Multi-channel microreactor and application method thereof
By designing an inlet section, mixing section, reaction section, and outlet section of a multi-channel microreactor, uniform fluid distribution and heat exchange within each channel were achieved, solving the problems of uneven fluid distribution and heat exchange in multiphase flow reaction systems, and improving reaction efficiency and temperature stability.
Patent Information
- Application Number
- CN202410770777.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-06-14
- Publication Date
- 2025-12-16
AI Technical Summary
Existing multi-channel microreactors struggle to achieve uniform fluid distribution and heat exchange in multiphase flow reaction systems, resulting in inconsistent reaction performance and failing to meet industrial application requirements.
A multi-channel microreactor is designed, including an inlet section, a mixing section, a reaction section, and an outlet section. By setting uniformly distributed fluid inlets, mixing channels, reaction channels, and heat exchange channels, the fluid is ensured to be uniformly distributed in each channel, and heat is exchanged in a timely manner through the heat exchange channels to maintain a stable reaction temperature.
It achieves uniform distribution of multiphase flow reaction systems such as gas-liquid, liquid-liquid, gas-liquid-liquid, and gas-liquid-solid, ensuring consistent residence time of the reaction fluid in each channel, avoiding undesirable reaction performance, and improving reaction efficiency and temperature stability.
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Figure CN121130769A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to a multichannel microreactor device and its application method, and more specifically, to a reactor suitable for continuous reactions in gas-liquid, liquid-liquid, gas-liquid-liquid, and gas-liquid-solid systems. Background Technology
[0002] Microreactor technology is an important process intensification technique, characterized by its small size, large specific surface area, high efficiency, and intrinsic safety. Microreactors can eliminate mass or heat transfer resistances in reaction processes, thereby improving reaction efficiency. In practical applications, microreactors often employ tubular channel structures to provide the reaction space, and reactor scale-up typically utilizes a multi-channel parallel scaling-up approach. A key challenge in the industrial application of multi-channel microreactors is achieving uniform fluid distribution, ensuring that the flow within each channel matches the reaction state, and preventing non-ideal conditions such as fluid short-circuiting or uneven distribution. Since actual reaction processes often involve multiphase flow systems such as gas-liquid, liquid-liquid, gas-liquid-liquid, or gas-liquid-solid, achieving uniform fluid distribution in multiphase flow systems using multi-channel microreactors is crucial.
[0003] CN217189486U provides a multi-channel microreactor for manufacturing microdroplets. A sleeve structure is formed within each channel. The continuous phase enters the channel through an annular flow channel formed between the injection tube and the channel, while the dispersed phase enters the channel through an internal injection tube and forms droplets under the action of the continuous phase. Fluid distribution in the multi-channel system employs a multi-way distribution pipe; that is, the fluid enters through an inlet into a distribution pipe connected to each channel, and then enters each flow channel.
[0004] CN102600779A provides a multi-channel reactor with heat exchange function, which consists of a tube bundle composed of multiple heat exchange tubes. The top of the heat exchange tubes is equipped with a hydraulic cavitation element to realize the mixing of liquid and liquid phases and enhance the heat transfer performance of the fluid inside the tube.
[0005] In existing technologies, when multi-channel microreactors are applied to multiphase flow reaction systems, studies on the uniformity of fluid distribution in each channel are mostly concentrated on laboratory scales. The multi-channel fluid distribution structures are often simple plate-type branched structures, making it difficult to guarantee uniform fluid distribution. Furthermore, in practical industrial applications, the reaction process often involves significant heat exchange, thus requiring consideration of the heat exchange function of the multi-channel microreactor. Therefore, a multi-channel microreactor suitable for practical industrial applications should possess the ability to uniformly distribute multiphase flow and facilitate timely heat exchange. Summary of the Invention
[0006] The technical problem to be solved by the present invention is to provide, on the basis of the prior art, a multi-channel microreactor with heat exchange function that is suitable for multiphase flow reaction systems such as gas-liquid, liquid-liquid, gas-liquid-liquid and gas-liquid-solid and its application method.
[0007] In a first aspect, the present invention provides a multi-channel microreactor, comprising an inlet section, a mixing section, a reaction section, and an outlet section connected in sequence; wherein:
[0008] The bottom of the inlet section is provided with a first fluid inlet;
[0009] The mixing section is provided with a mixing channel, the bottom of which passes through the first orifice plate and communicates with the inlet section. The mixing channel has distribution holes on its pipe wall, and the mixing section has a second fluid inlet on its side wall.
[0010] The reaction section is provided with a reaction channel and a heat exchange channel. The bottom of the reaction channel is connected to the mixing channel through a second orifice plate, and the heat exchange medium inlet is connected to the heat exchange medium outlet through the heat exchange channel.
[0011] The outlet section is provided with a top outlet and a bottom outlet that communicates with the reaction channel via a third perforated plate. The outlet section is used to collect materials from multiple reaction channels.
[0012] The multi-channel microreactor provided by this invention is suitable for various multiphase flow reaction systems such as gas-liquid, liquid-liquid, gas-liquid-liquid, and gas-liquid-solid.
[0013] Secondly, the present invention provides a gas-liquid reaction method for the aforementioned multi-channel microreactor. Liquid enters the inlet section through a first fluid inlet, flows upwards, is distributed by a uniform distribution plate, and then enters the mixing channel of the mixing section. Gas enters the mixing section through a second fluid inlet and enters the mixing channel through distribution holes. In the mixing channel, the liquid and gas mix and flow upwards through a second perforated plate into the reaction channel of the reaction section for reaction. The reacted fluid leaves the reaction channel and enters the outlet section, where it collects and is discharged from the multi-channel microreactor through the outlet. The gas-liquid volume ratio is 0.05–100:1, preferably 0.1–40:1. The gas-liquid volume ratio is the volume ratio of gas to liquid under reaction conditions.
[0014] Thirdly, the present invention provides a liquid-liquid reaction method for the above-mentioned multi-channel microreactor. A first liquid enters the inlet section through a first fluid inlet, flows upwards, is distributed through a uniform distribution plate, and then passes through a first perforated plate into the mixing channel of the mixing section. A second liquid enters the mixing section of the reactor through a second fluid inlet and enters the mixing channel through distribution holes to mix with the first liquid. The mixed fluid flows upwards, passes through the first perforated plate, and enters the reaction channel of the reaction section to react. The fluid that has completed the reaction leaves the reaction channel and enters the outlet section, where it collects and is discharged from the reactor through the outlet. The density of the first liquid is greater than that of the second liquid, and the volume ratio of the first liquid to the second liquid is 0.01 to 20:1, preferably 0.1 to 6:1.
[0015] When the multi-channel microreactor provided by this invention is used in a gas-liquid-solid system, the solid can be fixed in the reaction channel to form a bed in the form of a catalyst or internal components, or it can be in the form of nano or micron-sized particles to form a pseudo-homogeneous slurry with the liquid phase and pass through the reactor.
[0016] The beneficial effects of the multi-channel microreactor and its application method provided by this invention are as follows:
[0017] Compared with existing technologies, the multi-channel microreactor provided by this invention, through its special structural design, can achieve uniform distribution of various multiphase flow reaction systems such as gas-liquid, liquid-liquid, gas-liquid-liquid, and gas-liquid-solid, ensuring that the residence time of the reaction fluids in each channel is as consistent as possible, thus avoiding unsatisfactory reaction performance caused by uneven residence time distribution. The provided multi-channel microreactor has timely heat exchange capabilities, with a heat exchange space volume much larger than the reaction channel and mixing channel volume, ensuring stable temperature during the reaction process. The reaction channel is equipped with mixing components, which can enhance mixing and mass transfer during the reaction process, improving reaction performance. Attached Figure Description
[0018] Figure 1 This is a schematic diagram of the multi-channel microreactor structure provided by the present invention.
[0019] Figure 2 This is a side view of the first orifice plate with heat exchange function.
[0020] Figure 3 This is a top view of the first orifice plate structure with heat exchange function.
[0021] Figure 4 This is a schematic diagram of a multi-channel microreactor with multiple reaction sections.
[0022] Figure 5 This is a schematic diagram of the multichannel microreactor structure in Comparative Example 1.
[0023] Figure label:
[0024] 1-Top outlet; 2-First fluid inlet; 3-Outlet section
[0025] 4-Third well plate; 5-Reaction section; 6-Reaction channel
[0026] 7-Baffle plate 8-Inlet section 9-Dispersion components
[0027] 10 - Uniform distribution plate; 11 - Distribution holes; 12, 19 - Heat exchange medium inlet
[0028] 13, 20 - Heat exchange medium outlet; 14 - Second fluid inlet; 15, 16 - Discharge pipe
[0029] 17-First orifice plate 18-Second orifice plate 21-Orifice plate heat exchange piping
[0030] 22-Mixing Section 23-Mixing Channel Detailed Implementation
[0031] The specific embodiments of the present invention are described in detail below.
[0032] In this application, the terms "upper part," "lower part," and "bottom" are all based on the relative positional relationship of the container or component. Specifically, "bottom" refers to the position of the container from bottom to top of 0-10%, and "top" refers to the position of the container from bottom to top of 90-100%.
[0033] In a first aspect, the present invention provides a multi-channel microreactor, comprising an inlet section 8, a mixing section 22, a reaction section 5, and an outlet section 3 connected in sequence; wherein:
[0034] The bottom of the inlet section is provided with a first fluid inlet 2;
[0035] The mixing section is provided with a mixing channel 23, the bottom of which passes through the first orifice plate 17 and communicates with the inlet section. The mixing channel wall is provided with distribution holes 11, and the side wall of the mixing section is provided with a second fluid inlet 14.
[0036] The reaction section is provided with a reaction channel 6 and a heat exchange channel. The bottom of the reaction channel is connected to the mixing channel via a second perforated plate 18. The heat exchange medium inlet 12 is connected to the heat exchange medium outlet 13 via the heat exchange channel.
[0037] The outlet section is provided with a top outlet 1 and a bottom outlet connected to the reaction channel via a third perforated plate 4. The outlet section is used to collect materials from multiple reaction channels.
[0038] Preferably, the inlet section is an inverted conical cylinder with a cone angle of 20 to 150°.
[0039] Preferably, the inlet section is provided with a conical dispersing member 9, the dispersing member is coaxial with the inlet section, and the distance between the bottom of the dispersing member and the bottom of the inlet section is 10-150mm.
[0040] Preferably, an inlet section heat exchange pipeline is provided within the inlet section, and the heat exchange pipeline serves as a heat exchange medium channel.
[0041] Preferably, a distribution plate 10 is provided below the mixing channel, and the distribution plate is made of porous material or a sieve plate structure. Preferably, the distance between the distribution plate and the bottom of the mixing channel is 5-50 mm. The fluid in the inlet section is distributed by the distribution plate and then enters the mixing section.
[0042] In this invention, the mixing section is provided with multiple mixing channels, the cross-section of which can be circular or rectangular, preferably rectangular. Preferably, the cross-sectional area of the mixing channel is 0.1–65 mm². 2 The length is 10 to 500 mm, more preferably 15 to 150 mm.
[0043] Preferably, the mixing channel has an increasing diameter from bottom to top.
[0044] Optionally, the diameter of the distribution holes 11 on the mixing channel is 0.3-5 mm, preferably 0.5-1.5 mm, and the center distance between two adjacent distribution holes along the axial direction of the mixing channel is 5-100 mm, preferably 10-40 mm.
[0045] In this invention, the sidewall of the mixing section is provided with a second fluid inlet, and the distance between the second fluid inlet and the second orifice plate is 5-100 mm; preferably, the mixing section is provided with a heat exchange tube or a shell heat exchange structure, and the heat exchange shell is provided with a heat exchange medium inlet and a heat exchange medium outlet.
[0046] In this invention, the mixing channels of the mixing section and the reaction channels of the reaction section are connected in a one-to-one correspondence. There are at least two reaction channels and mixing channels, and the distance between adjacent reaction channels is 1 to 50 mm, preferably 3 to 30 mm. The cross-sectional area of the reaction channels is 0.1 to 65 mm². 2 The length is 50–20000 mm, preferably 100–6000 mm. Preferably, internal components are provided within the reaction channel. These internal components are used to enhance the mass and heat transfer processes of the fluid.
[0047] In this invention, the reaction section is provided with a reaction channel and a heat exchange channel, and the volume ratio of the heat exchange channel to the reaction channel in the reaction section is 2 to 50:1, preferably 5 to 30:1.
[0048] Preferably, the heat exchange channel of the reaction section is provided with multiple baffles, and the distance between two adjacent baffles is 100-600 mm.
[0049] Preferably, the first orifice plate and / or the second orifice plate contain heat exchange pipes.
[0050] In this invention, the height of the outlet section is less than 15cm; preferably, the bottom sidewall of the outlet section is also provided with a second outlet.
[0051] Optionally, the reaction section is divided into at least two sections, which are connected by an inter-section perforated plate.
[0052] The multi-channel microreactor provided by this invention can be used for reaction processes in multiphase flow systems such as gas-liquid, liquid-liquid, gas-liquid-liquid, or gas-liquid-solid.
[0053] In this invention, the inlet section is used to contain the first fluid and distribute it into the mixing channels. The inlet section can be a cylindrical body with a smooth bottom or an inverted conical body. In a preferred embodiment, the inlet section 8 is an inverted conical body, preferably with a cone angle of 20 to 150°. The inverted conical body allows the fluid flow to gradually stabilize and flow upwards into the mixing section, where it is evenly distributed into each mixing channel.
[0054] In a preferred embodiment, a dispersing component is provided within the inlet section. The dispersing component is coaxial with the inlet section and located above the first fluid inlet. The distance between the bottom of the dispersing component and the top of the first fluid inlet is 10–150 mm. The dispersing component adopts a porous plate, porous medium, or a dispersed particle layer structure, and can be conical, frustum-shaped, or similar shapes. The dispersing component can uniformly distribute the fluid entering the inlet section from the first fluid inlet, avoiding a situation where the flow velocity is high at the center and low at the wall, allowing the fluid passing through the dispersing component to flow with a relatively uniform velocity distribution before entering the mixing section.
[0055] In this invention, a heat exchange pipeline may or may not be provided within the inlet section. Besides the first fluid inlet at the bottom, the inlet section may also include other fluid inlets. In a preferred embodiment, a heat exchange pipeline is provided within the inlet section, serving as a heat exchange medium channel, and includes a heat exchange medium inlet and a heat exchange medium outlet.
[0056] In this invention, the inlet section and the mixing section are connected. In a preferred embodiment, a distribution plate is provided at the bottom of the mixing section. The fluid in the inlet section flows upward and is distributed by the distribution plate before entering the mixing section, making the fluid distribution in the mixing channel more uniform and avoiding a situation where the flow velocity is high in the center and low at the wall inside the mixing channel. The distribution plate can be a porous plate, porous media, corrugated packing, grid packing, or a particle bed, as well as combinations of the above.
[0057] In this invention, the mixing section is provided with multiple mixing channels, each with an opening at the bottom and distribution holes on its wall. After entering the mixing section, the fluid flows into the mixing channels through these distribution holes. Preferably, the cross-sectional area of the mixing channels is 0.1–65 mm². 2 The length is 10–500 mm; in a preferred embodiment, the cross-sectional area of the mixing channel is 0.1–65 mm². 2 The length is 15-150mm.
[0058] In this invention, the cross-section of the mixing channel is circular or rectangular. In one embodiment, the mixing channel is a circular tube with a constant diameter. In a preferred embodiment, the cross-section of the mixing channel is rectangular, with an aspect ratio of 0.1 to 15:1, preferably 0.5 to 10:1. A rectangular channel can reduce the characteristic dimensions of the mass transfer or heat transfer process, thereby improving the corresponding mass transfer or heat transfer performance.
[0059] The mixing channel is a straight pipe or a variable-diameter cylinder that expands from bottom to top. In a preferred embodiment, the mixing channel has an ever-increasing diameter, forming a tapered tube with a gradually expanding cross-sectional area, which effectively reduces the possibility of bubble or droplet aggregation and maintains a highly dispersed state of the dispersed phase.
[0060] In the application of the multi-channel microreactor of this invention, the fluid inside the mixing section exhibits stratification, with the fluid distribution from top to bottom being gas and liquid, or alternatively gas, a less dense liquid, and a more dense liquid. Higher fluid flow velocities within the mixing channels result in stronger shearing action on the dispersed phase fluid flowing in through the distribution holes, producing smaller bubbles or droplets and achieving better mixing with the continuous phase fluid. The higher fluid flow velocity also suppresses the coalescence of bubbles and droplets, enhancing the mixing between the dispersed and continuous phase fluids.
[0061] In this invention, a second fluid inlet is provided on the sidewall of the mixing section. Preferably, the distance between the second fluid inlet and the orifice plate above it is 5 to 100 mm.
[0062] In one specific embodiment, the inlet section, mixing section, and orifice plate of the reactor can all have heat exchange functions, enabling timely heat exchange and maintaining a stable reaction temperature. Heat exchange piping can be installed inside the inlet section, and a heat exchange shell can be installed in the mixing section. If the reaction system does not react at room temperature or lower temperatures, a heat exchange shell is not required in the mixing section.
[0063] In this invention, the mixing channels in the mixing section are connected to the reaction channels in the reaction section in a one-to-one correspondence. The mixing channels and reaction channels have the same cross-sectional area, which is 0.1–65 mm². 2 The cross-sectional shape of the reaction channel can be rectangular or circular. In this invention, the length of the reaction channel is 50–20000 mm, preferably 100–6000 mm. The distance between two adjacent reaction channels is 1–50 mm, preferably 3–30 mm.
[0064] In this invention, the reaction channel is an empty tube, or it may contain internal components or catalyst particles. The reaction channel may contain plate-shaped, porous, granular, corrugated, or grid-shaped internal components, or combinations thereof. The internal components enhance the mixing, mass transfer, and heat transfer processes of the fluid within the reaction channel, promoting the reaction process and promptly transferring heat to the channel walls. Heat exchange is also facilitated with the heat exchange medium inside the reaction section shell to maintain a stable reaction temperature. A catalyst bed is filled within the reaction channel to provide catalytic functionality and accelerate the reaction process.
[0065] In this invention, the outlet section has at least one outlet. In one embodiment, an outlet is located at the top of the outlet section, and the first and second fluids after the reaction are discharged from the reactor together through the top outlet. In another embodiment, an outlet is located at the top of the outlet section, and a second outlet is located on the bottom sidewall of the outlet section. The top outlet and the second outlet discharge different fluids respectively. In this case, the multiphase flow undergoes phase separation inside the outlet section. The top outlet is located above the phase interface and mainly discharges gas or light phase, while the second outlet is located below the phase interface and mainly discharges liquid or heavy phase. By using two outlets and utilizing fluid phase separation, the function of a separation device is integrated, which can avoid the problem of over-reaction caused by excessive contact time of multiphase flow.
[0066] The multi-channel microreactor provided by this invention can be used in reaction processes of multiphase flow systems such as gas-liquid, liquid-liquid, gas-liquid-liquid, or gas-liquid-solid. When used in gas-liquid-solid systems, the solid can be fixed in the reaction channel to form a bed in the form of a catalyst or internal components, or it can be in the form of nano- or micron-sized particles to form a pseudo-homogeneous slurry with the liquid phase and pass through the reactor. It is understood that when used in gas-liquid-liquid or gas-liquid-solid systems, the above-mentioned gas-liquid volume ratio and liquid-liquid volume ratio are still applicable.
[0067] The multi-channel microreactor provided by this invention is preferably placed vertically, which is beneficial for the uniform distribution of bubbles or droplets formed in the multiphase flow system within each channel.
[0068] Depending on the characteristics of the actual reaction, the reaction section can be set up in one or more series. The orifice plates connecting adjacent reaction sections can be equipped with heat exchange functions to facilitate timely heat exchange. Multiple reaction sections connected in series can be individually supplied with heat exchange media, allowing different reaction sections to have different reaction temperatures, thereby further enhancing reaction performance. Alternatively, the same heat exchange medium can flow sequentially through multiple reaction sections. The fluid flowing out of the reaction channel enters the outlet section and exits the reactor from the outlet. A shorter outlet section can suppress undesirable flow conditions such as flow deviation and vortices in the multiphase flow, and can also minimize the fluid residence time.
[0069] Secondly, the present invention provides a method for gas-liquid reaction using a multi-channel microreactor. Liquid enters the inlet section through a first fluid inlet, flows upwards, is distributed by a uniform distribution plate, and then passes through a first perforated plate into the mixing channel of the mixing section. Gas enters the mixing section through a second fluid inlet and enters the mixing channel through distribution holes. In the mixing channel, the liquid and gas mix and flow upwards through the first perforated plate into the reaction channel of the reaction section for reaction. The reacted fluid leaves the reaction channel and enters the outlet section, where it collects and is discharged from the reactor through the outlet. The gas-liquid volume ratio is 0.05–100:1, preferably 0.1–40:1. The gas-liquid volume ratio refers to the volume ratio of gas to liquid under reaction conditions.
[0070] Thirdly, the present invention provides a method for liquid-liquid reaction using a multi-channel microreactor. A first liquid enters the inlet section through a first fluid inlet, flows upwards, is distributed by a uniform distribution plate, and then enters the mixing channel of the mixing section. A second liquid enters the mixing section of the reactor through a second fluid inlet and enters the mixing channel through distribution holes to mix with the first liquid. The mixed fluid flows upwards through a first perforated plate and enters the reaction channel of the reaction section to react. The fluid that has completed the reaction leaves the reaction channel and enters the outlet section, where it collects and is discharged from the reactor through the outlet. The density of the first liquid is greater than that of the second liquid, and the volume ratio of the first liquid to the second liquid is 0.01–20:1, preferably 0.1–6:1.
[0071] In the specific implementation process, the first fluid enters the inlet section of the reactor through the first fluid inlet at the bottom of the reactor, and then enters the mixing channel through the first orifice plate. The second fluid enters the mixing section through the second fluid inlet with openings in the side wall of the mixing section, and then enters the mixing channel through distribution holes. Inside the mixing channel, the second fluid, as the dispersed phase, is dispersed into bubbles or droplets by the first fluid, which is the continuous phase, and mixes thoroughly with the first fluid. Then, it moves upward, passes through the second orifice plate, and enters the reaction channel. Because the mixing channel is relatively short, the thermal effect is not significant, and it has little impact on the overall reaction result. A heat exchange function can also be added to the mixing section to ensure that the temperature of the two fluids remains stable after mixing. The fluid entering the reaction channel continues to move upward, allowing for thorough reaction. Internal components that promote fluid mixing can be installed inside the reaction channel to enhance the mixing, mass transfer, and heat transfer processes. Furthermore, a bed with catalyst function can be installed inside the reaction channel to catalyze the reaction process. The reaction section is equipped with a heat exchange channel, thus forming a tube side for reaction and a shell side for heat exchange. Preferably, baffles are installed inside the shell side to enhance the heat exchange process and maintain a stable reaction temperature. When the reactor is shut down, the heat exchange medium can be emptied through the heat exchange medium inlet, or a heat exchange medium discharge pipe can be installed at the bottom of the heat exchange channel to discharge the heat exchange medium.
[0072] The gas-liquid mixture within the outlet section can flow out through the top outlet. If a second outlet is located at the bottom of the sidewall of the outlet section, the gas primarily flows out through the top outlet, while the liquid primarily flows out through the second outlet on the sidewall.
[0073] The multi-channel microreactor provided by this invention, when used in continuous multiphase flow reaction processes such as gas-liquid, liquid-liquid, gas-liquid-liquid, or gas-liquid-solid, achieves uniform distribution of fluids, especially dispersed phase bubbles and droplets, through a special structural design, ensuring the consistency of the reaction process within each channel. The multi-channel microreactor provided by this invention can be used in hydrogenation, oxidation, or other reaction processes involving continuous multiphase flow synthesis of fine chemicals and additives.
[0074] The specific embodiments of the present invention are described below with reference to the accompanying drawings. However, the present invention is not limited thereto.
[0075] Figure 1 A schematic diagram of the structure of the multi-channel microreactor provided by this invention is attached. Figure 1 As shown, the multi-channel microreactor comprises, from bottom to top, an inlet section 8, a mixing section 22, a reaction section 5, and an outlet section 3, all interconnected. The inlet section 8 has a first fluid inlet 2 at its bottom, and a dispersing component 9 above it. The mixing section 22 contains multiple mixing channels 23, the bottom of which passes through a first perforated plate 17 and communicates with the inlet section 8. Distribution holes 11 are provided on the walls of the mixing channels. A distribution plate 10 is provided at the junction of the mixing section 22 and the inlet section 8. This distribution plate can be a porous plate, porous media, corrugated packing, grid packing, or a granular bed, or a combination of these. The distribution plate is located below the bottom opening of the mixing channels. Fluid from the inlet section is distributed through the distribution plate before entering the mixing section, preventing uneven distribution of the continuous phase fluid in different mixing channels.
[0076] The reaction section 5 has a shell-and-tube structure, with the tube side serving as the reaction channel and the shell side as the heat exchange channel. Multiple reaction channels 6 and heat exchange channels are provided within the reaction section 5. The reaction channels are connected to and correspond one-to-one with the mixing channels. The bottom of each reaction channel is connected to the mixing channel via a second orifice plate 18. Baffles 7 are provided within each heat exchange channel, and each heat exchange channel has a heat exchange medium inlet 12 and a heat exchange medium outlet 13. The bottom of the outlet section 3 is connected to the reaction channels via a third orifice plate 4. The outlet section is used to collect materials from the multiple reaction channels, and a top outlet 1 is provided at the top of the outlet section.
[0077] Appendix Figure 2 , 3 These are side and top views of an orifice plate with heat exchange function. The orifice plate is internally equipped with heat exchange pipes 21, which have a heat exchange medium inlet 19 and a heat exchange medium outlet 20. This allows for timely heat exchange and maintains a stable reaction temperature.
[0078] Appendix Figure 4 This is a schematic diagram of a multi-channel microreactor with multiple reaction sections. Reaction section 5 is at least one section, but multiple sections can be connected in series. The sections are connected by inter-section perforated plates. The temperatures of different reaction sections can be the same or different. Each reaction section can be circulated with a separate heat exchange medium, or they can be connected in series and circulated with the same heat exchange medium. Since the actual reaction process is quite complex, different reaction temperatures are often set at different stages of the reaction to improve the overall reaction performance. Therefore, when setting multiple reaction sections, the temperature of different reaction sections can be controlled according to the actual reaction characteristics. Specifically, different reaction sections can be circulated with separate heat exchange media, without sharing the same heat exchange medium. Alternatively, the same heat exchange medium can be used to pass through the shell side of each reaction section sequentially.
[0079] The application method of the multi-channel microreactor provided by this invention involves introducing a liquid, slurry, or gas-liquid mixture into the first fluid inlet 2, preferably a liquid or slurry, and introducing a gas, liquid, slurry, or gas-liquid mixture into the second fluid inlet 14, preferably a gas. The first fluid enters the inlet section, is evenly distributed by the distribution plate 10, and then passes through the first perforated plate 17 into the mixing channel 23. The second fluid enters the mixing section and then enters the mixing channel through the distribution holes 10. The two fluids mix within the mixing channel 23, where the first fluid, as the continuous phase, disperses the second fluid, as the dispersed phase, into a highly dispersed system such as bubbles or droplets, thereby increasing the interphase surface area and enhancing mass transfer and the reaction process.
[0080] The mixture flows through the second orifice plate into the reaction channel to continue the reaction. A heat exchange medium is introduced into the heat exchange channel to exchange heat promptly and maintain a stable reaction temperature. The heat exchange channel is equipped with at least one baffle 7 to enhance the turbulence and heat transfer performance of the heat exchange fluid in the shell side. To ensure sufficient heat exchange in the reaction section 5, the volume ratio of the heat exchange channel to the reaction channel 6 is 2–50:1, preferably 5–30:1. The volume of the heat exchange channel is larger than that of the reaction channel, which is beneficial for maintaining the reactor temperature stability using the heat exchange medium. (Appendix) Figure 1 In the reactor, a heat exchange medium discharge pipe 15 is provided at the bottom of the reaction section 5 to facilitate the timely venting of the heat exchange medium in the shell side when the reactor stops operating. The post-reaction material enters the outlet section through the reaction channel, is collected and stratified in the outlet section, and exits the reactor through the top outlet.
[0081] The specific embodiments of the present invention have been further described above with reference to the accompanying drawings. However, the present invention is not limited thereto. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.
[0082] The following examples further illustrate the implementation method of the present invention, but do not limit the present invention.
[0083] In the examples and comparative examples:
[0084] The reactants, olefins, and chemical reagents involved were commercially available.
[0085] Flow rate was analyzed by mass flow meter; gas holdup distribution was obtained by differential pressure method; sulfur composition in hydrocarbon oil was analyzed by infrared spectroscopy.
[0086] Example 1
[0087] As shown in the attached document Figure 1 The multi-channel microcirculation reactor shown is a microreactor containing 94 reaction channels, each with a rectangular cross-section and a cross-sectional area of 54 mm². 2 The mixing channel is 120 mm long, and the reaction channel is 600 mm long. Each mixing channel has a distribution orifice, and the inner diameter of the connecting pipe passing through the orifice is 0.5 mm. Operating conditions are room temperature and a gauge pressure of 2.8 MPa. The primary fluid is 1-decene, with a flow rate of 0.89 m³ / min. 3 The second fluid is boron trifluoride, with a flow rate of 0.42 m³ / h. 3 / h. The local gas holdup at the outlets of different channels is basically the same, with an average value of 0.0912. The non-uniformity of the local gas holdup distribution in each reaction channel is only 0.088, indicating that the fluid, especially the gas, can be uniformly distributed in the multi-channel microreactor.
[0088] Example 2
[0089] Adopted and attached Figure 1 The diagram shows a segmented multi-channel microreactor. The microreactor contains eight reaction channels: six outer channels evenly arranged circumferentially, and two inner channels. The average distance between the two layers of channels is 25 mm. Each channel has a rectangular cross-section with a cross-sectional area of 18 mm². 2 The mixing channel is 60 mm long, and the reaction channel is 2400 mm long. Each mixing channel has a distribution hole, and the inner diameter of the connecting pipe passing through the distribution hole is 1 mm. The outlet section is 100 mm long. The reaction temperature is 25℃, and the reaction pressure is 1.5 MPa. The first fluid is 1-decene with a flow rate of 54 g / min, containing 0.6% butanol as an initiator. The second fluid is BF3 with a flow rate of 800 mL / h. The conversion rate of the reaction was measured to be 95%, and the product was polyalphaolefin synthetic oil.
[0090] Example 3
[0091] As shown in the attached document Figure 1The diagram shows a segmented multi-channel microreactor. The microreactor contains four reaction channels, each with a rectangular cross-section and a cross-sectional area of 10 mm². 2 The mixing channel is 120 mm long, and the reaction channel is 8800 mm long. Each mixing channel has a distribution hole, and the inner diameter of the connecting pipe passing through the distribution hole is 1.5 mm. The outlet section is 150 mm long. There is no heat exchange function between the mixing section and the inlet section. The reaction channel uses a four-layered toothed mixing component to enhance fluid mixing inside the channel. The first fluid is diluted residue oil (residue oil feedstock to diluent mass ratio is 1:1), which contains oil-soluble molybdenum-based catalyst (mass content 5%), with a flow rate of 16.56 L / h at room temperature. The second fluid is hydrogen peroxide (concentration 30%), with a flow rate of 4.2 L / h at room temperature. The two fluids, after being mixed in the mixing channel, enter the reaction channel for reaction. The reaction temperature is 90℃, and the reaction pressure is atmospheric pressure. Analysis of the residue oil sample flowing out of the reactor shows that 45% of the thiophene compounds are converted into sulfone compounds. This indicates that the multi-channel microreactor provided by this invention can complete the oxidation reaction of thiophene compounds in a relatively short time.
[0092] Example 4
[0093] As shown in the attached document Figure 1 The diagram shows a segmented multi-channel microreactor. The microreactor contains four reaction channels, each with a rectangular cross-section and a cross-sectional area of 10 mm². 2 The mixing channel is 20 mm long, and the reaction channel is 300 mm long. Each mixing channel has a distribution hole, and the inner diameter of the connecting pipe passing through the distribution hole is 1 mm. The outlet section is 120 mm long. There is no heat exchange between the mixing section and the inlet section. The first fluid is a 0.025 mol / L aqueous solution of 5-hydroxymethylfurfural, which also contains NaOH in a 4:1 molar ratio with 5-hydroxymethylfurfural, with a flow rate of 152.9 mL / h at room temperature. The second fluid is O2, with a flow rate of 10.7 L / h under standard conditions. The reaction channel is filled with Au / CeO2 powdered catalyst. The reaction temperature is 90℃, and the reaction pressure is 0.6 MPa. Under the action of the catalyst, 5-hydroxymethylfurfural can be oxidized to various oxidation products, with 2,5-furandicarboxylic acid as the main product. Analysis of the liquid at the reactor outlet shows that the conversion rate of 5-hydroxymethylfurfural is 100%, and the selectivity of the main product 2,5-furandicarboxylic acid is 90%.
[0094] Comparative Example 1
[0095] As shown in the attached document Figure 5 The multichannel microreactor structure shown is related to the attached Figure 1The main difference is that it does not include a mixing section, and the outlet section is 500 mm long. The microreactor system contains 108 reaction channels, each with a rectangular cross-section and a cross-sectional area of 54 mm². 2 The reaction channel is 1200 mm long. The first and second fluids flow concurrently into the reactor through the inlet section. Operating conditions are ambient temperature and pressure. The first fluid is water, with a flow rate of 1 m³ / min. 3 / h, the second fluid is air, with a flow rate of 4m³ / h. 3 / h. Observation revealed no air bubbles in the 12 channels, and the fluid distribution was significantly uneven.
Claims
1. A multi-channel microreactor, characterized in that, It includes a sequentially connected inlet section (8), mixing section (22), reaction section (5), and outlet section (3); wherein: The inlet section is provided with a first fluid inlet (2) at the bottom; The mixing section is provided with a mixing channel (23), the bottom of the mixing channel passes through the first orifice plate (17) and communicates with the inlet section, the mixing channel wall is provided with a distribution hole (11), and the side wall of the mixing section is provided with a second fluid inlet (14); The reaction section is provided with a reaction channel (6) and a heat exchange channel. The bottom of the reaction channel is connected to the mixing channel via a second perforated plate (18). The heat exchange medium inlet (12) is connected to the heat exchange medium outlet (13) via the heat exchange channel. The outlet section is provided with a top outlet (1) and the bottom is connected to the reaction channel via a third perforated plate (4).
2. The multichannel microreactor according to claim 1, characterized in that, The inlet section is an inverted conical cylinder with a cone angle of 20 to 150°; Preferably, the inlet section is provided with a conical dispersing member (9), the dispersing member is coaxial with the inlet section, and the distance between the bottom of the dispersing member and the bottom of the inlet section is 10-150mm; Preferably, an inlet section heat exchange pipeline is provided within the inlet section, and the heat exchange pipeline serves as a heat exchange medium channel.
3. The multichannel microreactor according to claim 1 or 2, characterized in that, A uniform distribution plate (10) is provided below the mixing channel. The uniform distribution plate is made of porous material or a sieve plate structure. Preferably, the distance between the uniform distribution plate and the bottom of the mixing channel is 5 to 50 mm.
4. The multichannel microreactor according to claim 1 or 2, characterized in that, The cross-sectional area of the mixing channel is 0.1–65 mm. 2 The length ranges from 10 to 500 mm; Preferably, the length of the mixing channel is 15–150 mm; Preferably, the mixing channel has an expanding diameter structure from bottom to top.
5. The multichannel microreactor according to claim 4, characterized in that, The diameter of the distribution holes on the mixing channel is 0.3 to 5 mm, and the center distance between two adjacent distribution holes along the axial direction of the mixing channel is 5 to 100 mm. Preferably, the diameter of the distribution holes on the mixing channel is 0.5–1.5 mm; Preferably, the center distance between two adjacent distribution holes is 10–40 mm.
6. The multichannel microreactor according to claim 1 or 2, characterized in that, The mixing section sidewall is provided with a second fluid inlet (14), and the distance between the second fluid inlet and the second orifice plate is 5 to 100 mm; Preferably, the mixing section is provided with heat exchange tubes or a shell heat exchange structure.
7. The multichannel microreactor according to claim 1 or 2, characterized in that, The distance between adjacent reaction channels is 1–50 mm, preferably 3–30 mm; the cross-sectional area of the reaction channel is 0.1–65 mm². 2 The length ranges from 50 to 20,000 mm; Preferably, the length of the reaction channel is 100–6000 mm; Preferably, internal components are provided within the reaction channel.
8. The multichannel microreactor according to claim 1 or 2, characterized in that, The volume ratio of the heat exchange channel to the reaction channel in the reaction section is 2 to 50:1, preferably 5 to 30:1; Preferably, the heat exchange channel of the reaction section is provided with multiple baffles, and the distance between two adjacent baffles is 100-600 mm.
9. The multichannel microreactor according to claim 1 or 2, characterized in that, The heat exchange pipes (21) are located within the first orifice plate and / or the second orifice plate.
10. The multi-channel reactor according to claim 1 or 2, characterized in that, The height of the exit section is less than 15cm; Preferably, the bottom sidewall of the outlet section is further provided with a second outlet.
11. The multichannel microreactor according to claim 1, characterized in that, The reaction section is divided into at least two sections, which are connected by an inter-section perforated plate.
12. The method of applying the multichannel microreactor according to any one of claims 1-11, characterized in that, Liquid enters the inlet section through the first fluid inlet, flows upward and is distributed by the uniform distribution plate, then enters the mixing channel of the mixing section. Gas enters the mixing section through the second fluid inlet and enters the mixing channel through the distribution holes. In the mixing channel, the liquid and gas mix and flow upward through the second orifice plate into the reaction channel of the reaction section to react. The fluid that has completed the reaction leaves the reaction channel and enters the outlet section, where it is collected and discharged from the multi-channel microreactor through the outlet. The volume ratio of the introduced gas to the liquid is 0.05 to 100:1, preferably 0.1 to 40:
1.
13. The method of applying the multichannel microreactor according to any one of claims 1-11, characterized in that, The first liquid enters the inlet section through the first fluid inlet, flows upward and is distributed through the uniform distribution plate, then passes through the first perforated plate and enters the mixing channel of the mixing section. The second liquid enters the mixing section of the reactor through the second fluid inlet, and enters the mixing channel through the distribution holes on the mixing channel to mix with the first liquid. The mixed fluid flows upward and passes through the first perforated plate to enter the reaction channel of the reaction section to react. The fluid that has completed the reaction leaves the reaction channel and enters the outlet section, where it collects and is discharged from the reactor through the outlet. The density of the first liquid is greater than that of the second liquid, and the volume ratio of the first liquid to the second liquid is 0.01 to 20:1, preferably 0.1 to 6:1.
Citation Information
Patent Citations
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