Tubular reactor unit and system

Abstract

The present invention discloses a tubular reactor unit and system, which is particularly used for gas-liquid-solid multiphase reactions, accompanied by crystal particle products, and the reaction conditions involve high temperature and high pressure reactions. The reactor mainly includes a jet mixer, a tubular reactor, a gas-liquid separation buffer tank, a circulation pump, and a crystal crusher. Under the action of the circulation pump, the mother liquor circulates in the tubular reactor and the gas-liquid separation buffer tank to control the flow state and residence time. The tubular reactor is a coil-type jacketed reactor with a heat exchange function, and the jet mixer has the characteristics of multiple input ports and microbubble generation function. The crystal crusher can fully crush the crystal particles in the circulating mother liquor. The present invention adopts a combination of local single circulation and global multi-circulation, combined with microbubble generation technology, in-tube turbulence technology, and grain crushing technology, which greatly shortens the length of the traditional tubular reactor and can achieve fully enclosed, continuous, high conversion rate, and rapid production.

Description

Technical Field

[0001] The invention belongs to the field of chemical process production equipment and relates to a tubular reactor unit and system. Background Art

[0002] In existing chemical process equipment, in many cases, liquid media, gaseous media and solid media need to be mixed before chemical reactions can be carried out. A common solution is to use ordinary kettle reactors to carry out chemical reactions in gas, liquid and solid multiphase heterogeneous systems. Due to the stratification between phases and the small contact area, the mass transfer during the reaction is relatively poor, which will cause uneven mixing of the reaction mother liquor. As a result, the reaction time is long and the conversion rate is low. In order to enhance the mixing effect, the usual practice is to add an agitator. However, if the reaction system involves high temperature and high pressure, or the gas medium is toxic, harmful, flammable and explosive, there will be huge safety hazards at the agitator seal.

[0003] The tank reactor cannot be completely filled with liquid material. Instead, a gas medium is introduced into the liquid material from the bottom, and stirring is used to achieve gas-liquid mixing. However, the gas's residence time in the liquid is short, resulting in an incomplete reaction. Furthermore, the reactor is large, and heat is transferred from the reactor shell into the interior, resulting in an uneven temperature gradient. Uneven mixing can easily lead to incomplete reaction. Mechanical stirring is even more difficult when the product contains crystals. Furthermore, the crystal particles can encapsulate some of the raw material, and if they are not broken and released, the yield will inevitably be reduced. Furthermore, the tank reactor cannot be used for continuous production. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to provide a fully enclosed, leak-proof, highly safe, high mother liquor utilization rate, high product yield, extremely low waste discharge, and environmentally friendly tubular reactor unit and system in response to the above problems.

[0005] The technical solutions adopted by the present invention to solve the technical problems are as follows:

[0006] The first tubular reactor unit provided by the present invention comprises a first jet mixer, a tubular reactor, and a circulation pump.

[0007] The tubular reactor includes a tank body and a spiral coil. The spiral coil is installed in the tank body. One end of the spiral coil is a material inlet, and the other end is a material outlet. The tank body is filled with a heat exchange medium. The top and bottom of the tank body are respectively provided with a heat exchange medium inlet and outlet. Liquid medium is introduced during operation for heat exchange.

[0008] The internal cavity of the first jet mixer is sequentially provided with an input port, a contraction section, a mixing chamber, a throat section, a diffusion section, and an output port, the contraction section is conical, and the inner diameter gradually decreases along the flow direction of the mother liquid, the large diameter port of the contraction section is connected to the input port, the small diameter port of the contraction section is inserted into the mixing chamber and faces the throat section, the mixing chamber is funnel-shaped, the large diameter port of the mixing chamber is adjacent to the input port, the small diameter port of the mixing chamber is connected to the throat section, the side wall of the mixing chamber is connected to one or more suction ports, a metal sponge or other porous material is installed inside the throat section, the micropore diameter of the metal sponge is larger than the diameter of the grain particles in the fluid, the diffusion section is conical, and the inner diameter gradually expands along the flow direction of the mother liquid, the small diameter end of the diffusion section is connected to the outlet of the throat section, and the large diameter end of the diffusion section is connected to the output port;

[0009] The first suction port of the first jet mixer is connected to the reaction material input pipeline, the output port of the first jet mixer is connected to the material inlet of the tubular reactor, and the material outlet pipeline of the tubular reactor is divided into two paths, one of which is connected to the inlet of the circulation pump, and the outlet of the circulation pump is connected to the input port of the first jet mixer, thereby forming a closed loop.

[0010] The second tubular reactor unit provided by the present invention also includes a gas-liquid separation buffer tank, the material inlet of the gas-liquid separation buffer tank is connected to the material outlet of the tubular reactor, the gas-liquid separation buffer tank has a gas outlet, a side wall liquid outlet and a tank bottom liquid outlet, the tank bottom liquid outlet is connected to the inlet of the circulation pump, and the outlet of the circulation pump is connected to the input port of the first jet mixer.

[0011] The third tubular reactor unit provided by the present invention further includes a first crystal crusher, wherein the inlet of the first crystal crusher is connected to the outlet of the circulation pump, and the outlet of the first crystal crusher is connected to the input port of the first jet mixer.

[0012] Furthermore, the gas outlet of the gas-liquid separation buffer tank can be connected to the second suction port of the first jet mixer.

[0013] The fourth tubular reactor unit provided by the present invention further includes a second jet mixer, wherein the output port of the second jet mixer is connected to the third suction port of the first jet mixer.

[0014] The fifth tubular reactor unit provided by the present invention also includes a third jet mixer and a second crystal crusher. The first suction port of the third jet mixer is connected to the material outlet pipeline of the tubular reactor, the output port of the third jet mixer is connected to the inlet of the second crystal crusher, the outlet of the second crystal crusher is connected to the material inlet of the gas-liquid separation buffer tank, and the outlet pipeline of the circulation pump is divided into two routes, one route is connected to the input port of the third jet mixer, and the other route is connected to the inlet of the first crystal crusher.

[0015] Furthermore, the output port of the jet mixer is equipped with a micro-nano bubble generating assembly, which can achieve micro-nano mixing of gas and liquid and flexibly adjust the intake volume according to process requirements.

[0016] Furthermore, a turbulent flow component is installed in the spiral coil and / or the tank of the tubular reactor, so that the fluid in the spiral coil and / or the heat exchange medium in the tank is in a turbulent state.

[0017] Furthermore, the crystal crusher is a new type of non-powered crusher that relies on the kinetic energy of the fluid to crush crystals. It is similar in structure to the jet mixer, but does not include a mixing chamber or a suction port.

[0018] Furthermore, the circulation pump is a power device that drives the mother liquor to circulate in the tubular reactor unit, forming a local small loop. The circulation pump adjusts the flow rate, causing the mother liquor to enter a turbulent state to enhance the mixing effect, and drives the crystal crusher and jet mixer to operate.

[0019] Furthermore, the gas-liquid separation buffer tank has a jacketed outer shell, through which a heat exchange medium can be introduced to control the temperature of the gas-liquid separation buffer tank. The gas outlet is located at the top of the buffer tank and is connected to the inlet of the jet mixer via a pipeline. This allows unreacted gas to be returned to the front inlet for re-reaction, thereby balancing the pressure. The gas can also be transported to other locations.

[0020] The present invention also provides a tubular reaction system comprising any one or more of the above-mentioned reaction units connected in series or in parallel, and applied to the initiation stage, the mid-stage reaction stage, the late stage reaction stage, etc. A multi-cycle or large-cycle mode is adopted between the reaction units to achieve a multi-stage, continuous reaction.

[0021] Furthermore, it also includes an endpoint determination unit, which includes a jet mixer for endpoint determination, a gas-liquid separation buffer tank for endpoint determination, a circulation pump for endpoint determination, a crystal crusher for endpoint determination, an air inlet flowmeter for endpoint determination and an air outlet flowmeter for endpoint determination. The first suction port of the jet mixer for endpoint determination is connected to the side wall liquid outlet pipeline of the gas-liquid separation buffer tank of the last tubular reaction unit, the output port of the jet mixer for endpoint determination is connected to the material inlet of the gas-liquid separation buffer tank for endpoint determination, the gas outlet pipeline of the gas-liquid separation buffer tank for endpoint determination is divided into two paths, one path is connected to the air outlet flowmeter for endpoint determination, and the other path is connected to the second suction port of the jet mixer for endpoint determination. The liquid outlet at the bottom of the gas-liquid separation buffer tank for endpoint determination passes through the circulation pump for endpoint determination, the crystal crusher for endpoint determination and the input port of the jet mixer in sequence. The third suction port of the jet mixer for endpoint determination is connected to the reaction gas input pipeline, and the air inlet flowmeter for endpoint determination is installed on the reaction gas input pipeline. The reactant gas input is metered gas, thoroughly mixed in the endpoint determination jet mixer, and then enters the endpoint determination gas-liquid mixing buffer tank. Unconsumed raw material gas is discharged from the top of the gas-liquid mixing buffer tank and measured and compared to the input raw material gas flow rate to ensure equality. When the measured input gas flow rate equals the output gas flow rate, the reaction is considered complete. When the measured input gas flow rate exceeds the output gas flow rate, the reaction is considered incomplete.

[0022] Furthermore, it also includes an input unit and a function auxiliary unit, which are a combination of auxiliary equipment selected according to different process flows.

[0023] Furthermore, various reaction gases and liquids may be further preheated after being mixed before entering the tubular reactor unit.

[0024] Furthermore, gas return and pressure balancing pipelines are provided between the multiple tubular reactors and the gas outlets of the gas-liquid separation buffer tank.

[0025] Furthermore, bypass pipes are set between the liquid outlets of multiple tubular reactors and gas-liquid separation buffer tanks to establish a large circulation between the reactor units and connect them to the accident pool.

[0026] Furthermore, according to the degree of heat release or heat absorption of each reaction unit, the heat generated by the heat release unit is reasonably introduced into the heat absorption unit, thereby minimizing energy consumption.

[0027] The advantages and beneficial effects of the present invention are:

[0028] 1. The present invention adopts a novel jet mixer, which first disperses the reaction gas A into the non-reactive reaction liquid B in the form of micron or even nanometer-sized bubbles, thereby greatly increasing the contact area of the gas-liquid phase. At this time, it is further mixed in the liquid phase with the reaction liquid C to be reacted before entering the tubular reactor. The reaction liquid C can be a liquid dispersed with a powdered catalyst, thereby achieving uniform mixing of the gas, liquid and solid phases and greatly increasing the three-phase contact area, which is conducive to accelerating the reaction speed, shortening the reaction time, and improving the conversion rate.

[0029] 2. The present invention adopts a tubular reactor with an outer shell, with the reaction liquid flowing inside the tube and the heat transfer medium flowing outside the tube. Compared with the kettle reactor, the tubular reactor has a larger surface area, so the heat transfer is faster, and the inner diameter of the pipe is smaller, so the temperature is more uniform and the temperature control is more accurate. According to the provisions of GB150-2011 "Pressure Vessel", when the inner diameter of the coil tubular reactor is less than 150 mm, it is a non-pressure vessel and can withstand greater pressure, thereby greatly accelerating the reaction speed, shortening the reaction time, and increasing the output.

[0030] 3. The present invention utilizes a jacketed gas-liquid separation buffer tank. The jacket contains a heat exchange medium for temperature control. The buffer tank has a certain gas-liquid separation capacity. The top outlet is connected to the suction port of the front jet mixer. This allows unreacted gas to return to the reactor inlet and, while balancing pressure, allows the reactant gas to be transferred to subsequent equipment for processing. The buffer tank can store a certain amount of mother liquor, ensuring that the circulating pump does not run idle, while also increasing the reactor's capacity.

[0031] 4. The circulating pump of the present invention provides power for local circulation, can drive the jet mixer to generate vacuum, and drive the crystal crusher to crush the crystal particles in the mother liquor.

[0032] 5. The function of the crystal crusher of the present invention is to fully crush the crystal particles in the mother liquor, on the one hand to prevent the pipe from being blocked, and on the other hand to release the unreacted raw materials wrapped in the crystal particles, thereby improving the conversion rate of the raw materials.

[0033] 6. The tubular reactor units of the present invention can be combined in two or more groups in series, thereby achieving independent control requirements for parameters such as temperature, pressure, flow rate, etc. at different reaction stages in the production process.

[0034] 7. The endpoint determination unit of the present invention is provided with an input gas flow meter and an output gas flow meter. Whether the reaction gas continues to be consumed is an important basis for determining whether the reaction is complete. When the measured input gas flow rate is equal to the output gas flow rate, the reaction is determined to be complete. When the measured input gas is greater than the output gas, the reaction is determined to be incomplete. At this time, the unreacted mother liquor is sucked back to the front end to continue the reaction, thereby improving the utilization rate of the raw materials.

[0035] Thanks to the above beneficial effects, the present invention adopts a tubular reactor that is not a pressure vessel, which can withstand greater pressure, higher reaction temperature, and better sealing. It adopts a design that combines local circulation with grain crushing, so that the reactants are mixed more evenly, the fluidity is better, and the conversion rate is higher, thereby achieving the purpose of fully sealed and continuous production. Therefore, the present invention effectively overcomes the problems commonly existing in kettle reactors, such as uneven mixing, incomplete reaction, low safety, and low product yield. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] The present invention will be further described below with reference to the accompanying drawings and examples;

[0037] Figure 1 This is a schematic diagram of the reactor structure of Example 1;

[0038] Figure 2 This is a schematic diagram of the reactor structure of Example 2;

[0039] Figure 3 This is a schematic diagram of the reactor structure of Example 3;

[0040] Figure 4 This is a schematic diagram of the reactor structure of Example 4;

[0041] Figure 5 This is a schematic diagram of the reactor structure of Example 5;

[0042] Figure 6 This is a schematic diagram of the reactor structure of Example 6;

[0043] Figure 7 This is a schematic diagram of the reactor structure of Example 7;

[0044] Figure 8 This is a schematic diagram of the reactor structure of Example 8;

[0045] Figure 9 Schematic diagram of the structure of the jet mixer;

[0046] Figure 10 Schematic diagram of the crystal crusher structure;

[0047] Figure 11 Schematic diagram of the tubular reactor structure;

[0048] Figure 12 This is a schematic diagram of the structure of the gas-liquid separation buffer tank;

[0049] In the figure: 1 jet mixer, 2 tubular reactor, 3 circulating pump, 4 and 5 are the inlet and outlet of the heat exchange medium of the tubular reactor, 6 gas-liquid separation buffer tank, 7 crystal crusher, 8 and 9 are the inlet and outlet of the heat exchange medium of the gas-liquid separation buffer tank, 1a second jet mixer, 1b first jet mixer, 1c third jet mixer, 7a first crystal crusher, 7b second crystal crusher, f1 endpoint determination using an inlet flowmeter, f2 endpoint determination using an outlet flowmeter.

[0050] Jet mixer: S1 inlet, S2 contraction section, S3 mixing chamber, S4 throat section, S5 sponge metal body, S6 diffusion section, S7 outlet, S8 suction port;

[0051] Crystal crusher: J1 input port, J2 contraction section, J3 throat section, J4 sponge metal body, J5 diffusion section, J6 output port;

[0052] Tubular reactor: F1 inlet, F2 insulation shell, F3 reactor tank, F4 upper interface of heat exchange medium, F5 flow equalizing plate, F6 outlet, F7 spiral coil, F8 lower interface of heat exchange medium.

[0053] Gas-liquid separation buffer tank: H1 lower interface of heat exchange medium, H2 outer insulation layer, H3 heat exchange jacket layer, H4 liquid inlet, H5 gas outlet, H6 defoaming net, H7 upper interface of heat exchange medium, H8 liquid storage liner, H9 lower liquid outlet, H10 bottom liquid outlet. DETAILED DESCRIPTION

[0054] The preferred embodiments of the present invention are described in detail below in conjunction with the accompanying drawings and relevant known technical knowledge so that the advantages and features of the present invention can be more easily understood by those skilled in the art, thereby making a clearer and more precise definition of the scope of protection of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative work are within the scope of protection of the present invention.

[0055] Example 1

[0056] A fully closed-loop continuous gas-liquid catalytic oxidation tubular reactor, such as Figure 1 、 Figure 9 、 Figure 11As shown, it includes a jet mixer 1, a tubular reactor 2, and a circulation pump 3. The jet mixer suction port is connected to the external raw material mother liquid, and the output port is connected to the tubular reactor input port. The lower interface of the tubular reactor is usually selected as the input port, and the upper interface is selected as the output port. In this way, when the liquid is input from the bottom, all the gas in the pipeline can be discharged. The circulation pump input port is connected to the tubular reactor output port, and the circulation pump output port is connected to the jet mixer input port, thereby forming a circulation path. Under the action of the circulation pump, the mother liquid can be circulated in a fully closed and continuous manner in the circulation path. Figure 9 It is a detailed structural diagram of a jet mixer. The jet mixer has more than one suction port distributed in the mixing chamber. The number of suction ports is designed according to different needs. The number of interfaces of the jet mixer in this embodiment is two-input and one-output. Another feature of the jet mixer is that a sponge metal body is fixedly installed in the throat section. When a high-speed jet passes through, in the internal pores of the sponge metal, the mixed fluid and the pore wall undergo violent collision, extrusion, segmentation, shearing and other effects, thereby realizing micro-nano-level mixing of the mother liquor. In particular, the jet mixer has a certain crystal particle crushing ability. Figure 11 This is a detailed schematic diagram of the tubular reactor. The tubular reactor has an insulation layer on the outside and a sealed tank inside. Inlet and outlet ports are located at the top and bottom of the tank, respectively. A flow equalizer plate is fixedly installed at a distance of 0.1D to 1D (D is the inner diameter of the tank) from the inlet and outlet. When the heat exchange medium flows, the flow equalizer plate ensures more uniform flow, improving heat exchange and temperature control. A spiral coil is fixedly installed between the two flow equalizer plates. A gap is provided between the coils to facilitate the circulation of the heat exchange medium. The coil is fixed to the upper and lower parts of the tank and extends a short distance from the tank, serving as the coil's input and output ports. The coil in this embodiment has an inner diameter of less than 150mm. According to GB150-2011, "Pressure Vessels," a vessel with an inner diameter less than 150mm is considered a non-pressure vessel. Therefore, under the same material conditions, a tubular reactor can withstand higher temperatures and greater pressures than a kettle reactor.

[0057] This embodiment is suitable for reactions involving a single mother liquor, which can be a mixture of various liquids, gases, and micron-sized solid particles. The apparatus of this embodiment provides a completely sealed, high-pressure, and temperature-controlled environment for the mother liquor reaction. The circulating pump and jet mixer continuously promote thorough mixing of the mother liquor, resulting in a more uniform reaction and improved conversion.

[0058] Example 2

[0059] A fully closed-loop continuous gas-liquid catalytic oxidation tubular reactor, such as Figure 2 、 Figure 12As shown, it includes a jet mixer 1, a tubular reactor 2, a circulation pump 3, and a gas-liquid separation buffer tank 6. The difference and improvement from Example 1 is that this embodiment adds a gas-liquid separation buffer tank, which is connected in series between the output port of the tubular reactor and the input port of the circulation pump. Figure 12 It is a detailed structural diagram of the gas-liquid separation buffer tank. The outermost layer of the gas-liquid separation buffer tank is an insulation layer H2, and the innermost layer is a sealed liquid storage liner H8. A plurality of interfaces are respectively provided on the upper, lower and side surfaces of the liner. A gas-liquid separator is fixedly installed at a position 0.1D to 1D (D is the inner diameter of the liner) away from the upper interface to intercept mist and particulate matter in the rising gas. The heat exchange jacket layer H3 of the gas-liquid separation buffer tank is a heat medium circulation layer. Interfaces H1 and H7 are provided on the upper and lower parts of the heat exchange medium layer. Preferably, the interfaces H1 and H7 have a certain cutting angle with the container wall. Usually, the heat exchange medium is input from the interface H1. Due to the certain angle with the container wall, the heat exchange medium will rotate around the container wall interlayer, rise in a spiral shape and be output after reaching the interface H7. The spiral heat exchange medium flow is in a turbulent state, so the heat exchange and temperature control effects are better. Preferably, the liquid storage liner H8 is a pressure vessel with an inner diameter less than 150 mm. According to GB150-2011 "Pressure Vessels," a vessel with an inner diameter less than 150 mm is considered a non-pressure vessel and can therefore withstand higher temperatures and pressures. Preferably, the gas-liquid separation buffer tank can be equipped with more input and output interfaces as needed. Preferably, in addition to the required liquid storage liner H8, the gas-liquid separation buffer tank can optionally include a heat exchange jacket layer H3 and an insulation layer H2.

[0060] This embodiment is suitable for reactions involving a mother liquor accompanied by the need to separate gaseous products. The mother liquor can be a mixture of various liquids, gases, and micron-sized solid particles. The apparatus of this embodiment provides a completely sealed, high-pressure environment for the mother liquor reaction, equipped with temperature control and gas-liquid separation capabilities. The circulating pump and jet mixer continuously promote thorough mixing of the mother liquor, resulting in a more uniform reaction and improved conversion rate.

[0061] Furthermore, the gas-liquid separation buffer tank has a certain gas-liquid separation capacity. When the mother liquor is accompanied by gas products, the gas-liquid separation buffer tank acts as a gas-liquid separator to ensure that the gas by-products can leave the system smoothly.

[0062] Furthermore, the gas-liquid separation buffer tank has a certain mother liquor temporary storage capacity, which is equivalent to expanding the volume of the tubular reactor. When a larger volume buffer tank is needed, a larger volume can be obtained by connecting multiple gas-liquid separation buffer tanks in parallel.

[0063] Furthermore, the lower output port of the gas-liquid separation buffer tank is connected to the input port of the circulation pump, providing the circulation pump with mother liquid without gas, thereby avoiding idling wear of the circulation pump and reducing cavitation loss of the circulation pump.

[0064] Example 3

[0065] A fully closed-loop continuous gas-liquid catalytic oxidation tubular reactor, such as Figure 3 、 Figure 10 As shown, it includes a jet mixer 1, a tubular reactor 2, a circulation pump 3, a gas-liquid separation buffer tank 6, and a crystal crusher 7. The difference and improvement from Example 2 is that this embodiment adds a crystal crusher, which is connected in series between the output inlet of the circulation pump and the suction port of the jet mixer. Figure 10 This is a detailed structural diagram of the crystal crusher, which includes: an input port J1, a contraction section J2, a throat section J3, a sponge metal body J4, a diffusion section J5, and an output port J6. The input port is a circular interface. The contraction section gradually reduces its inner diameter along the flow direction of the mother liquid and eventually connects to the throat section. The throat section is cylindrical. The sponge metal body is a porous metal material. The diameter of the sponge metal body's micropores should generally be larger than the diameter of the crystal particles in the fluid. The diffusion section is connected to the throat section outlet and is characterized by a transition section that changes from small to large. The output port is circular. The crystal crusher is an unpowered crusher. The flow rate of the mother liquid increases after passing through the contraction section. When there are crystal particles in the mother liquid, their kinetic energy increases according to the square of the flow rate. In the pores inside the sponge metal body, the crystal particles collide violently with the pore walls and between the crystal particles, achieving a crushing effect on the crystal particles.

[0066] Furthermore, there are a large number of shock waves and eddy currents in the well-developed pores of the sponge metal body, which will produce cavitation and further break the crystal particles.

[0067] Furthermore, when large-diameter reaction bubbles are mixed in the mother liquor, after entering the throat section, the developed pores of the sponge metal body have a segmentation and shearing effect on the bubbles, and there are a large number of shock waves and eddies in the pores, which will produce cavitation and further break up the bubbles, thereby dispersing the bubbles into the mother liquor at the micron or even nanometer level, greatly increasing the contact area between the gas and liquid phases and accelerating the reaction speed.

[0068] This embodiment is applicable to the reaction of a mother liquor with gaseous products that need to be separated, and the reaction products contain crystal particles. The mother liquor can be a mixed fluid of multiple liquids, gases, and micron-sized solid particles. The difference and improvement over Example 2 is that when crystal particles appear in the product, they are fully crushed by the crystal crusher, which, on the one hand, ensures the fluidity of the mother liquor and, on the other hand, releases the unreacted mother liquor contained in the large crystal particles. Under the action of the circulation pump and the jet mixer, the mother liquor is continuously promoted to be fully mixed and crushed, making the reaction more uniform and improving the reaction speed and conversion rate.

[0069] Example 4

[0070] A fully closed-loop continuous gas-liquid catalytic oxidation tubular reactor, such as Figure 4 As shown, it includes a jet mixer 1, a tubular reactor 2, a circulation pump 3, a gas-liquid separation buffer tank 6, and a crystal crusher 7. The difference and improvement from Example 3 is that the interface form of the jet mixer in this embodiment is four inputs and one output. The jet mixer has an input port and three suction ports. The input port is connected to the crystal crusher outlet, and the three suction ports are respectively connected to the reaction liquid, reaction gas and circulating reaction gas. The circulating reaction gas comes from the gas output port of the gas-liquid separation buffer tank.

[0071] This embodiment is applicable to reactions involving a mother liquor and a reaction gas, with gases requiring separation and the production of crystalline particles in the reaction product. The mother liquor can be a mixed fluid of various liquids, gases, and micron-sized solid particles, and the reaction gas is a raw gas. A further difference and improvement over Example 3 is that the gas outlet of the gas-liquid separation buffer tank is connected to an inlet of a jet mixer, allowing the separated unreacted gas to be returned to the front end for re-entry into the reaction, thereby greatly improving the utilization rate of the reaction gas. Furthermore, when the reaction gas is toxic or hazardous, the device of this embodiment can complete the reaction in a fully sealed, zero-leakage manner.

[0072] Example 5

[0073] A fully closed-loop continuous gas-liquid catalytic oxidation tubular reactor, such as Figure 5 As shown, it includes a second jet mixer 1a, a first jet mixer 1b, a tubular reactor 2, a circulation pump 3, a gas-liquid separation buffer tank 6, and a crystal crusher 7. The difference and improvement from Example 4 is that this embodiment has an additional two-input and one-output jet mixer. The input port of the second jet mixer 1a is connected to the external reaction liquid B, the suction port thereof is connected to the external reaction gas A, and the output port thereof is connected to a suction port of the above-mentioned four-input and one-output first jet mixer 1b.

[0074] This embodiment is applicable to the reaction of two mother liquors and one reaction gas, accompanied by the need for gas separation and the production of crystal particles in the reaction product. The mother liquor can be a mixed fluid of multiple liquids, gases, and micron-sized solid particles. The reaction gas A is the raw gas. The liquid B is usually a solvent that does not react with gas A and serves as a carrier for gas A. The difference and improvement over Example 4 is that gas A is first mixed with liquid B for the first time in the second jet mixer 1a to form a gas-liquid mixture, and then mixed with liquid C for the second time in the first jet mixer 1b. At this time, the impact on the main circulation is minimized, and the secondary mixing effect is better, ensuring that the reaction gas A is dispersed into the mother liquor in the form of micro-nano bubbles, greatly increasing the gas-liquid-solid three-phase contact area, and making the reaction speed faster and the conversion rate higher.

[0075] Example 6

[0076] A fully closed-loop continuous gas-liquid catalytic oxidation tubular reactor, such as Figure 6 As shown, it includes a first jet mixer 1b, a second jet mixer 1a, a third jet mixer 1c, a tubular reactor 2, a circulation pump 3, a gas-liquid separation buffer tank 6, a first crystal crusher 7a, and a second crystal crusher 7b. The difference and improvement from Example 5 is that this embodiment has an additional third jet mixer 1c, and the input port of the third jet mixer 1c is connected to a path of mother liquor separated from the output port of the circulation pump, and its suction port is connected to the output port of the tubular reactor, and its output port is connected to the input port of the second crystal crusher 7b, and the output port of the second crystal crusher 7b is connected to the input port of the gas-liquid separation buffer tank. Preferably, the tubular reactor and the gas-liquid separation buffer tank of this embodiment specifically require an insulation design.

[0077] This embodiment is applicable to the reaction of two mother liquors and one reaction gas, accompanied by the need to separate gases, and the production of crystal particles in the reaction products. The mother liquor can be a mixed fluid of multiple liquids, gases and micron-sized solid particles. The reaction gas A is the raw gas. Usually, the liquid B is a solvent that does not react with gas A and is used as a carrier of gas A. Preferably, the tubular reactor 2 in this embodiment has the best insulation and temperature control effects and is the main place for the reaction. When too many crystal particles are generated in the product and too quickly, the newly added third jet mixer 1c and second crystal crusher 7b can crush the crystals in time, thereby avoiding the crystal particles from staying in the gas-liquid separation buffer tank 6 and not being able to enter the circulation well. Furthermore, enhancing the insulation and temperature control effect of the gas-liquid separation buffer tank 6 is beneficial to improving the solubility of crystal particles in the mother liquor, reducing the viscosity of the mother liquor, and thus maintaining good fluidity of the mother liquor.

[0078] Example 7

[0079] A fully closed-loop continuous gas-liquid catalytic oxidation tubular reactor, such as Figure 7 As shown, two or more tubular reactor units are combined in series or parallel, and the tubular reactor unit can be any one of the above embodiments 1 to 6 or a combination of several thereof.

[0080] This embodiment is applicable to reactions involving multiple mother liquors and multiple reaction gases, with gas separation required, and the production of crystalline particles in the reaction products. The mother liquor can be a mixed fluid of various liquids, gases, and micron-sized solid particles, and the reaction gases can be one or more feedstock gases. This embodiment is applicable to, but not limited to, reaction processes requiring the adjustment of temperature and pressure at different time periods, reaction residence time, addition of appropriate reactants at different stages, and gas and solid separation. Furthermore, this embodiment achieves the goal of a fully closed-loop, continuous reaction.

[0081] Example 8

[0082] A fully closed-loop continuous gas-liquid catalytic oxidation tubular reactor, such as Figure 8 As shown, it is applied to the production of p-sulfonamidobenzoic acid. This embodiment uses an input section, three tubular reactor units, and an endpoint determination unit in series. The input section can be an independent material allocation unit and also includes auxiliary input interfaces for each unit. The three tubular reactor units are sequentially applied to the initiation reaction section, the mid-term reaction section, and the late reaction section. The endpoint determination unit is the endpoint determination.

[0083] The main process of p-sulfonamide benzoic acid includes the chemical equation:

[0084] The whole process from raw material PTSA to obtaining PSABA solid product includes: dissolution of PTSA, reaction of PTSA with O2, separation to obtain PSABA solid product, separation of PSABA solid product, etc.

[0085] The above main process flow includes the input of raw materials, three reaction sections connected in sequence, and an endpoint determination section, namely: raw material input, initiation reaction section, mid-term reaction section, late reaction section and endpoint determination section.

[0086] The raw material input section includes a 95% wt acetic acid solution prepared by mixing glacial acetic acid and water. A portion of the acetic acid solution is used to dissolve the catalyst and PTSA raw material. After optional preheating and other steps, it is first fed into the initiation reaction section by a booster pump. Furthermore, the acetic acid solution does not react with oxygen. Another portion of the acetic acid solution is used as a solvent and mixed with metered oxygen in a jet mixer to form a gas-liquid mixture. The mixture then enters the tubular reactor under the action of the jet mixer and is ultimately mixed into a gas-liquid mixture, the reaction slurry.

[0087] The slurry temperature in the initiation reaction section will be raised to above 90-100°C, and the gauge pressure will be ~0.3MPa(G). At this time, the reaction between PTSA and O2 is gradually initiated to generate PSABA. Under the action of the circulation pump, the intermediate slurry forms a local small circulation, and the crystal crusher fully crushes the PSABA grains during the circulation process. Furthermore, the raw material input amount can be adjusted through the suction port of the jet mixer. Furthermore, the raw material oxygen flow rate can be adjusted through the oxygen pressure reducing valve and the oxygen flow controller. Further, the system pressure of this reaction section can be adjusted and controlled by the booster pump and the oxygen pressure reducing valve. Further, after the cumulative circulation stays for 10-60 minutes, the slurry in the reaction enters the mid-term reaction section.

[0088] The above-mentioned mid-term reaction section is an exothermic stage, the reaction is relatively violent, a large amount of PSABA is generated and forms crystal particles, the temperature rises significantly, the reaction temperature is controlled at 120-130°C, and the gauge pressure is ~0.4MPa (G). Under the action of the circulation pump in this section, the medium slurry forms a local small circulation, and the crystal crusher fully crushes the PSABA grains under the action of the circulation pump. Furthermore, the raw material input amount can be adjusted through the suction port of the jet mixer. Further, the raw material oxygen flow rate can be adjusted through the oxygen pressure reducing valve and the oxygen flow controller. Further, the system pressure of this reaction section can be adjusted and controlled by the booster pump and the oxygen pressure reducing valve. Further, after the cumulative circulation stays for 10-60 minutes, the slurry in the reaction enters the late reaction section.

[0089] The late reaction section is identical to the mid-stage reaction section, with a reaction temperature of 120-130°C and a gauge pressure of ~0.4 MPa (G). The heat release in this section is lower than that in the mid-stage reaction section. A circulating pump operates to form a localized small circulation of the intermediate slurry, and the crystal crusher, under the action of the circulating pump, fully crushes the PSABA crystals. Furthermore, the raw material input amount can be adjusted through the jet mixer's intake port. Furthermore, the raw material oxygen flow rate can be adjusted through an oxygen pressure reducing valve and an oxygen flow controller. Furthermore, the system pressure in this reaction section can be adjusted and controlled through a booster pump and an oxygen pressure reducing valve. Furthermore, after a cumulative circulation period of 10-60 minutes, the intermediate slurry enters the endpoint determination section.

[0090] The endpoint determination section is used to determine reaction completion. Under normal circumstances, the reaction is complete before the slurry enters the endpoint determination section, achieving a cumulative completion rate of 100%. The oxygen entering this process section through endpoint determination inlet flowmeter f1 is not consumed, but rather exits the system continuously and evenly through endpoint determination outlet flowmeter f2. Since there is no reaction and no temperature rise within this process section, only temperature control is required, maintaining a temperature of 130°C and a gauge pressure of ~0.4 MPa (G). If the flow rates from endpoint determination inlet flowmeter f1 and endpoint determination outlet flowmeter f2 are equal, the reaction is considered complete and the reaction slurry can be removed from the system for post-reaction material separation. If the flow rates from endpoint determination inlet flowmeter f1 and endpoint determination outlet flowmeter f2 are not equal, conversion is considered incomplete. The appropriate valves are opened to pump the reacting slurry back to the subsequent reaction section and into the current section's circulation process to continue the reaction.

[0091] The above is a schematic description of the present invention and its embodiments, which is not restrictive. The drawings show only one embodiment of the present invention, and the actual structure is not limited thereto. Therefore, if a person skilled in the art is inspired by this and, without departing from the purpose of the present invention, designs a structure and embodiment similar to this technical solution without inventiveness, they shall fall within the scope of protection of the present invention.

Claims

1. A tubular reactor unit, characterized in that It includes a first jet mixer, a tubular reactor, and a circulation pump; The tubular reactor comprises a tank body and a spiral coil, wherein the spiral coil is installed in the tank body, one end of the spiral coil is a material inlet, and the other end is a material outlet. The tank body is filled with a heat exchange medium, and the top and bottom of the tank body are respectively provided with a heat exchange medium inlet and outlet. A flow equalizing plate is fixedly installed at a position 0.1D to 1D away from the heat exchange medium inlet and outlet, where D is the inner diameter of the tank body; The internal cavity of the first jet mixer is sequentially provided with an input port, a contraction section, a mixing chamber, a throat section, a diffusion section, and an output port, the contraction section is conical, and the inner diameter gradually decreases along the flow direction of the mother liquid, the large diameter port of the contraction section is connected to the input port, the small diameter port of the contraction section is inserted into the mixing chamber and faces the throat section, the mixing chamber is funnel-shaped, the large diameter port of the mixing chamber is adjacent to the input port, the small diameter port of the mixing chamber is connected to the throat section, the side wall of the mixing chamber is connected to one or more suction ports, a porous material is installed inside the throat section, the pore diameter of the porous material is larger than the diameter of the crystal particles in the fluid, the diffusion section is conical, and the inner diameter gradually expands along the flow direction of the mother liquid, the small diameter end of the diffusion section is connected to the throat section outlet, and the large diameter end of the diffusion section is connected to the output port; The first suction port of the first jet mixer is connected to the reaction material input pipeline, the output port of the first jet mixer is connected to the material inlet of the tubular reactor, and the material outlet pipeline of the tubular reactor is divided into two routes, one of which is connected to the inlet of the circulation pump, and the outlet of the circulation pump is connected to the input port of the first jet mixer; It also includes a gas-liquid separation buffer tank, the material inlet of the gas-liquid separation buffer tank is connected to the material outlet of the tubular reactor, the gas-liquid separation buffer tank has a gas outlet, a side wall liquid outlet and a tank bottom liquid outlet, the tank bottom liquid outlet is connected to the inlet of the circulation pump, the outlet of the circulation pump is connected to the input port of the first jet mixer, and the gas outlet of the gas-liquid separation buffer tank is connected or not connected to the second suction port of the first jet mixer; The invention also includes a first crystal crusher, wherein the inlet of the first crystal crusher is connected to the outlet of the circulation pump, and the outlet of the first crystal crusher is connected to the input port of the first jet mixer; It also includes a second jet mixer, wherein the output port of the second jet mixer is connected to the third suction port of the first jet mixer; It also includes a third jet mixer and a second crystal crusher, the first suction port of the third jet mixer is connected to the material outlet pipeline of the tubular reactor, the output port of the third jet mixer is connected to the inlet of the second crystal crusher, the outlet of the second crystal crusher is connected to the material inlet of the gas-liquid separation buffer tank, and the outlet pipeline of the circulation pump is divided into two routes, one route is connected to the input port of the third jet mixer, and the other route is connected to the inlet of the first crystal crusher.

2. The tubular reactor unit according to claim 1, characterized in that The output port of the jet mixer is equipped with a micro-nano bubble generating component.

3. The tubular reactor unit according to claim 1, characterized in that A turbulent flow component is installed in the spiral coil and / or the tank of the tubular reactor, so that the fluid in the spiral coil and / or the heat exchange medium in the tank is in a turbulent state.

4. The tubular reactor unit according to claim 1, characterized in that The crystal crusher is similar in structure to the jet mixer, but does not include a mixing chamber and a suction port.

5. A tubular reaction system comprising the tubular reactor unit according to any one of claims 1 to 4, which is composed of a plurality of identical or different tubular reactor units connected in series or in parallel.

6. The tubular reaction system according to claim 5, characterized in that: It also includes an endpoint determination unit, which includes a jet mixer for endpoint determination, a gas-liquid separation buffer tank for endpoint determination, a circulation pump for endpoint determination, a crystal crusher for endpoint determination, an air inlet flowmeter for endpoint determination and an air outlet flowmeter for endpoint determination. The first suction port of the jet mixer for endpoint determination is connected to the side wall liquid outlet pipeline of the gas-liquid separation buffer tank of the last tubular reactor unit, the output port of the jet mixer for endpoint determination is connected to the material inlet of the gas-liquid separation buffer tank for endpoint determination, the gas outlet pipeline of the gas-liquid separation buffer tank for endpoint determination is divided into two paths, one path is connected to the air outlet flowmeter for endpoint determination, and the other path is connected to the second suction port of the jet mixer for endpoint determination. The liquid outlet at the bottom of the gas-liquid separation buffer tank for endpoint determination passes through the circulation pump for endpoint determination and the crystal crusher for endpoint determination in sequence, and is then connected to the input port of the jet mixer for determination. The third suction port of the jet mixer for endpoint determination is connected to the reaction gas input pipeline, and the air inlet flowmeter for endpoint determination is installed on the reaction gas input pipeline.

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