阅读说明：本技术 具有多孔泡沫载体结构的扩散式气液固三相微反应器 (Diffusion type gas-liquid-solid three-phase micro-reactor with porous foam carrier structure ) 是由 陈蓉 陈刚 朱恂 叶丁丁 廖强 李俊 付乾 于 2019-10-09 设计创作，主要内容包括：本发明公开了一种具有多孔泡沫载体结构的扩散式气液固三相微反应器,包括上盖板、多孔泡沫板、左、右中间夹板和底板；其特征在于：上盖板、多孔泡沫板和底板按从上往下顺序设置；所述上盖板的底部沿水平方向设置有槽道一,底板的顶部沿水平方向设置有槽道二；槽道一、二的长度和宽度与分别多孔泡沫板的长度和厚度一致；多孔泡沫板的顶部和底部分别嵌入槽道一、二中；在多孔泡沫板的左、右侧分别放置左、右中间夹板；左、右中间夹板的中部开有凹槽,凹槽的长度与多孔泡沫板的长度一致,多孔泡沫板的左、右侧壁与左、右中间夹板之间均留有间隙,该间隙作为气体通道；该气体通道由上盖板和底板密封；可广泛适用于化工、环保等领域。(The invention discloses a diffusion type gas-liquid-solid three-phase microreactor with a porous foam carrier structure, which comprises an upper cover plate, a porous foam plate, a left middle clamping plate, a right middle clamping plate and a bottom plate; the method is characterized in that: the upper cover plate, the porous foam plate and the bottom plate are arranged from top to bottom in sequence; the bottom of the upper cover plate is provided with a first channel along the horizontal direction, and the top of the bottom plate is provided with a second channel along the horizontal direction; the length and the width of the first channel and the second channel are consistent with the length and the thickness of the porous foam plate respectively; the top and the bottom of the porous foam plate are respectively embedded into the first channel and the second channel; a left middle clamping plate and a right middle clamping plate are respectively arranged on the left side and the right side of the porous foam plate; the middle parts of the left and right middle splints are provided with grooves, the length of the grooves is consistent with that of the porous foam plate, gaps are reserved between the left and right side walls of the porous foam plate and the left and right middle splints, and the gaps are used as gas channels; the gas channel is sealed by an upper cover plate and a bottom plate; can be widely applied to the fields of chemical industry, environmental protection and the like.)

1. A diffusion type gas-liquid-solid three-phase micro-reactor with a porous foam carrier structure comprises an upper cover plate (2), a porous foam plate (3), a left middle clamping plate, a right middle clamping plate (4, 5) and a bottom plate (6); a catalyst is prepared on the porous foam plate (3); the method is characterized in that: the upper cover plate (2), the porous foam plate (3) and the bottom plate (6) are arranged from top to bottom in sequence; the bottom of the upper cover plate (2) is provided with a first channel along the horizontal direction, and the top of the bottom plate (6) is provided with a second channel along the horizontal direction; the top and the bottom of the porous foam plate (3) are respectively embedded into the first channel and the second channel; a left middle splint and a right middle splint (4, 5) are respectively arranged on the left side and the right side of the porous foam board (3); grooves are formed in the sides, close to the porous foam plate 3, of the left and right middle clamping plates (4 and 5), so that gaps are reserved between the left and right side walls of the porous foam plate (3) and the left and right middle clamping plates (4 and 5) respectively and used as gas channels, and the gas channels are sealed by the upper cover plate (2) and the bottom plate (6); the gas channel is divided into a left gas channel (12) and a right gas channel (11) by a porous foam plate (3); a gap is reserved between the left middle splint and the right middle splint (4 and 5); the gap serves as a liquid inlet channel (9) and a liquid outlet channel (10); one side of the upper cover plate (2) is provided with a first air inlet hole and a second air inlet hole (2a and 2b), and the other side of the upper cover plate (2) is provided with a first air outlet hole and a second air outlet hole (2c and 2 d); the first air inlet hole (2a) and the first air outlet hole (2c) are communicated with the left air passage, and the second air inlet hole (2b) and the second air outlet hole (2d) are communicated with the right air passage;

gas-phase reactants enter the microreactor from the first and second gas inlet holes (2a, 2b), are diffused in the gas channel, react with the solution at the active sites of the catalyst on the porous foam plate (3) in the diffusion process, the reacted gas is discharged out of the microreactor from the first and second gas outlet holes (2c, 2d), and the liquid-phase reactants and products are discharged out of the microreactor from the liquid outflow channel (10).

2. The diffused gas-liquid-solid three-phase microreactor with a porous foam support structure of claim 1, wherein: the reactor further comprises a syringe pump (7), the syringe pump (7) being used for controlling the liquid flow.

3. The diffused gas-liquid-solid three-phase microreactor with a porous foam support structure of claim 1, wherein: the reactor further comprises a gas mass flow controller (8), the gas mass flow controller (8) being adapted to control the gas flow.

4. The diffused gas-liquid-solid three-phase microreactor with a porous foam support structure of claim 1, wherein: the reactor is characterized in that an upper cover plate (2), left and right middle clamping plates (4, 5) and a bottom plate (6) are fixed by bolts (1).

Technical Field

The invention relates to the field of microreactors, in particular to a diffusion type gas-liquid-solid three-phase microreactor with a porous foam carrier structure.

Background

Since the 21 st century, a series of problems such as energy exhaustion and environmental deterioration face unprecedented challenges in the traditional chemical industry, and the search for a more green and safe reaction technology is urgent. The micro-reactor attracts the wide attention of the scientific field due to the advantages of small volume, large specific surface area, good heat and mass transfer performance, safe reaction and the like. The scholars are dedicated to screening catalysts by utilizing the microreactor, exploring a new reaction path and optimizing the reaction process so as to ensure that the chemical production is more economic and environment-friendly.

As the most common microreactor type, a gas-liquid-solid three-phase microreactor is considered to be an ideal reactor structural form for heterogeneous catalytic reactions due to the outstanding heat and mass transfer characteristics of the microreactor. In most cases, the solid phase is a catalyst and is loaded on the wall surface of the micro-channel, the gas and the liquid are reactants or products, the reactants are conveyed to the surface of the catalyst from the main flow region of the reactor after entering the micro-channel, and are adsorbed and reacted at the active sites of the catalyst, and then the products generated by the reaction are desorbed at the active sites and are conveyed to the main flow region of the reactor from the surface of the catalyst. The mode that the catalyst is loaded on the wall surface of the micro-channel ensures short diffusion distance and good phase-to-phase contact, thereby having excellent heat and mass transfer performance. However, deactivated regeneration of the catalyst is a problem, which when the catalyst is deactivated may result in the entire microreactor not being reused, necessitating replacement of a new reactor, thereby increasing manufacturing costs. Therefore, the researchers have proposed the concept of micro-packed bed, which is to pack catalyst-loaded nano-microspheres in micro-channels and obtain excellent mass transfer rate, but has the disadvantage of large pressure drop, which is not suitable for industrial application.

The porous foam board is a novel functional material consisting of a solid skeleton and a large number of pores, and is mainly characterized by high specific surface area and low density. Common porous foam plates include graphite foam, metal foam, silicon carbide foam, and the like. Tourvieille et al used porous foam as a catalyst carrier for the first time in a square microchannel with a side length of 2mm, found that the mass transfer rate of the reactor is improved by 50% compared with that of a microchannel without filling, and fully proved the feasibility of using a porous foam plate as a catalyst carrier in a microreactor. However, it has been found that when the gas phase and the liquid phase are reactants entering the interior of the porous foam plate, the liquid pulse flow and the gas capillary fingering phenomenon are caused. Meanwhile, Serres et al believe that a gas channel is formed in the porous material by the gas, which undoubtedly reduces the contact area of the gas-liquid two-phase reactant and reduces the use efficiency of the catalyst, thereby reducing mass transfer and affecting the performance of the reactor. In addition, the instability of the internal flow of the porous structure can cause pressure fluctuation in the microreactor, and the pressure fluctuation is not beneficial to the normal operation of the microreactor.

Disclosure of Invention

The invention aims to provide a diffusion type gas-liquid-solid three-phase microreactor with a porous foam carrier structure.

In order to solve the above technical problem, a first technical solution of the present invention is: a diffusion type gas-liquid-solid three-phase micro-reactor with a porous foam carrier structure comprises an upper cover plate, a porous foam plate, a left middle clamping plate, a right middle clamping plate and a bottom plate; a catalyst is prepared on the porous foam board; the method is characterized in that: the upper cover plate, the porous foam plate and the bottom plate are arranged from top to bottom in sequence; the bottom of the upper cover plate is provided with a first channel along the horizontal direction, and the top of the bottom plate is provided with a second channel along the horizontal direction; the length and the width of the first channel and the second channel are consistent with the length and the thickness of the porous foam plate respectively; the top and the bottom of the porous foam plate are respectively embedded into the first channel and the second channel; a left middle clamping plate and a right middle clamping plate are respectively arranged on the left side and the right side of the porous foam plate; the middle parts of the left and right middle clamping plates are provided with grooves, the length of the grooves is consistent with that of the porous foam plate, gaps are reserved between the left and right side walls of the porous foam plate and the left and right middle clamping plates respectively, the gaps are used as gas channels, and the gas channels are sealed by the upper cover plate and the bottom plate; the gas channel is divided into a left gas channel and a right gas channel by a porous foam plate; a gap is reserved between the left and right middle splints; the gap is used as a liquid inlet channel and a liquid outlet channel; a first air inlet hole and a second air inlet hole are formed in one side of the upper cover plate, and a first air outlet hole and a second air outlet hole are formed in the other side of the upper cover plate; the first air inlet hole and the first air outlet hole are communicated with the left air passage, and the second air inlet hole and the second air outlet hole are communicated with the right air passage.

Gas-phase reactants enter the microreactor from the first air inlet hole and the second air inlet hole, are diffused in the gas channel, react with the catalyst active sites of the solution on the porous foam plate in the diffusion process, the reacted gas is discharged out of the microreactor from the first air outlet hole and the second air outlet hole, and liquid-phase reactants and products are discharged out of the microreactor from the liquid outflow channel.

The porous foam plate is used as a catalyst framework and is combined with the microreactor, the advantage of short mass transfer distance of the microreactor is fully utilized, and meanwhile, the porous foam plate provides a larger surface area and can improve the dispersity of the catalyst. In addition, the defects of small contact area and pressure fluctuation caused by the fact that gas-liquid two-phase reactants enter the porous material at the same time are avoided, and therefore the performance of the microreactor is improved.

According to the preferable scheme of the diffusion type gas-liquid-solid three-phase micro-reactor with the porous foam carrier structure, the reactor further comprises an injection pump, and the injection pump is used for controlling the liquid flow.

According to the preferable scheme of the diffusion type gas-liquid-solid three-phase micro-reactor with the porous foam carrier structure, the reactor further comprises a gas mass flow controller, and the gas mass flow controller is used for controlling the gas flow.

According to the preferable scheme of the diffusion type gas-liquid-solid three-phase micro-reactor with the porous foam carrier structure, the upper cover plate, the left middle clamping plate, the right middle clamping plate and the bottom plate are fixed by bolts.

The diffusion type gas-liquid-solid three-phase microreactor with the porous foam carrier structure has the beneficial effects that:

1) the invention adopts the porous foam board as the catalyst framework, which is beneficial to improving the loading area and the dispersion degree of the catalyst, and meanwhile, the integral catalyst is easy to replace.

2) The adoption of the porous material effectively reduces the pressure drop of the reactor and is beneficial to reducing the energy loss of the reactor.

3) And only liquid-phase reactants flow in the porous material by adopting a gas diffusion mode, so that the uniform distribution of a liquid phase is facilitated, the stability of the internal pressure and the flow of the reactor is kept, and the safe operation is facilitated.

4) Effectively increases the gas-liquid contact area, thereby strengthening the mass transfer.

5) The reactor is miniaturized, can independently run in a unit mode for exploration and process optimization of the reaction, and can form a reactor stack for large-scale production.

The invention can be widely applied to the fields of chemical industry, environmental protection and the like.

Drawings

FIG. 1 is an assembly schematic diagram of a diffusion type gas-liquid-solid three-phase micro-reactor with a porous foam carrier structure.

FIG. 2 is a front view of the left and right intermediate decks of the present invention assembled with a cellular foam deck.

FIG. 3 is a top view of the left and right intermediate cleats of the present invention assembled with a cellular foam deck.

FIG. 4 is a left side view of the assembled left and right intermediate clamping plates and cellular foam boards of the present invention.

FIG. 5 is a schematic structural diagram of a diffusion type gas-liquid-solid three-phase micro-reactor with a porous foam carrier structure.

In the drawings: 1-bolt; 2, an upper cover plate; 2 a-a first inlet port; 2 b-a second inlet port; 2 c-a first outlet hole; 2 d-a second air outlet; 3-porous foam board; 4-left middle splint; 5-right middle splint; 6-a bottom plate; 7-injection pump; 8-gas mass flow controller; 9-liquid inlet channel; 10-liquid outflow channel; 11 — right airway; 12 — left airway.

Detailed Description

The present invention will be described in further detail with reference to test examples and specific embodiments. It should be understood that the scope of the above-described subject matter is not limited to the following examples, and any techniques implemented based on the disclosure of the present invention are within the scope of the present invention.

Referring to fig. 1 to 5, a diffusion type gas-liquid-solid three-phase micro-reactor with a porous foam carrier structure is composed of an upper cover plate 2, a porous foam plate 3, left and right middle clamping plates 4 and 5, a bottom plate 6, an injection pump 7 and a gas mass flow controller 8; a catalyst is prepared on the porous foam plate 3; the upper cover plate 2, the porous foam plate 3 and the bottom plate 6 are arranged from top to bottom in sequence; the bottom of the upper cover plate 2 is provided with a first channel along the horizontal direction, and the top of the bottom plate 6 is provided with a second channel along the horizontal direction; the length and the width of the first channel and the second channel are consistent with the length and the thickness of the porous foam plate 3 respectively; the top and the bottom of the porous foam plate 3 are respectively embedded into the first channel and the second channel; a left middle splint 4 and a right middle splint 5 are respectively arranged on the left side and the right side of the porous foam board 3; the left and right middle splints 4, 5 limit the porous foam plate 3, one side of the left and right middle splints 4, 5 near the porous foam plate 3 is provided with a groove, the length of the groove is consistent with the length of the porous foam plate 3, the porous foam plate 3 is arranged in the groove, so that a gap is left between the left and right side walls of the porous foam plate 3 and the left and right middle splints 4, 5 respectively, the gap is used as a gas channel, and the gas channel is sealed by the upper cover plate 2 and the bottom plate 6; the gas channel is divided into a left gas channel 12 and a right gas channel 11 by a porous foam plate 3; and a gap is also left between the left and right middle splints 4 and 5; the gap is communicated with the groove and serves as a liquid inlet channel 9 and a liquid outlet channel 10; one side of the upper cover plate 2 is provided with a first air inlet hole 2a and a second air inlet hole 2b, and the other side of the upper cover plate 2 is provided with a first air outlet hole 2c and a second air outlet hole 2 d; the first air inlet hole 2a and the first air outlet hole 2c are communicated with the left air passage 12, and the second air inlet hole 2b and the second air outlet hole 2d are communicated with the right air passage 11.

The syringe pump 7 is used to control the liquid flow rate.

The first and second air inlet holes 2a and 2b are connected with a gas mass flow controller 8, and the gas mass flow controller 8 is used for controlling the gas flow.

The reactor is fixed by bolts 1 to an upper cover plate 2, left and right middle clamping plates 4 and 5 and a bottom plate 6.

Gas-phase reactants enter the microreactor from the first and second gas inlet holes 2a and 2b, are diffused in the gas channel, react with a solution at the active sites of the catalyst on the porous foam plate 3 in the diffusion process, the reacted gas is discharged out of the microreactor from the first and second gas outlet holes 2c and 2d, and the liquid-phase reactants and the liquid-phase products are discharged out of the microreactor from the liquid outflow channel 10.

When the device is used specifically, a liquid, such as a nitrobenzene solution, is injected into the microreactor by using an injection pump 7, the nitrobenzene solution enters the reactor from a liquid inlet channel 9, the nitrobenzene solution is uniformly dispersed and flows in the porous foam under the action of pump thrust and capillary force, a gas-phase reactant, such as hydrogen, enters the reactor from the first and second gas inlet holes 2a and 2b and is diffused in the gas channel, the hydrogen reacts with the catalyst active sites of the nitrobenzene solution on the porous foam plate 3 through diffusion in the diffusion process, the reacted gas is discharged out of the reactor from the first and second gas outlet holes 2c and 2d, and the liquid-phase reactant and a product are discharged out of the microreactor from a liquid outlet channel 10.

Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art may still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some technical features. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.