sections of support pipes 31 and micro-channels 32 arranged around the support pipes 31, the adjacent two sections of support pipes 31 are vertically distributed, a primary reaction product as a raw material enters the micro-channel 32 on the first section of support pipe through an inlet 36 of the micro-channel, and is led out from a product leading outlet 33, enters the micro-channel on the second section of support pipe from a product leading inlet 34 after changing the direction, and is then led out from a product leading outlet of the micro-channel on the second section of support pipe, the steps are repeated until the reaction product is obtained from an outlet 35 of the micro-channel of the coil pipe micro-reactor, and a fluid redistribution component 341 with a cone structure is arranged at the inlet (or the product leading inlet) of the micro-channel on each section of support pipe, and the cone structure enables the fluid to flow out from the tip of the cone and enter the downstream of the micro-channel. The support tube and the microchannels disposed around the support tube are disposed within a coil microreactor housing 37, and an interior space formed by the coil microreactor housing is filled with a material capable of exchanging heat with a fluid in the microchannels, the material capable of exchanging heat being introduced through a coil microreactor heat-exchange fluid inlet 38 and introduced through a coil microreactor heat-exchange fluid outlet 39.
As mentioned above, the second aspect of the present invention provides a microreactor system comprising a two-phase microchannel reactor 2 and a coiled microreactor 3 connected in series, wherein the coiled microreactor 3 is the coiled microreactor according to the first aspect of the present invention.
According to a preferred embodiment, the two-phase microchannel reactor 2 is provided with a first inlet channel 21 and a fluid distribution member connected to the first inlet channel 21, the fluid distribution member is arranged in the distribution chamber 291 such that the first material introduced from the first inlet channel 21 can pass through the fluid distribution member to enter the distribution chamber 291 to contact the second material introduced from the first stream collection chamber 22, and the distribution chamber 291 communicates with the crude product collection chamber 26 through the reaction microchannels 25, and the crude product collection chamber 26 communicates with the inlet of the coil microreactor.
More preferably, a raw product outlet channel 27 is further provided in the two-phase microchannel reactor, and the raw product collection chamber 26 is communicated with the inlet of the coil microreactor 3 through the raw product outlet channel 27.
Preferably, in the two-phase microchannel reactor 2, the number of the fluid distribution members is at least two, and the adjacent first fluid distribution member 23 and the second fluid distribution member 24 are connected by a connecting member 29.
Preferably, the two-phase microchannel reactor 2 is further provided with a two-phase microchannel reactor shell 282, and the two-phase microchannel reactor shell 282 is provided with a two-phase microchannel reactor heat exchange fluid inlet channel 281 and a two-phase microchannel reactor heat exchange fluid outlet channel 283 for respectively introducing and extracting heat exchange fluid.
According to a preferred embodiment, the microreactor system further comprises an impinging stream microchannel mixer 1, said impinging stream microchannel mixer 1 being arranged upstream of the two-phase microchannel reactor 2 and being in communication with said two-phase microchannel reactor 2.
According to a preferred embodiment, a material conveying unit and a material flow impacting unit 14 are arranged in the impinging stream microchannel mixer 1, the number of the material conveying units is at least two, and each material conveying unit is communicated with the material flow impacting unit 14 so that the material in each material conveying unit can enter the material flow impacting unit 14 to be mixed, each material conveying unit comprises a raw material inlet channel 11, a raw material liquid collecting chamber 12 and a raw material impacting microchannel 13 which are sequentially communicated, so that the raw material can sequentially flow through the raw material liquid collecting chamber 12 and the raw material impacting microchannel 13 to enter the material flow impacting unit 14 after entering from the raw material inlet channel 11, and an outlet of the material flow impacting unit 14 is communicated with an inlet (namely, the first inlet channel 21) of the two-phase microchannel reactor 2.
Preferably, in the impinging stream microchannel mixer 1, the ratio of the inner diameters of the feed impinging microchannels 13 to the stream impinging unit 14 is 1: (2-50); more preferably 1: (5-20).
Preferably, in the impinging stream microchannel mixer 1, the number of the raw material impinging microchannels 13 is one or more.
Preferably, in the impinging stream microchannel mixer 1, the angle between each of the feed impinging microchannels 13 and the stream impinging unit 14 is independently from 15 to 165 °.
Preferably, a coil microreactor housing 37 is further disposed on the coil microreactor 3, and a coil microreactor heat exchange fluid inlet 38 and a coil microreactor heat exchange fluid outlet 39 for respectively leading in and leading out a heat exchange fluid are disposed on the coil microreactor housing 37.
A preferred embodiment of a microreactor system to which the present invention may be applied is provided below in conjunction with FIGS. 2-4:
the micro-reactor system comprises an impinging stream micro-channel mixer 1, a two-phase micro-channel reactor 2 and a coil micro-reactor 3 which are sequentially communicated, wherein a plurality of strands of compatible or incompatible liquid-phase raw materials are premixed in the impinging stream micro-channel mixer 1, then the mixed solution is effectively mixed with a gas-phase raw material in the two-phase micro-channel reactor 2 for gas-liquid mixing and reaction, and a primary reaction product obtained by reaction flows out of the two-phase micro-channel reactor 2 and then enters the subsequent coil micro-reactor 3 for further reaction.
The impinging stream microchannel mixer 1 comprises two material conveying units, namely a first material conveying unit and a second material conveying unit, wherein the first material conveying unit and the second material conveying unit respectively enter the impinging stream microchannel mixer 1 from the first material conveying unit and the second material conveying unit, and the first material and the second material are in contact mixing in the material flow impinging unit; in the first material conveying unit and the second material conveying unit, a first raw material and a second raw material respectively and sequentially pass through a raw material inlet channel 11, a raw material liquid collecting chamber 12 and a raw material impact micro-channel 13, then enter the material flow impact unit 14, and obtain a mixed liquid by the material flow impact unit 14 and enter the subsequent two-phase micro-channel reactor 2.
In the two-phase microchannel reactor 2, a first material (e.g. a gas-phase raw material) is introduced into the two-phase microchannel reactor 2 from a first inlet channel 21, uniformly enters a distribution chamber 291 through a fluid distribution member (sequentially comprising a first fluid distribution member 23 and a second fluid distribution member 24, wherein the first fluid distribution member 23 and the second fluid distribution member 24 are connected by a connecting member 29) to contact with a second material (e.g. a mixed liquid obtained by the aforementioned flow impinging unit) entering from a first flow collecting chamber 22, and a reactant flow enters a reaction microchannel 25 from the distribution chamber 291 to react to obtain a primary reaction product, and the primary reaction product then enters a crude product collecting chamber 26 and is led out from a crude product outlet channel 27 to enter a subsequent coiled microreactor 3 to further react. The two-phase microchannel reactor 2 further includes a two-phase microchannel reactor shell 282, the two-phase microchannel reactor shell 282 defining an interior space that may contain a heat exchange material that is introduced from a two-phase microchannel reactor heat exchange fluid inlet passage 281 and that is withdrawn from a two-phase microchannel reactor heat exchange fluid outlet passage 283.
With respect to the specific flow scheme in the coiled microreactor 3, the present invention is not described in detail herein, as described in the specific embodiments of the first aspect of the present invention.
The present invention will be described in detail below by way of examples.
The product distribution and conversion analyses in the following examples were determined by off-line chromatographic methods using an agilent GC6890-SCD instrument.
The process that takes place in the following examples is the PAO synthesis process, using 1-decene as the polymerization raw material, 1-butanol as the co-catalyst, and BF as the catalyst3。
The conversion in table 1 below was calculated as: the product is cooled to room temperature and transferred to a separating funnel, and after NaOH solution and a small amount of distilled water are added, the mixture is shaken up and stands still. After the water layer is separated out, the pH value of the water layer is detected by using a pH test paper. Repeating the operation until the pH value of the water layer is 7, and standing for a period of time. After all the water is separated out, the water is separated and directly subjected to liquid chromatography analysis. The conversion of the feed was 1-decene concentration in the product/1-decene concentration in the feed.
The selectivity in table 1 below was calculated as: the product is cooled to room temperature and transferred to a separating funnel, and after adding NaOH solution and a small amount of distilled water, the mixture is shaken up and stands still. After the water layer is separated out, the pH value of the water layer is detected by using a pH test paper. Repeating the operation until the pH value of the water layer is 7, and standing for a period of time. Separating after all water is separated out, directly carrying out liquid chromatography analysis, and respectively measuring the concentrations of the monomer, the dimer, the trimer and the tetramer in the product. The selectivity for each product (N-mer) is the concentration of N-mer in the product per feed conversion.
Comparative example 1
The test method comprises the following steps: purging the reaction kettle with nitrogen, adding 20mL of 1-decene into a stainless steel stirred tank reactor, dropwise adding 0.3mL of n-butanol, and introducing BF3And gas bubbling on the liquid surface. The reaction was terminated at 40 ℃ for 4 hours with the reaction pressure maintained at 0.4 MPa.
The conversion and product distribution of the reaction are shown in table 1.
Example 1
This example employed the microreactor system shown in fig. 2 for the sulfur-containing hydrocarbon adsorptive desulfurization process, and the specific configurations of the impinging stream microchannel mixer, two-phase microchannel reactor, and coiled-tube microreactor referred to in fig. 2 are shown in fig. 3, 4, and 1, respectively.
The process flow in this example is as described in the foregoing preferred embodiments of the present invention, and other relevant matters are as follows:
in the impinging stream microchannel mixer 1, the angle between each of the feed impinging microchannels 13 and the stream impinging unit 14 is 90 °; the inner diameter of the raw material impact microchannel 13 is 1mm, and the length is 5 mm; the inner diameter of the material flow impacting unit 14 is 5 mm;
in the two-phase microchannel reactor 2, the cross-sectional area of the reaction microchannel 25 was 1.5mm2The distance between two adjacent reaction microchannels 25 is 5 mm;
in the coiled tube microreactor 3, the outer diameter of the support tube 31 is 30 mm; the inner diameter of the microchannel 32 is 1 mm; on the same supporting tube, the distance between two adjacent micro-channel rings is 2 mm; the angles between two adjacent sections of the supporting tubes 31 are both 90 degrees; the cone angle of the cone structure is 90 degrees; the inner diameter of the connecting pipe 342 is 0.2 mm; the length of the connecting pipe 342 is 1 mm.
1-decene and 1-butanol respectively enter the impinging stream micro-channel mixer 1 from the two raw material inlet channels 11 in fig. 3 and are mixed in the material stream impinging unit 14 to obtain a mixed solution; the mixed liquid enters a first material flow collecting chamber 22 in the two-phase microchannel reactor 2 shown in FIG. 4, and BF3From the first inletThe mixed liquid and the gas-phase catalyst are introduced into the channel 21 to perform a preliminary reaction in the two-phase microchannel reactor 2 to generate a preliminary reaction product, the preliminary reaction product is led out of the two-phase microchannel reactor 2 from the crude product outlet channel 27 and enters the coil microreactor shown in fig. 1 from the inlet 36 to perform a further reaction, and the obtained reaction product is led out from the outlet 35.
The reaction temperature in the test method related to this example was the same as that in comparative example 1, and the pressure was 1.5MPa, and the feed rate of 1-decene was 10mL/min, that of n-butanol was 1mL/min, and BF in this example3The feeding speed of (2) is 40mL/min, and stable product discharge is obtained after reactants are fed for 15min, wherein the product properties are shown in a table 1.
TABLE 1
| Example 1 | Comparative example 1 | |
| Conversion (%) | 93.14 | 90.42 |
| Dimer selectivity (%) | 9.21 | 12.3 |
| Trimer selectivity (%) | 39.31 | 34.92 |
| Tetramer selectivity (%) | 29.5 | 24.33 |
| Pentameric selectivity (%) | 15.41 | 17.95 |
| >Pentameric selectivity (%) | 6.57 | 10.5 |
As can be seen from the results in Table 1, compared with the conventional batch kettle reactor, the technical scheme of the invention can obtain higher raw material conversion rate, and the selectivity of tripolymer and tetramer in the product is obviously superior to that of the batch kettle technology. Besides, the invention can reduce the reaction time from 4h to 15min, and realizes the continuous flow production of PAO.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (29)
1. A microreactor system characterized in that it comprises a two-phase microchannel reactor (2) and a coiled microreactor (3) in serial communication, wherein the two-phase microchannel reactor (2) is provided with a first inlet channel (21) and fluid distribution means connected to the first inlet channel (21), the fluid distribution means being arranged in a distribution chamber (291) such that a first material introduced from the first inlet channel (21) can pass through the fluid distribution means into the distribution chamber (291) to be contacted with a second material introduced from a first stream collection chamber (22), and the distribution chamber (291) communicates with a crude product collection chamber (26) through a reaction microchannel (25), and the crude product collection chamber (26) communicates with the inlet of the coiled microreactor; wherein the first inlet channel (21) and the first stream collection chamber (22) are located on the same side of the distribution chamber (291);
the micro-reactor system also comprises an impinging stream micro-channel mixer (1), wherein the impinging stream micro-channel mixer (1) is arranged at the upstream of the two-phase micro-channel reactor (2) and is communicated with the two-phase micro-channel reactor (2).
2. A microreactor system as claimed in claim 1 wherein the coiled-tube microreactor (3) comprises a support tube (31) and a microchannel (32) arranged around the support tube (31), the interior of the microchannel (32) being provided with at least two fluid redistribution means (341), and wherein one of the fluid redistribution means (341) is arranged at an inlet (36) of the microchannel (32), the fluid redistribution means (341) being of a pyramidal structure which allows fluid to exit from the pyramidal tip and enter downstream of the microchannel (32).
3. A microreactor system according to claim 2 wherein the cone tip of the fluid redistribution means (341) is further provided with a connecting tube (342) such that the fluid from the cone tip enters the connecting tube (342) and then downstream the microchannel (32).
4. A microreactor system according to claim 2 or 3, wherein the cone structure has a cone angle of 10-170 °.
5. A microreactor system according to claim 3, wherein the ratio of the internal diameter of the connecting tube (342) to the internal diameter of the microchannel (32) is 1: (2-50).
6. A microreactor system according to claim 3 wherein the ratio of the internal diameter of the connecting tube (342) to the internal diameter of the microchannel (32) is 1: (5-20).
7. A microreactor system according to claim 3 wherein the connecting tube (342) has an internal diameter to length ratio of 1: (0.01-100).
8. A microreactor system according to claim 3 wherein the connecting tube (342) has an internal diameter to length ratio of 1: (0.1-10).
9. A microreactor system as claimed in claim 2 or 3, wherein the support tube (31) is arranged such that there is or is not a height difference between two adjacent microchannel rings formed by microchannels (32) running around the circumference of the support tube (31).
10. A microreactor system according to claim 9 wherein the distance between two adjacent microchannel rings formed on the support tube (31) is equal or unequal.
11. A microreactor system according to claim 9 wherein the distance between two adjacent microchannel rings formed on the support tube (31) is equal.
12. A microreactor system according to claim 10 or 11 wherein the ratio of the distance between two adjacent microchannel rings to the outer diameter of the support tube (31) supporting the microchannel rings is each independently 1: (1-1000).
13. A microreactor system according to claim 10 or 11, wherein the ratio of the distance between two adjacent microchannel rings to the outer diameter of the support tube (31) supporting the microchannel rings is each independently 1: (5-200).
14. A microreactor system as claimed in claim 2 or 3 wherein the number of stages of support tubes (31) is two or more and the angle between adjacent stages of support tubes (31) is independently 0-180 °.
15. A microreactor system as claimed in claim 14 wherein the angle between adjacent segments of support tubes (31) is independently 45-135 °.
16. A microreactor system as claimed in claim 14 wherein the number of fluid redistribution means (341) is such that at least one fluid redistribution means (341) is present in the microchannel (32) surrounding each section of the support tube (31).
17. A microreactor system according to claim 14 wherein at least one outlet (35) is provided in the microchannel (32) to enable fluid to flow out of the coiled microreactor.
18. A microreactor system according to claim 17 wherein the number of inlets and outlets in the microchannels (32) is such that there is at least one inlet and at least one outlet in each section of the microchannel (32) surrounding the support tube (31) and such that in the coiled microreactor fluid from an outlet in an upstream microchannel (32) can re-enter a microchannel (32) from an inlet in an adjacent downstream microchannel (32).
19. A microreactor system as claimed in claim 2 or 3 wherein the microchannels (32) are arranged wound on the outside of the support tube (31) or the microchannels (32) are recesses embedded in the outer wall of the support tube (31).
20. A microreactor system according to claim 2 or 3 wherein the interior cross-section of the microchannel (32) is circular, regular triangular, square, regular pentagonal or regular hexagonal.
21. A microreactor system according to claim 1 wherein a raw product outlet channel (27) is further provided in the two-phase microchannel reactor, the raw product collection chamber (26) communicating with the inlet of the coiled microreactor (3) through the raw product outlet channel (27).
22. A microreactor system according to claim 1 wherein in the two-phase microchannel reactor (2) the number of fluid distribution members is at least two and adjacent first (23) and second (24) fluid distribution members are connected by a connection (29).
23. The microreactor system of claim 1, wherein a two-phase microchannel reactor housing (282) is further provided on the two-phase microchannel reactor (2), and a two-phase microchannel reactor heat exchange fluid inlet channel (281) and a two-phase microchannel reactor heat exchange fluid outlet channel (283) for introducing and withdrawing a heat exchange fluid, respectively, are provided on the two-phase microchannel reactor housing (282).
24. Microreactor system according to claim 1, wherein a material conveying unit and a stream impinging unit (14) are provided in the impinging stream microchannel mixer (1), the number of material conveying units being at least two, and each material conveying unit is communicated with the material flow striking unit (14) so that the materials in each material conveying unit can enter the material flow striking unit (14) to be mixed, and each material conveying unit comprises a raw material inlet channel (11), a raw material liquid collecting chamber (12) and a raw material impact micro-channel (13) which are sequentially communicated, so that raw materials can sequentially flow through the raw material liquid collecting chamber (12) and the raw material impact micro-channel (13) to enter the material flow impact unit (14) after entering from the raw material inlet channel (11), and the outlet of the stream impact unit (14) is communicated with the inlet of the two-phase microchannel reactor (2).
25. A microreactor system according to claim 24 wherein in the impinging stream microchannel mixer (1) the ratio of the internal diameters of the feedstock impinging microchannel (13) and the stream impinging unit (14) is 1: (2-50).
26. A microreactor system according to claim 24 wherein in the impinging stream microchannel mixer (1) the ratio of the internal diameters of the feedstock impinging microchannel (13) and the stream impinging unit (14) is 1: (5-20).
27. A microreactor system as claimed in any one of claims 24-26 wherein in the impinging stream microchannel mixer (1) the number of feedstock impinging microchannels (13) is more than one.
28. A microreactor system according to claim 27 wherein in the impinging stream microchannel mixer (1) the angle between each of the feedstock impinging microchannels (13) and the stream impinging unit (14) is independently 15-165 °.
29. A microreactor system according to claim 1, wherein a coiled microreactor housing (37) is provided on the coiled microreactor (3), and a coiled microreactor heat exchange fluid inlet (38) and a coiled microreactor heat exchange fluid outlet (39) are provided on the coiled microreactor housing (37) for introducing and withdrawing heat exchange fluid, respectively.
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