Integrated tower type circulating flow reactor with separation function

Abstract

The invention relates to an integrated tower type circulating flow reactor with a separation function, which is applied to mass and heat transfer processes among gas, liquid and solid phases in fine chemical engineering, drug intermediates and the like, the upper part of the reactor is of a three-stage circulating flow structure, and an outer sleeve (7) of each stage is divided into an inner ascending circulating area and an outer descending circulating area by an inner net (5); the inner sleeve (5) is connected with the outer sleeve (7) through a bolt (6); a breather pipe (1), a gas distributor (2), a liquid collector (3), a solid collector (4), an inner sleeve (5), a bolt (6) and a gas outlet pipe (8) are sequentially arranged on the tower body from bottom to top; the interface and the external pipeline are sequentially a gas inlet gas supplementing pipe (a), a gas circulating pipe (c), a liquid discharging pipe (e), a liquid inlet pipe (d), a solid feeding pipe (f) and an exhaust pipe (b) from bottom to top; the liquid collector (3) is positioned in the middle of the equipment and between the liquid inlet pipe (d) and the liquid discharge pipe (e); the gas supplementing pipe (a) is connected with the gas circulating pipe (c) through the drainage ejector (9), and circulating gas is drained through supplementing gas. The integrated circulating flow reactor with the separation function is applied to the processes of fine chemical engineering, drug intermediate production and the like, integration of vapor-liquid-solid circulating fluidization and separation is achieved, the design and manufacturing cost is reduced, and the gas utilization rate is increased; and the problems of high energy consumption and many dead zones of the original stirred tank reactor are solved, and the heat and mass transfer efficiency is improved.

Description

Technical Field

[0001] The invention relates to an integrated tower circulating flow reactor with separation function, which is applied to fine chemical industry, synthesis of pharmaceutical intermediates and other processes involving mass transfer and heat transfer reaction between gas, liquid and solid three phases. Background Art

[0002] Compared with stirred tank reactors, circulating flow reactors have a simple structure, good heat transfer, mass transfer and mixing performance, low pressure drop, low energy consumption, low shear stress, can maintain a high biological concentration and activity, and reduce the deposition of solid materials at the bottom of the reactor. It is of great significance to the fields of fine chemicals, biopharmaceutical production, etc. As a special fluidized bed, the circulating fluidized bed can realize the fluidization of solids, increase the gas-liquid-solid contact time, improve the heat transfer and mass transfer efficiency, facilitate clean production, and has good application prospects and value.

[0003] Existing processes such as fine chemicals and pharmaceutical intermediate production mostly use stirred tank reactors, which use stirring paddles to achieve uniform mixing. However, they have problems such as high energy consumption, many dead zones, and low heat and mass transfer efficiency.

[0004] CN201520012655.0 proposes a continuous kettle reactor for producing diuron, which achieves uniform mixing through a "U-shaped" agitator connected to a variable speed shaft, making it easy to change and control reaction conditions. However, it has high energy consumption, dead zones in the flow, and requires further separation later.

[0005] CN201220050518.2 proposes a reactor for efficiently preparing pesticide synergists, which improves product quality and production efficiency through a stirrer and jacket heating (or cooling), but it also has the problems of high energy consumption, dead flow zones, inability to directly achieve separation, and requires an additional heating (or cooling) medium.

[0006] CN200620041978.3 proposed an airlift circulating flow membrane bioreactor, which realizes the circulation and reaction of three phases of reaction gas, activated sludge and wastewater; however, the equipment has a single purpose and the membrane is easily contaminated, which is not suitable for production in the fields of fine chemicals.

[0007] CN201520752085.9 proposes a microaerobic circulating fluidized bed bioreactor, which distributes microaerobic microorganisms in the microaerobic circulating fluidized reaction zone through circulating fluidization, effectively solving the problem of high-solid content, high-pollutant organic wastewater being difficult to degrade, but there are problems such as gas waste.

[0008] In order to solve many problems existing in the industrial production of fine chemical and pharmaceutical intermediate production equipment at this stage, the present invention proposes an integrated tower circulating flow reactor equipment with separation function, which has simple structure, high efficiency, strong adaptability and large processing capacity, based on the existing technology. Summary of the invention

[0009] The present invention proposes an integrated tower circulating flow reactor with separation function for use in the production of fine chemicals and pharmaceutical intermediates. The fluidized bed, solid-liquid separator, and circulating system are integrated into one, solving the problems of high energy consumption and flow dead zones in traditional stirred tank reactors; it also solves the problems that traditional fluidized bed reactors cannot achieve liquid-solid separation and gas recycling. It can reduce the flow dead zone, realize solid phase fluidization and piston flow flow, and avoid gas short circuit; it can also complete liquid-solid separation in time, realize the timely discharge of the solid phase internal circulation product, which is beneficial to the reaction; more importantly, the equipment has no stirring device and uses a drainage ejector to drain the external circulation gas, which reduces the operating energy consumption and has good uniformity. Therefore, the invention can greatly improve the heat and mass transfer efficiency of processes such as fine chemicals and pharmaceutical intermediates production, reduce production and design costs, and has broad industrial application prospects.

[0010] The technical solution of the present invention is as follows:

[0011] A tower type circulating flow reactor with separation function. The reactor is characterized in that the upper part is a three-stage circulating flow structure, each stage is divided into an inner sleeve (5) by an outer sleeve (7) into an inner ascending area and an outer descending area, and the inner sleeve (5) is connected to the outer sleeve (7) by bolts (6); the tower body is composed of an air inlet pipe (1), a gas distributor (2), a liquid collector (3), a solid collector (4), an inner net (5), bolts (6), and an air outlet pipe (8) from bottom to top; the interfaces and external pipelines are composed of an air supply pipe (a), a gas circulation pipe (c), a liquid discharge pipe (e), a liquid supply pipe (d), a solid feed pipe (f), and an exhaust pipe (b) from bottom to top; the liquid collector (3) is located in the middle of the equipment, between the liquid supply pipe (d) and the liquid discharge pipe (e); the air supply pipe (a) is connected to the gas circulation pipe (c) through a drainage ejector (9), and the circulating gas is drained by the supplementary gas.

[0012] The inner sleeve (5) is made of a Johnson mesh or similar material, and has a diameter ratio of 0.1-0.95 to the outer sleeve (7). The pore size is 1-10 mm, and liquid can pass through but air bubbles cannot.

[0013] The liquid collector (3) is composed of a small chute (10), an inclined plate (11) and a large chute (12); a layer of liquid-solid separation membrane (14), such as a ceramic membrane or an inorganic membrane, with a porosity of 0.5-0.9 is laid on the upper part of the inclined plate (11) to collect liquid while blocking solid from entering.

[0014] The number of aeration heads in the gas distributor (2) increases as the tower diameter increases.

[0015] The gas supply pipe (a) continuously introduces reaction gas or inert gas, and the exhaust pipe (b) is used to exhaust gas that inhibits the reaction.

[0016] The equipment has a diameter of 0.7-10 m and an aspect ratio of 1.5-10.

[0017] The tower-type circulating flow reactor with separation function of the present invention is operated as follows: the liquid phase is introduced through the liquid inlet pipe (d), and solid particles are added through the solid inlet (f); the gas phase is introduced through the gas supply pipe (a), and enters the tower after passing through the gas inlet pipe (1) and the gas distributor (2), so that the three phases of gas, liquid and solid are fluidized in the inner net (5); compared with the fluidized ascending zone inside the inner net (5), the fluid velocity between the inner net (5) and the outer sleeve (7) is larger, the static pressure is smaller, and the three phases of gas, liquid and solid move downward to form a descending zone; the bubble size can be adjusted by adjusting the aperture of the gas distributor (2), and the circulation rate, void ratio, residence time and reaction kinetics performance can be adjusted by adjusting the gas velocity of the gas distributor (2).

[0018] After passing through the descending zone, the three phases of gas, liquid and solid leave the upper circulation zone of the tower and descend to the middle of the tower. After passing through the solid collector (4), the solid is mixed with the ascending gas from the gas distributor (2) and enters the inner network (5) for fluidized circulation. After passing through the solid collector (4) and the liquid collector (3), the liquid is collected at the axis of the tower and enters the ascending zone or is discharged through the drain pipe (e); the solid collector (4) ensures that the solid particles re-enter the center of the tower to continue to achieve fluidization, and also plays a role in gas uniformity and bubble breaking. The liquid collector (3) realizes the collection of liquid and also plays a role in liquid-solid separation.

[0019] The gas that does not enter the internal circulation is discharged through the gas outlet pipe (8), and part of the gas that inhibits the reaction is discharged through the exhaust pipe (b). The remaining gas enters the gas circulation pipe (c), and then enters the gas inlet pipe (1) and the gas distributor (2) after passing through the drainage ejector (9), thereby realizing gas recovery.

[0020] The advantages of the present invention are:

[0021] 1. The integrated circulating flow reactor with separation function is applied to fine chemicals, pharmaceutical intermediate production and other processes, which realizes the orderly directionality of the flow in the reactor, reduces the irregular flow of the liquid phase, and reduces the probability of bubbles coalescing to form large bubbles; there are no mechanical moving parts and seals, and solves the problems of high energy consumption and many dead zones of the original stirred tank reactor; at the same time, the shear stress inside the reactor is low, which is of great significance to industries such as biomedicine.

[0022] 2. Under reasonable conditions, part of the liquid reactants can be vaporized and introduced as feed gas, which can achieve circulating fluidization while increasing the contact area of ​​the reactants and improving the conversion rate.

[0023] 3. It integrates fluidized bed, solid-liquid separation and other systems, saving process floor space, simplifying production equipment, reducing energy consumption, and reducing design and manufacturing costs and production operation costs.

[0024] 4. The bubble size and gas velocity can be controlled by adjusting the equipment structure parameters and process operation parameters, the reaction contact area can be increased, the mass transfer efficiency can be improved, and the conversion rate, residence time and kinetic performance can be effectively controlled.

[0025] 5. The solid collector below the circulation zone can evenly distribute the gas and break up the bubbles, making the gas flow in a piston flow state, so that the gas and solid phases are fully in contact and dead zones are avoided.

[0026] 6. The drainage ejector can drain the external circulation gas that has not entered the internal circulation through the supplementary gas, thereby realizing gas recovery and utilization. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is the overall structure diagram of the present invention.

[0028] Figure 2 It is a cross-sectional view taken along the AA plane of the present invention.

[0029] Figure 3 It is the left side view of the liquid collector used in the present invention.

[0030] Among them, 1-inlet pipe; 2-gas distributor; 3-liquid collector; 4-solid collector; 5-inner sleeve; 6-bolt; 7-outer sleeve; 8-outlet pipe; 9-drainage ejector; 10-small chute; 11-inclined plate; 12-large chute; 13-drainage pipe inlet; 14-liquid-solid separation membrane; a-air supply pipe; b-exhaust pipe; c-gas circulation pipe; d-liquid inlet pipe; e-drainage pipe; f-solid feed pipe. DETAILED DESCRIPTION

[0031] The present invention is further described in conjunction with the accompanying drawings:

[0032] like Figure 1 , 23: An integrated tower circulating flow reactor with separation function used in fine chemicals, pharmaceutical intermediates and other processes involving gas-liquid-solid three-phase mass transfer and heat transfer. The tower body is composed of an air inlet pipe (1), a gas distributor (2), a liquid collector (3), a solid collector (4), an inner sleeve (5), bolts (6), and an air outlet pipe (8) from bottom to top; the interfaces and external pipelines are composed of an air inlet and air supply pipe (a), a gas circulation pipe (c), a liquid discharge pipe (e), a liquid inlet pipe (d), a solid feed pipe (f), and an exhaust pipe (b) from bottom to top; the liquid collector (3) is located in the middle of the equipment, between the liquid inlet pipe (d) and the liquid discharge pipe (e); the air inlet pipe (a) is connected to the gas circulation pipe (c) through a drainage ejector (9), and the circulating gas is drained by the supplementary gas.

[0033] The gas distributor (2) is connected to the air inlet pipe (1) and has a pore diameter of 3 mm.

[0034] The inner sleeve (5) is a Johnson mesh with a seam width of 2.5 mm and a diameter ratio of 3:10 to the outer sleeve (7). The inner sleeve (5) is connected to the outer sleeve (7) by bolts (6). The interior of the inner mesh (5) is a rising zone for gas-liquid-solid fluidization. The gas-solid two-phase flow state is adjusted by adjusting the gas velocity of the gas distributor (2).

[0035] Liquid reactants are introduced through the liquid inlet pipe (d) until the liquid level reaches 50% of the tower height, and solid reactant particles accounting for 30% of the equipment volume are added into the device through the solid inlet (f). The exhaust pipe (b) is closed, and the reaction gas and inert gas are introduced through the gas supply pipe (a), and enter the tower through the gas distributor (2), and the gas, liquid and solid are rapidly fluidized in the inner sleeve (5), and a circulation is formed through the descending zone in the gap between the inner net (5) and the outer sleeve (7). The uncirculated gas passes through the gas outlet pipe (8) and is separated from the exhaust pipe (b) to partially inhibit the reaction. The remaining gas passes through the gas circulation pipe (c) and is drained by the drainage ejector (9) and enters the intake pipe (1) and the gas distributor (2), so as to realize gas recycling. The unreacted solid is collected by the solid collector (4) after passing through the descending zone, and the liquid-solid separation is realized at the liquid collector (3) because the particle size is larger than the aperture of the liquid collector (3), and the gas from the gas distributor (2) is brought into the multi-stage circulation again. The liquid in the descending zone also enters the intermediate ascending zone after passing through the solid collector (4) and the liquid collector. After the equipment has been running for a period of time, the liquid product is collected by the liquid collector (3) and discharged through the drain pipe (e) to enter the next process.

[0036] This circulating flow reactor with separation function successfully realizes the integration of gas-liquid-solid circulating fluidization and separation, saves floor space and energy consumption, reduces the cost of design, manufacturing and operation while ensuring high mass transfer efficiency and conversion rate; it is applied in the production process of fine chemicals and pharmaceutical intermediates to solve the problems of high energy consumption and many dead zones of the original stirred tank reactor.

[0037] The above examples are only preferred embodiments for fully illustrating the present invention, and the protection scope of the present invention is not limited thereto. Equivalent substitutions or changes made by those skilled in the art based on the present invention are within the protection scope of the present invention. The protection scope of the present invention shall be subject to the claims.

Claims

1. A tower type circulating flow reactor with separation function used in fine chemical industry, pharmaceutical intermediate production and other processes, characterized by: The upper part is a three-stage circulation flow structure, and each stage is divided into an inner rising area and an outer descending area by an inner net (5), and the inner net (5) is connected to the outer sleeve (7) by bolts (6); the tower body is composed of an air inlet pipe (1), a gas distributor (2), a liquid collector (3), a solid collector (4), an inner net (5), bolts (6), and an air outlet pipe (8) from bottom to top; the interface and the external pipeline are composed of an air supply pipe (a), a gas circulation pipe (c), a liquid discharge pipe (e), a liquid inlet pipe (d), a solid feed pipe (f), and an exhaust pipe (b) from bottom to top; the liquid collector (3) is located in the middle of the equipment, between the liquid inlet pipe (d) and the liquid discharge pipe (e); the air supply pipe (a) is connected to the gas circulation pipe (c) through a drainage ejector (9), and the circulating gas is drained by the supplementary gas.

2. A tower circulating flow reactor with separation function as claimed in claim 1, characterized in that The inner net (5) is a Johnson net or similar material, and has a diameter ratio of 0.1-0.95 to the outer sleeve (7). The slit width is 1-10 mm, and liquid can pass through but not air bubbles.

3. A tower type circulating flow reactor with separation function as claimed in claim 1, characterized in that The liquid collector (3) is composed of a small chute (10), an inclined plate (11) and a large chute (12); a layer of liquid-solid separation membrane (14), such as a ceramic membrane or an inorganic membrane, with a porosity of 0.5-0.9 is laid on the upper part of the inclined plate (11) to collect liquid while blocking solid from entering.

4. A tower type circulating flow reactor with separation function as claimed in claim 1, characterized in that The number of aeration heads in the gas distributor (2) increases as the tower diameter increases.

5. A tower circulating flow reactor with separation function as described in claim 1, characterized in that the gas supply pipe (a) continuously introduces reaction gas or inert gas, and the exhaust pipe (b) is used to exhaust gas that inhibits the reaction.

6. A tower circulating flow reactor with separation function as claimed in claim 1, characterized in that the equipment diameter is 0.7-10m and the aspect ratio is 1.5-10.

Images