CN114699939A - Hypergravity gas mixing device for cutting bubbles step by step and application thereof - Google Patents
Hypergravity gas mixing device for cutting bubbles step by step and application thereof Download PDFInfo
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Abstract
The invention discloses a supergravity gas mixing device for cutting bubbles step by step and application thereof, wherein the device comprises a motor, a rotating shaft, a shell, a gas-liquid inlet, a gas supplementing port, a flow guide piece, a gas-liquid outlet, a rotor and a bubble crushing part; the rotating shaft serving as an output shaft of the motor extends into the shell from the center of the top end of the shell and is connected with the rotor to drive the rotor to rotate; a gas-liquid outlet and a plurality of air supplementing ports are arranged outside the shell from top to bottom; the rotor is internally provided with a gas crushing part, and the multistage rotor structure is provided with the gas crushing part with smaller and smaller aperture from bottom to top. The device can realize effectively regulating and controlling the bubble size through the rotational speed of adjusting hypergravity device on the one hand, and multistage tonifying qi is assisted to on the other hand, and the while is through the synergistic effect of the multistage rotor who loads the broken part of hydrophilic/hydrophobic bubble in different apertures, realizes cutting step by step of bubble, makes the bubble size that obtains less, bubble size distribution homogeneous.
Description
Technical Field
The invention belongs to the field of a supergravity reactor and application thereof, and particularly relates to a supergravity gas mixing device for cutting bubbles step by step and application thereof.
Background
Gas-liquid mixing processes are widely found in the chemical industry. The gas-liquid mixing process greatly influences the gas-liquid mass transfer process, and the research on the gas-liquid mass transfer strengthening technology has important significance in shortening the process flow, reducing the equipment size, reducing the investment and the operation cost and the like. The supergravity technology with rotating bed as core equipment is one of the effective reinforced gas-liquid mass transfer technology.
The problem of poor gas-liquid mass transfer is often existed in the gas-liquid mass transfer process involving insoluble gases such as hydrogen, oxygen, carbon monoxide and the like, so that the macroscopic reaction rate is limited by the gas-liquid mass transfer rate. With the development of gas-liquid mass transfer strengthening technology in recent years, large bubbles are broken to form micro bubbles, the gas-liquid mass transfer area is increased, the gas-liquid mass transfer process is further strengthened, and the gas-liquid mass transfer rate is matched with the intrinsic reaction rate, so that the macroscopic reaction rate is improved, the reaction time is shortened, and the intrinsic safety of the system is improved. Chinese patent 201910163989.0 discloses a super-gravity sodium microbubble generating device and reaction system, which can realize the effective regulation of the size of microbubbles and the preparation of microbubbles with small size and uniform size distribution in a large batch at present. Therefore, the device for rapidly and controllably preparing the microbubbles with small size and uniform size distribution, which has simple equipment structure and large gas flux, is developed, and has important practical application value for improving the problems of high energy consumption, high material consumption and high pollution in the chemical industry and realizing national energy conservation and emission reduction.
Disclosure of Invention
The invention provides a hypergravity gas mixing device for cutting bubbles step by step; the device mainly aims at the gas-liquid mass transfer process that indissolvable gases such as hydrogen, oxygen, carbon monoxide participate in, liquid phase is as the continuous phase in the device, the gaseous phase is as the dispersed phase, liquid phase and some gaseous phases pass through the gas-liquid import of casing lower part and get into the inside of hypergravity device, other some gaseous phases carry out many times tonifying qi through the tonifying qi mouth, improve its gas content rate, get into the gas-liquid mixture of hypergravity device through the gas-liquid import, drive the rotor high-speed rotation through the motor, the gas crushing part who loads in the rotor shears the gas-liquid mixture, the gas crushing part that gas-liquid mixture after the shearing gets into next stage rotor with the gas that the tonifying qi mouth got into together and shears, and from bottom to top, the aperture of the gas crushing part that loads in the rotor is littleer, finally the gas-liquid mixture leaves the device from the gas-liquid export. Finally, the rapid and large-scale controllable preparation of microbubbles with the diameter of 10-300 mu m is realized, and the size distribution of the microbubbles is uniform.
The second technical problem to be solved by the invention is to provide an application of the supergravity gas mixing device for cutting bubbles step by step.
In order to solve the first technical problem, the invention adopts the following technical scheme:
a hypergravity gas mixing device for cutting bubbles step by step comprises a motor, a rotating shaft, a shell, a gas-liquid inlet, a gas supplementing port, a gas-liquid outlet, a multi-stage rotor and a bubble crushing part;
the rotating shaft serving as an output shaft of the motor extends into the shell from the center of the top end of the shell and is connected with the rotor to drive the rotor to rotate;
a plurality of flow guide pieces are fixedly arranged on the inner wall of the shell and positioned between each stage of rotor and the shell;
the multistage rotor is internally loaded with gas crushing parts, and the aperture of the gas crushing parts loaded in the multistage rotor is smaller and smaller from bottom to top;
a gas-liquid outlet is formed in the upper outer part of the shell; air supply ports are arranged on the shell which transversely corresponds to the gaps between the rotors at all levels;
the bottom of the shell is provided with a gas-liquid inlet;
and a plurality of pore channels which are convenient for gas-liquid to pass through are arranged at the bottom of the rotor.
Preferably, the multi-stage rotor in the shell is 3-30 layers, and the distance between every two layers is 10-50 mm; more preferably, the multi-stage rotor in the housing has 3-5 layers.
Preferably, the number of the air supplementing ports is 2-29.
Preferably, the gap between the flow guide piece and the rotor is 2-10 mm.
Preferably, the surface of the gas breaking part is a hydrophilic surface layer or a hydrophobic surface layer.
Preferably, the bubble-breaking part is a nano-micron porous filler, a nano-micron porous sintered film.
Preferably, the aperture of the gas crushing parts loaded in the multistage rotor is decreased in proportion from bottom to top.
Preferably, the plurality of pore passages arranged at the bottom of each stage of rotor are symmetrically and uniformly distributed around the axis of the rotating shaft.
Preferably, a gas flow control valve is arranged at the gas-liquid inlet.
Preferably, the air supplementing openings are provided with one-way valves.
In order to solve the second technical problem, the invention adopts the following technical scheme:
the application of the supergravity gas mixing device for cutting the bubbles step by step comprises a gas-liquid mixing process in a gas-liquid mixing process or a gas-liquid-solid catalytic reaction process.
Preferably, the gas-liquid mixing process refers to a mixing process involving a poorly soluble gas; more preferably, the sparingly soluble gas is one of hydrogen, oxygen, ozone, carbon monoxide, carbon dioxide, nitric oxide, and lower hydrocarbons.
Any range recited herein is intended to include the endpoints and any number between the endpoints and any subrange subsumed therein or defined therein.
The starting materials of the present invention are commercially available, unless otherwise specified, and the equipment used in the present invention may be any equipment conventionally used in the art or may be any equipment known in the art.
Compared with the prior art, the invention has the following beneficial effects：
The invention provides a supergravity gas mixing device for cutting bubbles step by step, which mainly aims at the gas-liquid mass transfer process of insoluble gases such as hydrogen, oxygen, carbon monoxide and the like, in the device, liquid phase is used as continuous phase, gas phase is used as dispersed phase, the liquid phase and part of the gas phase enter the supergravity device through a gas-liquid inlet at the lower part of the shell, the other part of the gas is supplied with gas for a plurality of times through the gas supply port to improve the gas content rate, and enters the gas-liquid mixture of the supergravity device through the gas-liquid inlet, the rotor is driven by the motor to rotate at high speed, the gas crushing part loaded in the rotor shears the gas-liquid mixture, the sheared gas-liquid mixture and the gas entering from the gas supplementing port enter the next-stage rotor to be sheared, from bottom to top, the aperture of the gas crushing part loaded in the rotor is smaller and smaller, and finally, a gas-liquid mixture leaves the device from a gas-liquid outlet; finally, the rapid and large-scale controllable preparation of microbubbles of 10-300 mu m is realized, and the size distribution of the microbubbles is uniform; on the other hand, for the gas-liquid mixing process in the gas-liquid and gas-liquid-solid catalytic reaction processes, the reaction rate is improved, the volume of the reactor is reduced and the safety of the reaction process is improved by strengthening the gas-liquid mass transfer process.
Drawings
The following detailed description of embodiments of the invention is provided in connection with the accompanying drawings
FIG. 1 is a schematic structural diagram of a supergravity gas mixing device for cutting bubbles stage by stage according to the present invention;
FIG. 2 shows a schematic view of the distribution of the holes in the bottom of the rotor of FIG. 1 according to the invention;
fig. 3 shows a schematic hole diameter view of the gas-fracturing elements carried by the rotors of fig. 1 of the present invention.
FIG. 4 is a schematic view showing the structure of a reaction system in example 1 of the present invention;
FIG. 5 is a schematic view showing the structure of a reaction system in example 2 of the present invention;
FIG. 6 is a schematic view showing the structure of a reaction system in example 3 of the present invention.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below with reference to preferred embodiments and the accompanying drawings. Similar parts in the figures are denoted by the same reference numerals. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
Various cross-sectional views in accordance with the disclosed embodiment of the invention are shown in the drawings. The figures are not drawn to scale, wherein certain details are exaggerated and possibly omitted for clarity of presentation. The shapes of various regions, layers, and relative sizes and positional relationships therebetween shown in the drawings are merely exemplary, and deviations may occur in practice due to manufacturing tolerances or technical limitations, and a person skilled in the art may additionally design regions/layers having different shapes, sizes, relative positions, as actually required.
The problem of poor gas-liquid mass transfer is often existed in the gas-liquid mass transfer process involving insoluble gases such as hydrogen, oxygen, carbon monoxide and the like, so that the macroscopic reaction rate is limited by the gas-liquid mass transfer rate. With the development of gas-liquid mass transfer strengthening technology in recent years, large bubbles are broken to form micro bubbles, the gas-liquid interphase mass transfer area is increased to further strengthen the gas-liquid mass transfer process, and the gas-liquid mass transfer rate is matched with the intrinsic reaction rate, so that the macroscopic reaction rate is improved, the reaction time is shortened, and the intrinsic safety of the system is improved. However, at present, the effective control of the size of microbubbles is realized, and the mass preparation of microbubbles with small size and uniform size distribution still has certain difficulty.
Therefore, as one aspect of the invention, the invention provides a hypergravity gas mixing device for cutting bubbles step by step, which is characterized in that a traditional hypergravity reactor is improved, on one hand, a multi-stage rotor structure is adopted, parts with nanometer and micron holes are placed in a rotating environment to reduce coalescence, meanwhile, the aperture of a gas crushing part is gradually reduced from bottom to top, so that the step by step fine crushing of the bubbles is realized, and on the other hand, hydrophilic or hydrophobic surface modification is carried out on the surfaces of the bubble crushing parts, so that the dispersion process of the gas crushing parts on gas is further strengthened.
It is well known to those skilled in the art that the acceleration of the centrifugal force generated by the supergravity field should be greater than 10g (i.e. more than 10 times the acceleration of gravity), and will not be described herein.
As will be appreciated by those skilled in the art, "microbubbles" in the present application refer to bubbles on the micron scale, generally considered to be between 1 μm and 1000 μm.
Referring to fig. 1, the present invention provides a supergravity gas mixing device for cutting bubbles step by step, comprising:
a motor 1 for providing power to the rotation of the rotor in the apparatus of the present invention;
a rotating shaft 2; for power transmission and for fixing to the rotors 4 of the various stages in the housing 3
A housing 3 for accommodating the components and reaction solution of the apparatus of the present invention;
the gas-liquid inlet 6 is used for introducing gas and liquid materials to form a gas-liquid mixture;
the gas supplementing port 8 is used for supplementing gas in the device;
a gas-liquid outlet 9 for outputting a gas-liquid mixture;
the multistage rotor 4 is used for loading a gas crushing part to crush gas; and
a bubble breaking part 5 for breaking the gas;
the rotating shaft 2 serving as an output shaft of the motor extends into the shell 3 from the center of the top end of the shell 3 and is fixed with each stage of rotor 4 to drive the rotors 4 to rotate;
a plurality of flow guide pieces 10 are fixedly arranged on the inner wall of the shell 3 and are positioned between each stage of rotor and the shell; the flow guide piece 10 is used for gas-liquid mixture and gas newly supplemented from the gas supplementing port 8 to sequentially pass through the rotor according to design requirements;
the multistage rotor 4 is internally loaded with gas crushing parts 5, and the aperture of the gas crushing parts 5 loaded in the multistage rotor 4 is smaller and smaller from bottom to top; the rotating speed of the rotor can be 100-3000r/min, for example, the rotating speed of the rotor can be 400r/min, 500r/min, 600r/min, 700r/min, 800r/min, 900r/min, 1000r/min, 2000r/min, 3000 r/min; the size of the nano-micro bubbles is controlled by the rotation speed of the rotor, for example, the bubbles are smaller when the rotation speed of the rotor is higher.
A gas-liquid outlet 9 is arranged at the upper part outside the shell 3; air supply ports 8 are arranged on the shell 3 which is transversely corresponding to the gaps between the rotors 4 at all levels;
the bottom of the shell 3 is provided with a gas-liquid inlet 6;
the bottom of the rotor 4 is provided with a plurality of ducts for facilitating the passage of gas and liquid, as shown in fig. 3.
According to some embodiments of the invention, the multi-stage rotor in the housing 3 has 3-30 layers with a distance of 10-50mm between each layer; more preferably, the multi-stage rotor in the housing 3 has 3-5 layers. The rotor structure shown in fig. 1, for example, is provided with 4 layers.
According to some embodiments of the invention, the number of the air supply ports 8 is 2 to 29. For example, 3 air supply ports are shown in fig. 1.
According to some embodiments of the invention, the gap between the flow guide 10 and the rotor 4 is 2-10 mm.
According to some embodiments of the invention, the gas-fracturing element surface is a hydrophilic surface layer or a hydrophobic surface layer. The size of the microbubbles can be controlled by hydrophilic/hydrophobic surface modification of the gas disruption parts, e.g., for oil phase systems the more hydrophilic the smaller the bubbles, and for water phase systems the more hydrophobic the smaller the bubbles.
According to some embodiments of the invention, the bubble-breaking parts 5 are a nano-microporous porous filler, a nano-microporous sintered film.
According to some embodiments of the present invention, the aperture of the gas crushing elements 5 loaded in the multistage rotor 4 is decreased in equal proportion from bottom to top. The gas breaker elements carried in the rotor will now be described in more detail with reference to fig. 2. Fig. 2 shows a side view of the gas-liquid crushing members loaded in the rotors of the respective stages, and it can be seen from fig. 2 that the pore diameters of the gas-liquid crushing members become smaller as the gas-liquid mixture flows.
In a preferred embodiment, the gas breaking elements should match the pore size of the channels in the bottom of the rotor, taking into account the gas-liquid ratio of the gas breaking elements loaded in the rotor, the inlet device and the actual application process, and the pore size of the channels in the bottom of the rotor should decrease as the pore size of the gas breaking elements decreases. Therefore, the diameter of the pore canal increases or decreases along the direction of gas flow; or the pore diameter of the pore canal increases or decreases along the flowing direction of the liquid in the outer cavity. Therefore, the size of the hole diameter of the gas crushing part and the size of the hole channel at the bottom of the rotor can be adjusted according to the whole flow system, and the hole diameter of the gas crushing part and the size of the hole channel at the bottom of the rotor are matched with the specific system.
According to some embodiments of the invention, the plurality of ducts provided at the bottom of each stage of rotor 4 are distributed symmetrically and uniformly around the axis of rotation, as shown for example in fig. 3.
According to some embodiments of the invention, a gas flow control valve is provided at the gas-liquid inlet. Can then control the proportion of gas-liquid mixture through the velocity of flow of control gas like this, of course, this application does not restrict gas flow control valve and sets up on the casing, for example gas flow control valve can set up on the air supply (generally, all has gas flow control valve on every gas steel bottle), but to the longer system of pipeline, the error of controlling gas flow from the air supply department is great, and it is little to control the error at gas import department directly, can eliminate the influence that pipeline self pressure differential brought.
According to some embodiments of the invention, the gas supply ports are each provided with a one-way valve.
The average particle size of the microbubbles formed in the supergravity gas mixing device for cutting the bubbles step by step is between 10 and 300 microns, and the microbubbles can be detected by a visualization technology, an X-ray imaging technology and a method of an optical fiber probe or a conductance probe.
Based on the inventive concept of the supergravity gas mixing device for cutting bubbles step by step in the first aspect of the present invention, as a second aspect of the present invention, there is provided an application of the above supergravity gas mixing device for cutting bubbles step by step, the application including a gas-liquid mixing process in a gas-liquid mixing process or in a gas-liquid-solid catalytic reaction process.
Preferably, the gas-liquid mixing process refers to a mixing process in which a sparingly soluble gas participates; more preferably, the insoluble gas is one of hydrogen, oxygen, ozone, carbon monoxide, carbon dioxide, nitric oxide, and lower hydrocarbons.
Example 1
The supergravity gas mixing device for cutting bubbles step by step is used as gas-liquid mixing equipment to be applied to the fixed bed catalytic reaction process, and comprises the following steps:
referring to fig. 4, the device shown in fig. 1 is applied to a catalytic reaction process, the reaction system device comprises a hypergravity gas mixing device-41 for cutting bubbles step by step, a nitrogen gas steel cylinder-11, a hydrogen gas steel cylinder-12, a gas mass flow meter-13, a fixed bed reactor-14, a condensing tank-15, a back pressure valve-16, a gas-liquid separation tank-17, a ball valve-18, a raw material tank-19 and a plunger pump-20, wherein the hypergravity gas mixing device for cutting bubbles step by step, the fixed bed reactor and the raw material tank are all provided with electric heating sleeves, and the reaction process comprises the following steps:
1) a gas-liquid inlet of the hypergravity gas mixing device for cutting the bubbles step by step is respectively connected with a gas steel cylinder and a raw material tank, a gas-liquid outlet of the hypergravity gas mixing device for cutting the bubbles step by step is connected with a fixed bed reactor, an outlet of the fixed bed is connected with a condensing tank and a gas-liquid separating tank, and the gas-liquid separating tank is connected with the raw material tank; (as shown in FIG. 4);
2) purging the whole reaction system by using nitrogen, and opening a heating device to a preset temperature;
3) starting a plunger pump, enabling a reaction solution to enter a hypergravity gas mixing device for cutting bubbles step by step and forming liquid phase circulation, starting a gas steel cylinder to introduce hydrogen after a system is stabilized, adjusting the gas flow by using a gas mass flowmeter, adjusting the gas flow to a preset pressure by using a back pressure valve to perform gas-liquid-solid three-phase catalytic reaction, wherein the pressure of a reaction system is controlled by the back pressure valve, and the temperature is controlled by a temperature control system;
4) separating the gas-liquid mixture with the reaction product generated in the step 3) through a condensing tank and a gas-liquid separation tank, discharging the gas through an emptying valve, and allowing the liquid to flow into a raw material tank; in addition, the system can be controlled to be in one-way catalytic reaction or circulating catalytic reaction by controlling the switch of the ball valve, when the ball valve is opened, the system is in circulating catalytic reaction, and when the ball valve is closed, the system is in one-way catalytic reaction; and separating the reacted sample and then carrying out further detection.
Taking the hydrogenation of alpha-methylstyrene (AMS) as an example: Pd/Al with the equivalent diameter of 3mm is filled in a fixed bed layer2O3The number of rotor stages of the catalyst and the hypergravity gas mixing device for cutting bubbles step by step is 3, and porous fillers with hydrophilic nanometer micron pores are filled in the rotor; using isopropyl benzene as solvent, preparing AMS working solution with volume fraction of 20%, under the condition of 50 deg.C, 0.3MPa pressure and rotating speed of supergravity gas mixing device 800r/min, its air-space reaction rate (STY) can be up to 5.2mmol AMS. gPd-1·s-1(ii) a Under the same temperature and pressure conditions, the rotating speed of the hypergravity gas mixing device only changing step by step bubble cutting is 1500r/min, and the time-space reaction rate (STY) reaches 7.8 mmoleAMS-gPd-1·s-1Under the same experimental conditions, a supergravity gas mixing device for cutting bubbles step by step is not added, and the time-space reaction rate (STY) is 1.1mmolAMS & gPd-1·s-1。
Example 2
The hypergravity gas mixing device for cutting bubbles step by step is used as gas-liquid mixing equipment to be applied to the catalytic reaction process of a stirring kettle, and comprises the following steps:
referring to fig. 5, the device shown in fig. 1 is applied to a catalytic reaction process, the reaction system device comprises a hypergravity gas mixing device-41 for cutting bubbles step by step, a nitrogen gas steel cylinder-21, a hydrogen gas steel cylinder-22, a gas mass flow meter-23, a stirred tank reactor-24, a condensing tank-25, a back pressure valve-26, a gas-liquid separation tank-27, a ball valve-28, a raw material tank-29 and a plunger pump-30, wherein the hypergravity gas mixing device for cutting bubbles step by step and the raw material tank are both provided with electric heating sleeves, the stirred tank reactor is provided with a cooling system, and the reaction process comprises the following steps:
1) a gas-liquid inlet of the hypergravity gas mixing device for cutting the bubbles step by step is respectively connected with a gas steel cylinder and a raw material tank, a gas-liquid outlet of the hypergravity gas mixing device for cutting the bubbles step by step is connected with a stirred tank reactor, the stirred tank reactor is connected with a condensing tank and a gas-liquid separation tank, and the gas-liquid separation tank is connected with the raw material tank; (as shown in FIG. 5);
2) purging the whole reaction system by using nitrogen, and opening a heating device to a preset temperature;
3) starting a plunger pump, enabling a reaction solution to enter a hypergravity gas mixing device for cutting bubbles step by step and forming liquid phase circulation, starting a gas steel cylinder to introduce hydrogen after a system is stabilized, adjusting the gas flow by using a gas mass flowmeter, adjusting the gas flow to a preset pressure by using a back pressure valve to perform gas-liquid-solid three-phase catalytic reaction, wherein the pressure of a reaction system is controlled by the back pressure valve, and the temperature is controlled by a temperature control system;
4) separating the gas-liquid mixture with the reaction product generated in the step 3) through a condensing tank and a gas-liquid separation tank, discharging the gas through an emptying valve, and allowing the liquid to flow into a raw material tank; in addition, the system can be controlled to be in one-way catalytic reaction or circulating catalytic reaction by controlling the switch of the ball valve, when the ball valve is opened, the system is in circulating catalytic reaction, and when the ball valve is closed, the system is in one-way catalytic reaction; and separating the reacted sample and then carrying out further detection.
Taking catalytic hydrogenation of p-nitroanisole to prepare p-anisidine as an example: adding Raney nickel catalyst into a stirred tank reactor, wherein the number of rotor stages of the supergravity gas mixing device for cutting bubbles step by step is 3, and porous filler with hydrophilic nano-micron pores is filled in a rotor. Methanol is used as a solvent to prepare a p-nitroanisole working solution with the mass fraction of 35%. Reacting for 1h under the conditions that the temperature is 75 ℃, the pressure is 1.2MPa and the rotating speed of a hypergravity gas mixing device for cutting bubbles step by step is 800r/min, and the conversion rate of the paranitroanisole reaches over 90 percent; under the conditions of the same temperature, pressure and reaction time, the rotating speed of the hypergravity gas mixing device for cutting bubbles step by step is only changed to be 1500r/min, the conversion rate of the paranitroanisole reaches more than 95%, and under the same experimental conditions, the hypergravity gas mixing device for cutting bubbles step by step is not added, and the conversion rate of the paranitroanisole is about 60%.
Example 3
The supergravity gas mixing device for cutting bubbles step by step is used as gas-liquid mixing equipment to be applied to the catalytic reaction process of a slurry bed, and comprises the following steps:
referring to fig. 6, the device shown in fig. 1 is applied to a catalytic reaction process, the reaction system device comprises a hypergravity gas mixing device-41 for cutting bubbles step by step, a nitrogen gas steel cylinder-31, a hydrogen gas steel cylinder-32, a gas mass flow meter-33, a stirred tank reactor-34, a condensing tank-35, a back pressure valve-36, a gas-liquid separation tank-37, a ball valve-38, a raw material tank-39 and a plunger pump-40, wherein the hypergravity gas mixing device for cutting bubbles step by step and the raw material tank are both provided with electric heating sleeves, the slurry bed reactor is provided with a cooling system, and the reaction process comprises the following steps:
1) a gas-liquid inlet of the hypergravity gas mixing device for cutting the bubbles step by step is respectively connected with a gas steel cylinder and a raw material tank, a gas-liquid outlet of the hypergravity gas mixing device for cutting the bubbles step by step is connected with a stirred tank reactor, the stirred tank reactor is connected with a condensing tank and a gas-liquid separation tank, and the gas-liquid separation tank is connected with the raw material tank; (as shown in FIG. 6);
2) purging the whole reaction system by using nitrogen, and opening a heating device to a preset temperature;
3) starting a plunger pump, enabling a reaction solution to enter a hypergravity gas mixing device for cutting bubbles step by step and forming liquid phase circulation, starting a gas steel cylinder to introduce hydrogen after a system is stabilized, adjusting the gas flow by using a gas mass flowmeter, adjusting the gas flow to a preset pressure by using a back pressure valve to perform gas-liquid-solid three-phase catalytic reaction, wherein the pressure of a reaction system is controlled by the back pressure valve, and the temperature is controlled by a temperature control system;
4) separating the gas-liquid mixture with the reaction product generated in the step 3) through a condensing tank and a gas-liquid separation tank, discharging the gas through an emptying valve, and allowing the liquid to flow into a raw material tank; in addition, the system can be controlled to be in one-way catalytic reaction or circulating catalytic reaction by controlling the switch of the ball valve, when the ball valve is opened, the system is in circulating catalytic reaction, and when the ball valve is closed, the system is in one-way catalytic reaction; and separating the reacted sample and then carrying out further detection.
Taking the preparation of 2-amino-4-acetamino anisole by catalytic hydrogenation of 2-nitro-4-acetamino anisole as an example: adding Raney nickel catalyst into a slurry bed reactor, and cutting bubbles step by step, wherein the rotor stage number of the hypergravity gas mixing device is 3, and porous filler with hydrophilic nano-micron pores is filled in the rotor. Methanol is used as a solvent to prepare a working solution of 2-nitro-4-acetamino anisole with the solid content of 30 percent. The reaction is carried out for 1h under the conditions that the temperature is 100 ℃, the pressure is 1.5MPa and the rotating speed of a hypergravity gas mixing device for cutting bubbles step by step is 800r/min, and the conversion rate of the 2-nitro-4-acetamino anisole reaches more than 85 percent; under the conditions of the same temperature, pressure and reaction time, the rotating speed of the hypergravity gas mixing device for cutting bubbles step by step is only changed to be 1500r/min, the conversion rate of the paranitroanisole reaches more than 92 percent, under the same experimental conditions, the hypergravity gas mixing device for cutting bubbles step by step is not added, and the conversion rate of the paranitroanisole is about 55 percent.
Therefore, the supergravity gas mixing device capable of cutting bubbles step by step can be used as gas-liquid mixing equipment to be applied to catalytic reaction processes participated by reactors such as a fixed bed, a stirring kettle, a slurry bed and the like, the gas-liquid contact area in the hydrogenation/oxidation reaction process is increased due to the large amount of micro bubbles, and the gas content of a solution to be reacted is increased, so that the gas-liquid mass transfer is enhanced, the purposes of improving the macroscopic reaction rate and shortening the reaction time are achieved, and the supergravity gas mixing device has important industrial application significance in the fields of petrochemical industry, fine chemical industry, coal chemical industry, biochemical industry and the like.
Of course, the above scenarios are merely exemplary, and the present invention can be applied to various gas-liquid mixing processes, or gas-liquid mixing reactions in hydrogenation/oxidation reactions, and is not exhaustive, but it should be understood that the substitution of the reaction system based on the concept of the present invention, which is not necessarily one of hydrogenation or oxidation, still falls within the scope defined by the present application.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. Not all embodiments are exhaustive. All obvious changes and modifications which are obvious to the technical scheme of the invention are covered by the protection scope of the invention.
Claims (10)
1. A hypergravity gas mixing device for cutting bubbles step by step is characterized by comprising a motor, a rotating shaft, a shell, a gas-liquid inlet, a gas supplementing port, a gas-liquid outlet, a multi-stage rotor and a bubble crushing part;
the rotating shaft serving as an output shaft of the motor extends into the shell from the center of the top end of the shell and is connected with the rotor to drive the rotor to rotate;
a plurality of flow guide pieces are fixedly arranged on the inner wall of the shell and positioned between each stage of rotor and the shell;
the multistage rotor is internally loaded with gas crushing parts, and the aperture of the gas crushing parts loaded in the multistage rotor is smaller and smaller from bottom to top;
a gas-liquid outlet is formed in the upper outer part of the shell; air supply ports are arranged on the shell which transversely corresponds to the gaps between the rotors at all levels;
the bottom of the shell is provided with a gas-liquid inlet;
and a plurality of pore channels for facilitating gas-liquid to pass through are arranged at the bottom of the rotor.
2. The supergravity gas mixing device for stage-by-stage cutting of gas bubbles according to claim 1, wherein: the multistage rotors in the shell are 3-30 layers, and the distance between every two layers is 10-50 mm; more preferably, the multi-stage rotor in the shell has 3-5 layers.
3. The supergravity gas mixing device for stage-by-stage cutting of gas bubbles according to claim 2, wherein: the number of the air supplementing ports is 2-29.
4. The supergravity gas mixing device for stage-by-stage cutting of gas bubbles according to claim 1, wherein: the gap between the flow guide piece and the rotor is 2-10 mm.
5. The supergravity gas mixing device for stage-by-stage cutting of gas bubbles according to claim 1, wherein: the surface of the gas crushing part is a hydrophilic surface layer or a hydrophobic surface layer.
6. The hypergravity gas mixing device for cutting gas bubbles stage by stage according to claim 1, characterized in that: the bubble breaking parts are porous fillers with nano-micron pores and sintering films with nano-micron pores.
7. The supergravity gas mixing device for stage-by-stage cutting of gas bubbles according to claim 1, wherein: the aperture of the gas crushing part loaded in the multistage rotor is decreased gradually according to equal proportion from bottom to top.
8. The supergravity gas mixing device for stage-by-stage cutting of gas bubbles according to claim 1, wherein: the plurality of pore canals arranged at the bottom of each stage of rotor are symmetrically and uniformly distributed around the axis of the rotating shaft.
9. The hypergravity gas mixing device for cutting gas bubbles stage by stage according to claim 1, characterized in that: a gas flow control valve is arranged at the gas-liquid inlet; preferably, the air supplementing openings are all provided with one-way valves.
10. Use of a supergravity gas mixing device for progressively cutting gas bubbles according to any one of claims 1 to 9, wherein: the application includes a gas-liquid mixing process in a gas-liquid mixing process or in a gas-liquid-solid catalytic reaction process;
preferably, the gas-liquid mixing process refers to a gas-liquid mixing process in which a sparingly soluble gas participates; more preferably, the sparingly soluble gas is one of hydrogen, oxygen, ozone, carbon monoxide, carbon dioxide, nitric oxide, and lower hydrocarbons.
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