CN117244495A - Continuous flow coupling reactor for enhancing mass and heat transfer - Google Patents
Continuous flow coupling reactor for enhancing mass and heat transfer Download PDFInfo
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/82—Combinations of dissimilar mixers
- B01F33/821—Combinations of dissimilar mixers with consecutive receptacles
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0046—Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
Abstract
The invention discloses a continuous flow coupling reactor for enhancing mass and heat transfer, which comprises a shell; the premixing reactor, the tubular reactor and the dynamic mixing strengthening reactor are arranged in the shell from top to bottom, and the outlet of the premixing reactor is communicated with the tubular reactor distributor; after the materials are mixed and reacted, the reactants are sent to a feed tube of a tube-array tubular reactor; the inlet of the dynamic mixing strengthening reactor is communicated with the inlet of the feeding tube array, and the dynamic mixing strengthening reactor is used for mixing reactants efficiently; the outlet of the dynamic mixing strengthening reactor is communicated with a reflux tube of the tube array type reactor, the discharged materials of the dynamic mixing strengthening reactor react in the reflux tube array and the circulating tube array, and part of the materials circulate in the circulating tube array; the outlet of the reflux tube and the upper port of the circulating tube send the reactant out of the reactor through a liquid collecting disc. The invention relates to the technical field of reaction system design, and has the advantages of continuous and efficient mixing and enhanced mass and heat transfer performance.
Description
Technical Field
The invention relates to the technical field of reaction system design, in particular to a continuous flow coupling reactor for enhancing mass and heat transfer.
Background
The advantages of continuous flow reactions over batch reactions are mainly manifested in their efficiency, control and safety. High efficiency: continuous flow reactions can achieve a continuous reaction process, thereby increasing the utilization and throughput of the reactor. Materials continuously enter and leave the reactor, which can react at a higher rate without waiting for the reaction to complete and cleaning up the reactants. Control of: the continuous flow reaction is easier to control and regulate. By adjusting parameters such as the feeding rate, the reaction temperature, the proportion of reaction materials and the like, the reaction conditions can be controlled more accurately, so that the reaction process is optimized, and the selectivity and the yield are improved. Safety: continuous flow reactions can reduce risk factors during the reaction. The liquid holdup of the materials in the reactor is less, the residence time is shorter, the accumulation of heat and pressure is relatively smaller, and the risks of explosion and accidents can be reduced. The adoption of continuous flow reaction to strengthen chemical process becomes an important development direction of chemical industry and is always a research hot spot. The implemented path is mainly based on two aspects of new equipment and new technology, including two aspects of process strengthening equipment and a process strengthening method. In some cases, the two aspects are interrelated, interpenetrating, and intersecting.
In the prior art, (1) the reactor of CN202310245903.5, a tubular reactor and an impinging stream reactor are employed, and by rapid mixing in the impinging stream reactor, good mass transfer conditions are provided. The reaction can occur and equilibrate in a short time due to the rapid mixing and high flow characteristics of the reactants. The main problem is the short residence time of the impinging stream material, which, in addition to the difficulty in arranging multiple stages of processes, limits the range of applications for pure impinging streams. While balanced processes, simple impinging streams may enhance inter-phase transfer to accelerate, it is difficult to ensure that the process is completed to the desired degree and the final absorption or conversion may not reach the desired level. The heat exchange area is small, and the method is not suitable for severe reactions and reactions with slower reaction speeds, such as nitrification, sulfonation and oxidation of high-concentration sewage. (2) Yang Tao, yao Wenbo, et al, "impinging stream catalytic ozonation-membrane filtration treatment of emulsified oil wastewater", chemical environmental protection, 2022, volume 42, 6 th phase, 678-685, treatment of emulsified oil wastewater by impinging stream catalytic ozonation-membrane filtration process, and control effect of impinging stream catalytic ozonation on membrane pollution under continuous operation process. The main problems are short reaction residence time, small heat exchange area, low reaction temperature and influence on the treatment effect. (3) The reactor of CN 115041119A adopts a hypergravity reactor, and has high mass transfer effect: the supergravity reactor improves the mass transfer effect by increasing the contact area and the mixing degree between the gas phase and the liquid phase. The main problems are short residence time, large liquid holdup of the reactor, small heat exchange area and potential safety hazard. (5) The reactor of CN 102432410B realizes the continuous production of pipelining, and has the main problems of low efficiency of parallel flow reaction stages and high production efficiency. (6) The reactor of CN 107793316B has the main problems of thinner micro-reactor channels, easy blockage, inconvenient maintenance, short residence time and unfavorable reaction with slower reaction speed. (7) In the reactor of CN 104710062A, ultrasonic waves are introduced into mechanical vibration, so that local intense vortex and shearing force are generated, the mixing of reaction materials is further promoted, the interfacial reaction rate is increased, and the ultrasonic waves can damage the aggregation of solid particles, so that the solid particles are easier to react. The main problem is the short processing time, which is not suitable for relatively slow reactions and exothermic or endothermic reactions.
The existing continuous flow technology mostly adopts a mode of combining two reactors and three reactors in parallel, has the advantages of long heat transfer distance, small heat exchange area, low heat transfer efficiency, possibility of high temperature of a local reactor, short residence time and low reaction stage efficiency, particularly has potential safety hazard for a fast and strongly exothermic reaction system, fully utilizes the respective advantages of various reinforced mass transfer and heat transfer reactors, and is particularly important to develop the reinforced mass transfer and heat transfer continuous flow coupling reactors.
Disclosure of Invention
Aiming at the problems of long heat transfer distance, small heat exchange area, low heat transfer efficiency, high temperature possibility of a local reactor, short residence time and low reaction stage efficiency of the existing reactor, and potential safety hazards of a reaction system with rapid and strong heat release, the invention provides the continuous flow coupling reactor for enhancing mass transfer and heat transfer.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a continuous flow coupling reactor for enhancing mass and heat transfer comprises a shell, a premixing reactor, a shell and tube reactor and a dynamic mixing enhancement reactor which are arranged in the shell and are connected up and down, a material first inlet and a material second inlet which pass through the shell and are connected with the premixing reactor, a system material outlet which passes through the shell and is connected with the shell and tube reactor, a heat exchange medium inlet which passes through the shell and is arranged at the lower part of the shell, and a heat exchange medium outlet which passes through the shell and is arranged at the upper part of the shell.
Further, the premixing reactor is provided with the first material inlet, the second material inlet and a discharging port of the premixing reactor or a tubular reactor distributor;
the premixing reactor can introduce materials through at least the first material inlet and the second material inlet, and the direction of the first material inlet and the direction of the second material inlet are axially opposite, tangentially opposite or tangentially identical, so that impact and rotational flow can be conveniently generated, cavitation is generated, micro-nano mixing is realized, and the reaction is enhanced.
Further, the premixing reactor can be provided with at least one ultrasonic feeder which is arranged at the middle part or the middle upper part of the premixing reactor and is used for assisting in strengthening the mixing reaction process;
the ultrasonic frequency range of the ultrasonic feeder is 1.8 MHz-5 MHz.
Further, the tubular reactor is provided with a feeding tubular, a reflux tubular and a circulating tubular;
the feeding tube nest is positioned in the middle of the tube nest tube reactor, the backflow tube nest is positioned outside the circulation tube nest, and the circulation tube nest is positioned between the backflow tube nest and the feeding tube nest;
the number of the feeding tubes is at least one, and the number of the reflux tubes and the number of the circulating tubes are at least two;
at least one of the feed tubes is connected to the premix reactor outlet of the premix reactor.
Further, the dynamic mixing strengthening reactor comprises a dynamic mixing strengthening reactor feed inlet, a circulating tube array feed inlet, a dynamic mixing strengthening reactor discharge outlet, a rotating shaft, a high-speed rotating member and a motor;
the material inlet of the dynamic mixing strengthening reactor is connected with the material inlet of the material inlet tube, the material outlet of the material inlet tube is connected with the material outlet tube, the material outlet of the dynamic mixing strengthening reactor is connected with the material outlet tube, the material discharged from the dynamic mixing strengthening reactor reacts in the material outlet tube and the material outlet tube, and part of the material circulates in the material outlet tube, and the material outlet tube upper port of the material outlet tube discharge the final material from the material outlet tube of the system through a liquid collecting disc;
the feed inlet of the dynamic mixing strengthening reactor vertically enters the high-speed rotating member from top to bottom from the central part of the high-speed rotating member, the feed inlet of the circulating tube array is concentrated at the edge of the central part of the high-speed rotating member, a certain gap is reserved between the feed inlet of the dynamic mixing strengthening reactor and the feed inlet of the circulating tube array and the high-speed rotating member, the discharge outlet of the dynamic mixing strengthening reactor is positioned at two sides of the feed inlet of the dynamic mixing strengthening reactor and is connected with the reflux tube array, a motor is positioned outside the bottom of the shell and vertically opposite to the center of the dynamic mixing strengthening reactor, a filler seal, a mechanical seal, a dry gas seal or a magnetic coupling is adopted, the motor drives the high-speed rotating member positioned at the central position of the dynamic mixing strengthening reactor to rotate at high speed by virtue of electric power driving the rotating shaft, and radial diffusion and mixing are realized under the centrifugal force effect, and high material is realizedMixing, strengthening mass transfer and heat transfer, and strengthening reaction;
at least one group of discharge ports of the dynamic mixing strengthening reactor are connected with the reflux tube array of the tube array tubular reactor;
at least one group of circulating tubulars of the tubular reactor are communicated with the discharge port of the dynamic mixing strengthening reactor.
Further, the premixing reactor, the tubular reactor and the dynamic mixing strengthening reactor are arranged in the shell, and heat exchange is realized through the heat exchange medium inlet which passes through the shell and is arranged at the lower part of the shell and the heat exchange medium outlet which passes through the shell and is arranged at the upper part of the shell.
Further, the pre-mix reactor may be subject to efficient dispersion and cavitation;
the premixing reactor has a microscopic size of between 0.5 microns and 2000 microns.
Further, at least one feeding tube may be disposed between the tube reactor and the dynamic mixing enhancement reactor, and connected to the feeding port of the dynamic mixing enhancement reactor, and sent to the high-speed rotating member of the dynamic mixing enhancement reactor.
Further, at least one group of circulation tubes can be arranged between the tube type reactor and the dynamic mixing strengthening reactor and communicated with the dynamic mixing strengthening reactor, and self-priming circulation reaction is realized by utilizing the rotation of the high-speed rotating member of the dynamic mixing strengthening reactor.
Further, the micro-size of the dynamic mixing enhancement reactor is between 0.5 microns and 3000 microns, and the rotating speed of the rotating member is between 500 rpm and 5000 rpm.
Further, the characteristic diameter ratio of the tubular reactor is between 1:100 and 1:5;
the tubular reactor is internally provided with a filler and a static mixing member so as to realize interface updating, heterogeneous catalysis and residence time extension.
Further, the ratio of the residence time of the fluid in the premixing reactor to the residence time of the fluid in the tubular reactor is between 1:200 and 1:50;
the ratio of the residence time of the fluid in the shell-and-tube reactor to the residence time of the fluid in the dynamic mixing enhancement reactor is between 50:1 and 300:1.
Compared with the prior art, the invention has the following advantages:
the invention provides a continuous flow coupling reactor for enhancing mass transfer and heat transfer, which combines the characteristics of heat exchange of a tube array heat exchanger according to the theoretical basis of impinging flow/rotational flow, ultrasonic wave, tube array tube reactor and centrifugal rotation for enhancing mass transfer and heat transfer, prolongs the reaction time and quickens the updating of an interface by utilizing the tube array tube reactor, increases the heat exchange area, reasonably optimizes a premixing reactor, the tube array tube reactor, a dynamic mixing enhanced reactor and a shell, ensures the full mixing and dead angle-free forced circulation of materials by a strong dynamic rotation stirring centrifugal force self-priming circulation technology, greatly improves the mass transfer and heat transfer efficiency, ensures the heat exchange of the tube array surface and the shell side under any condition, avoids the possibility of wholly or partially high temperature, ensures the high-efficiency mixing, mass transfer and heat transfer performance of the reactor, improves the efficiency, the conversion rate and the yield of a reaction stage, realizes isothermal continuous reaction, reasonably sets the heat exchange area of the reactor, fundamentally ensures the safety and eliminates the hidden trouble.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. In the drawings:
FIG. 1 is a schematic diagram of a continuous flow coupled reactor for enhanced mass and heat transfer according to an embodiment of the present invention;
FIG. 2 is a cross-sectional view A-A of FIG. 1 according to an embodiment of the present invention;
FIG. 3 is a cross-sectional view B-B of FIG. 1 according to an embodiment of the present invention;
FIG. 4 is a cross-sectional view of FIG. 1 according to an embodiment of the present invention;
reference numerals illustrate:
1. a housing; 2. a premixing reactor; 201. a material first inlet; 202. a material second inlet; 203. a premixing reactor discharge/the tubular reactor distributor; 204. an ultrasonic feeder; 3. a shell and tube reactor; 301. a feed shell and tube reactor; 302. a reflux shell-and-tube reactor; 303. a circulating tubular reactor; 4. a dynamic mixing strengthening reactor; 401. a feed inlet of the dynamic mixing strengthening reactor; 402. a dynamic mixing strengthening reactor circulating tube feeding port; 403. a discharge port of the dynamic mixing strengthening reactor; 404. a rotating shaft; 405. a high-speed rotating member; 406. a motor; 5. a system material outlet; 6. a heat exchange medium inlet; 7. a heat exchange medium outlet; 8. a liquid collecting disc.
Detailed Description
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
In the description of the present invention, it should be noted that the azimuth or positional relationship indicated by the terms "upper", "lower", "inner", "back", etc. are based on the azimuth or positional relationship shown in the drawings, and are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or element referred to must have a specific azimuth, be constructed and operated in a specific azimuth, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
The invention will be described in detail below with reference to the drawings in connection with embodiments.
Example 1
The embodiment relates to a continuous flow coupling reactor for enhancing mass and heat transfer, which is shown in fig. 1-4, and specifically comprises a shell 1, a premixing reactor 2, a tubular reactor 3 and a dynamic mixing enhancement reactor 4 which are arranged in the shell 1 and are connected up and down, a first material inlet 201 and a second material inlet 202 which are connected with the premixing reactor 2 through the shell 1, a system material outlet 5 connected with the tubular reactor 3 through the shell 1, a heat exchange medium inlet 6 arranged at the lower part of the shell 1 through the shell 1, and a heat exchange medium outlet 7 arranged at the upper part of the shell 1 through the shell 1.
The premixing reactor 2 is provided with a material first inlet 201, a material second inlet 202 and a premixing reactor discharge outlet/the tubular reactor distributor 203; the premixing reactor 2 can introduce materials through at least a first material inlet 201 and a second material inlet 202, and the first material inlet 201 and the second material inlet 202 can be opposite in axial direction and tangential direction, and also can be opposite in tangential direction, so that impact and rotational flow can be generated, cavitation can be generated, micro-nano mixing can be realized, and the reaction can be enhanced.
A premixing reactor 2, at least one ultrasonic feeder 204 can be arranged, and the ultrasonic feeder 204 is arranged at the middle part or the middle upper part of the premixing reactor 2 to assist in strengthening the mixing reaction process; the ultrasonic frequency range of the ultrasonic feed 204 is 1.8 khz-5 mhz.
The shell-and-tube reactor 3 is provided with a feed shell-and-tube 301, a reflux shell-and-tube 302 and a circulation shell-and-tube 303; the feeding tube array 301 is positioned in the middle of the tube array reactor 3, the reflux tube array 302 is positioned outside the circulating tube array 303, and the circulating tube array 303 is positioned between the reflux tube array 302 and the feeding tube array 301; the number of the feeding pipes 301 is at least one, and the number of the reflux pipes 302 and the circulation pipes 303 is at least two; at least one feed tube array 301 is in communication with the premix reactor outlet 203 of the premix reactor 2; the dynamic mixing and strengthening reactor 4 comprises a dynamic mixing and strengthening reactor feed inlet 401, a circulating tube feed inlet 402, a dynamic mixing and strengthening reactor discharge outlet 403, a rotating shaft 404, a high-speed rotating member 405 and a motor 406.
The feed inlet 401 of the dynamic mixing strengthening reactor is communicated with the feed tube array reactor 301, the material inlets below the reflux tube array 302 and the circulation tube array 303 are communicated with the dynamic mixing strengthening reactor, the outlet 403 of the dynamic mixing strengthening reactor is communicated with the reflux tube array 302 of the tube array reactor, the discharged materials of the dynamic mixing strengthening reactor react in the reflux tube array 302 and the circulation tube array 303, partial materials circulate in the circulation tube array 303, and the outlet of the reflux tube array 302 and the upper port of the circulation tube array 303 discharge the final materials from the system material outlet 5 through the liquid collecting disc 8.
The feed inlet 401 of the dynamic mixing strengthening reactor vertically enters the high-speed rotating member 405 from top to bottom from the center of the high-speed rotating member 405, the circulating tube array feed inlet 402 is concentrated at the edge of the center of the high-speed rotating member 405, a certain gap is reserved between the feed inlet 401 of the dynamic mixing strengthening reactor and the circulating tube array feed inlet 402 of the dynamic mixing strengthening reactor and the high-speed rotating member 405, the discharge outlets 403 of the dynamic mixing strengthening reactor are positioned at two sides of the dynamic mixing strengthening reactor 401 and are connected with the backflow tube array tubular reactor 302, the motor 406 is positioned outside the bottom of the shell 1 and vertically opposite to the center of the dynamic mixing strengthening reactor 4, and the motor 406 drives the high-speed rotating member 405 positioned at the center of the dynamic mixing strengthening reactor to rotate at high speed by virtue of the electric drive rotating shaft 404, so that the radial diffusion and mixing are realized, the mass transfer and heat transfer are strengthened and the reaction are strengthened under the centrifugal force effect; at least one set of dynamic mixing enhancement reactor discharge ports 403 are connected to the return train 302 of the tubular reactor 3.
At least one set of recycle tubes 303 of the tube array reactor 3 is in communication 403 with a dynamic mixing enhancement reactor.
The components of the premixing reactor 2, the tubular reactor 3 and the dynamic mixing strengthening reactor 4 which are arranged in the shell 1 exchange heat through a heat exchange medium inlet 6 which is arranged at the lower part of the shell 1 and a heat exchange medium outlet 7 which is arranged at the upper part of the shell 1 and passes through the shell 1.
The premixing reactor 2 can generate efficient dispersion and cavitation; the micro-size of the premixing reactor 2 is between 0.5 and 2000 microns.
At least one dynamic reactor feeding tube 301 can be arranged between the tube array type reactor 3 and the dynamic mixing enhancement reactor 4 and is communicated with a dynamic mixing enhancement reactor feeding hole 401 of the dynamic mixing enhancement reactor 4, and the dynamic mixing enhancement reactor feeding hole is sent into a high-speed rotating component 405 of the dynamic mixing enhancement reactor 4.
At least one group of circulating tube reactors 303 can be arranged between the tube reactors 3 and the dynamic mixing strengthening reactor 4 and communicated with the dynamic mixing strengthening reactor 4, and self-priming circulating reaction is realized by utilizing the rotation of a high-speed rotating member 405 of the dynamic mixing strengthening reactor 4.
The dynamic mixing enhancement reactor 4 has a microscopic size of between 0.5 microns and 3000 microns and a rotating member rotation speed of between 500 rpm and 5000 rpm.
The characteristic diameter ratio of the tubular reactor 3 is between 1:100 and 1:5.
The shell and tube reactor 3 is internally provided with packing and static mixing members to facilitate interface renewal, heterogeneous catalysis and prolonged residence time.
The ratio of the residence time of the fluid in the premixing reactor 2 to the residence time of the fluid in the tubular reactor 3 is between 1:200 and 1:50; the ratio of the residence time of the fluid in the shell-and-tube reactor 3 to the residence time of the fluid in the dynamic mixing enhancement reactor 4 is between 50:1 and 300:1.
Example 2
The continuous synthesis of the nitrochlorobenzene by adopting the intensified mass and heat transfer continuous flow coupling reactor of the invention.
The invention adopts chlorobenzene (CP, mass fraction 99%), concentrated sulfuric acid (CP, mass fraction 98%) and nitric acid (CP, mass fraction 65% -68%) as raw materials, and adopts the reinforced mass transfer and heat transfer continuous flow coupling reactor to continuously synthesize nitrochlorobenzene. The sulfuric acid and the nitric acid firstly establish circulation in the continuous flow nitration reactor, chlorobenzene is preheated and then continuously and stably enters the continuous flow nitration reactor, and the material flow and the reaction condition are accurately measured and controlled. When the residence time is 70s, the temperature is 80 ℃, the mixed acid ratio (the molar ratio of nitric acid to sulfuric acid) =1:1.5, the comparison (the molar ratio of nitric acid to chlorobenzene) =1:1, the ultrasonic frequency is 2.6 kilohertz, the rotating speed of a rotating member of the dynamic mixing strengthening reactor is 3000 revolutions per minute, the micro negative pressure of the reactor is achieved, the neighbor contrast in the product is between 0.68 and 0.80, the single pass conversion rate of chlorobenzene is 83.26%, and the selectivity of mononitrochlorobenzene is 93.60%. After continuous nitration, the reaction residence time is greatly reduced, and the ortho-contrast ratio of the mononitrochlorobenzene is obviously improved. The nitration of aromatic compounds is a rapid and strong exothermic reaction, and the reaction heat is rapidly removed from cooling water through the tube wall by adopting the nitration process, so that the potential risk possibly caused by intermittent operation can be reduced, and compared with the traditional kettle type process, the continuous nitration in the continuous flow reactor is safer and more efficient.
Example 3
Pretreatment of cimetidine pharmaceutical wastewater by adopting the enhanced mass transfer and heat transfer continuous flow coupling reactor
Cimetidine pharmaceutical wastewater has high COD and complex components. The method comprises the steps of utilizing the enhanced mass transfer and heat transfer continuous flow coupling reactor, pretreating the wastewater by using Fenton reagent, and firstly establishing circulation of the wastewater in the enhanced mass transfer and heat transfer continuous flow coupling reactor, wherein FeSO is carried out in the enhanced mass transfer and heat transfer continuous flow coupling reactor 4 After preheating, the waste water and the same water are continuously and stably fedInto a continuous flow reactor, the flow and reaction conditions are precisely metered. Optimal reaction conditions: h 2 O 2 The mass concentration is 3000mg/L, feSO 4 The mass concentration is 750mg/L, the ultrasonic frequency is 2.0 ten thousand hertz, the rotating speed of a dynamic mixing strengthening reactor rotating member is 3000 rpm, the oxidation time is 80s, the pH is 3.5, the reaction temperature is 75 ℃, and the COD removal rate is more than 56 percent.
Example 4
Pretreatment of glyphosate production wastewater by adopting the enhanced mass and heat transfer continuous flow coupling reactor
The invention uses the reinforced mass transfer and heat transfer continuous flow coupling reactor, uses copper sulfate and zinc nitrate solution as catalyst, and adopts catalytic wet oxidation method to pretreat the waste water of glyphosate production. Raw water of the process: COD 46300mg/L, total phosphorus 6800mg/L, inorganic phosphorus-, pH 8.0. The pH value of the wastewater is regulated to 8.5 by using 1mol/LNa0H solution, the wastewater is sent into a preheater by a high-pressure metering pump, the air pressure of a high-pressure steel bottle is regulated to 3MPa by a valve, the mass controller controls the air flow to be mixed with the wastewater in the preheater, the wastewater is heated to 220 ℃ by an automatic temperature-control electric heating device and then is sent into a reactor for oxidation reaction, the treated water mixture is condensed by a condenser, and the water mixture is respectively discharged after being separated by a gas-liquid separator. The residence time of the wastewater in the reactor is 100s, the ultrasonic frequency is 2.8 MHz, and the rotating speed of the rotating component of the dynamic mixing strengthening reactor is 3500 rpm. The water quality analysis results after the catalytic wet oxidation of the wastewater comprise 7600mg/L of COD, 6800mg/L of total phosphorus, 6500mg/L of inorganic phosphorus, 85% of COD removal rate and 99.6% of organic phosphorus removal rate.
Claims (12)
1. A continuous flow coupling reactor for enhancing mass and heat transfer is characterized in that: the device comprises a shell (1), a premixing reactor (2), a shell and tube reactor (3) and a dynamic mixing strengthening reactor (4) which are arranged in the shell (1) and are connected up and down, a first material inlet (201) and a second material inlet (202) which are connected with the premixing reactor (2) and pass through the shell (1), a system material outlet (5) connected with the shell and tube reactor (3), a heat exchange medium inlet (6) which is arranged at the lower part of the shell (1) and a heat exchange medium outlet (7) which is arranged at the upper part of the shell (1) and passes through the shell (1) and are arranged in the shell (1).
2. The mass and heat transfer enhanced continuous flow coupled reactor according to claim 1, wherein: the premixing reactor (2) is provided with the first material inlet (201), the second material inlet (202) and a discharging outlet (203) of the premixing reactor or a tubular reactor distributor;
the premixing reactor (2) can introduce materials through at least the first material inlet (201) and the second material inlet (202), and the first material inlet (201) and the second material inlet (202) are axially opposite, tangentially opposite or tangentially identical in orientation so as to facilitate impact and rotational flow, generate cavitation, realize micro-nano mixing and strengthen reaction.
3. The mass and heat transfer enhanced continuous flow coupled reactor according to claim 1, wherein: the premixing reactor (2) can be provided with at least one ultrasonic feeder (204), and the ultrasonic feeder (204) is arranged in the middle part or the middle upper part of the premixing reactor (2) to assist in strengthening the mixing reaction process;
the ultrasonic frequency range of the ultrasonic feeder (204) is 1.8 MHz-5 MHz.
4. The mass and heat transfer enhanced continuous flow coupled reactor according to claim 1, wherein: the shell and tube reactor (3) is provided with a feeding shell and tube (301), a reflux shell and tube (302) and a circulating shell and tube (303);
the feeding tube nest (301) is positioned in the middle of the tube nest reactor (3), the reflux tube nest (302) is positioned outside the circulating tube nest (303), and the circulating tube nest (303) is positioned between the reflux tube nest (302) and the feeding tube nest (301);
the number of the feeding pipes (301) is at least one, and the number of the reflux pipes (302) and the number of the circulating pipes (303) are at least two;
at least one of the feed trains (301) is connected to the premixing reactor outlet (203) of the premixing reactor (2).
5. The mass and heat transfer enhanced continuous flow coupled reactor according to claim 4, wherein: the dynamic mixing strengthening reactor (4) comprises a dynamic mixing strengthening reactor feed inlet (401) and a circulating tube array feed inlet (402), a dynamic mixing strengthening reactor discharge outlet (403), a rotating shaft (404), a high-speed rotating component (405) and a motor (406);
the feed inlet (401) of the dynamic mixing strengthening reactor is connected with the feed tube (301), the reflux tube (302) and the material inlet below the circulation tube (303) are communicated with the dynamic mixing strengthening reactor, the discharge outlet (403) of the dynamic mixing strengthening reactor is communicated with the reflux tube (302), the discharged material of the dynamic mixing strengthening reactor reacts in the reflux tube (302) and the circulation tube (303), part of the material circulates in the circulation tube (303), and the outlet of the reflux tube (302) and the upper port of the circulation tube (303) discharge the final material from the material outlet (5) of the system through a liquid collecting disc (8);
the dynamic mixing strengthening reactor feed inlet (401) vertically enters the high-speed rotating member (405) from top to bottom from the center of the high-speed rotating member (405), the circulating tube array feed inlet (402) is concentrated at the edge of the center of the high-speed rotating member (405), a certain gap is reserved between the dynamic mixing strengthening reactor feed inlet (401) and the circulating tube array feed inlet (402) and the high-speed rotating member (405), the dynamic mixing strengthening reactor discharge outlet (403) is positioned at two sides of the dynamic mixing strengthening reactor feed inlet (401) and is connected with the backflow tube array (302), the motor (406) is positioned outside the bottom of the shell (1) and vertically opposite to the center of the dynamic mixing strengthening reactor (4), and the motor (406) drives the high-speed rotating member (405) positioned at the center of the dynamic mixing strengthening reactor by virtue of electric drive of the rotating shaft (404) to rotate at high speed by adopting a packing seal or a mechanical seal or a dry gas seal or a magnetic coupling, so that the radial mixing and the mass transfer and the strengthening of materials are realized under the high-speed rotation effect and the high-speed mixing and the strengthening effect of the materials are realized;
at least one group of discharge ports (403) of the dynamic mixing strengthening reactor are communicated with the reflux tube array (302) of the tube array reactor (3);
at least one group of circulating tubulars (303) of the tubular reactor (3) is communicated with a discharge outlet (403) of the dynamic mixing strengthening reactor.
6. The mass and heat transfer enhanced continuous flow coupled reactor according to claim 1, wherein: the components arranged in the shell (1) are the premixing reactor (2), the tubular reactor (3) and the dynamic mixing strengthening reactor (4), and heat exchange is realized through the heat exchange medium inlet (6) which passes through the shell (1) and is arranged at the lower part of the shell (1) and the heat exchange medium outlet (7) which passes through the shell (1) and is arranged at the upper part of the shell (1).
7. The mass and heat transfer enhanced continuous flow coupled reactor according to claim 1, wherein: the premixing reactor (2) can generate efficient dispersion and cavitation;
the premixing reactor (2) has a microscopic size of between 0.5 and 2000 microns.
8. The mass and heat transfer enhanced continuous flow coupled reactor according to claim 5, wherein: at least one feeding tube (301) can be arranged between the tube array type reactor (3) and the dynamic mixing strengthening reactor (4) and connected with a feeding port (401) of the dynamic mixing strengthening reactor (4), and the feeding tube is sent into the high-speed rotating component (405) of the dynamic mixing strengthening reactor (4).
9. The mass and heat transfer enhanced continuous flow coupled reactor according to claim 5, wherein: at least one group of circulating tubes (303) can be arranged between the tube array type reactor (3) and the dynamic mixing strengthening reactor (4) and communicated with the dynamic mixing strengthening reactor (4), and self-priming circulation reaction is realized by utilizing the rotation of the high-speed rotating member (405) of the dynamic mixing strengthening reactor (4).
10. The mass and heat transfer enhanced continuous flow coupled reactor according to claim 1, wherein: the micro-size of the dynamic mixing strengthening reactor (4) is between 0.5 micrometers and 3000 micrometers, and the rotating speed of the rotating member is between 500 and 5000 revolutions per minute.
11. The mass and heat transfer enhanced continuous flow coupled reactor according to claim 1, wherein: the characteristic diameter ratio of the tubular reactor (3) is between 1:100 and 1:5;
the tubular reactor (3) is internally provided with a filler and a static mixing member so as to realize interface updating, heterogeneous catalysis and prolong the residence time.
12. The mass and heat transfer enhanced continuous flow coupled reactor according to claim 1, wherein: the ratio of the residence time of the fluid in the premixing reactor (2) to the residence time of the fluid in the tubular reactor (3) is between 1:200 and 1:50;
the ratio of the residence time of the fluid in the shell-and-tube reactor (3) to the residence time of the fluid in the dynamic mixing enhancement reactor (4) is between 50:1 and 300:1.
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