CN114699939B - Supergravity gas mixing device for gradually cutting bubbles and application thereof - Google Patents
Supergravity gas mixing device for gradually cutting bubbles and application thereof Download PDFInfo
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Abstract
The application 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 guide piece, a gas-liquid outlet, a rotor and a bubble crushing part; the rotating shaft is used as an output shaft of the motor, extends from the center of the top end of the shell to the inside of the shell, and is connected with the rotor to drive the rotor to rotate; the shell is provided with a gas-liquid outlet and a plurality of gas-supplementing ports from top to bottom; the rotor is internally provided with gas crushing parts, and the multistage rotor structure is provided with the gas crushing parts with smaller and smaller apertures from bottom to top. The device can be used for effectively regulating and controlling the size of bubbles by adjusting the rotating speed of the supergravity device, assisting in multistage air supplementing, and realizing gradual cutting of the bubbles through the synergistic effect of multistage rotors of hydrophilic/hydrophobic bubble crushing parts with different apertures, so that the obtained bubbles are smaller in size and uniform in size distribution.
Description
Technical Field
The application belongs to the field of supergravity reactors 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 used in the chemical industry. The gas-liquid mixing process greatly influences the gas-liquid-gas-liquid mass transfer process, and the research of the gas-liquid mass transfer strengthening technology has important significance in shortening the process flow, reducing the equipment size, reducing the investment and operation cost and the like. The supergravity technology using the rotating bed as the core equipment is one of the effective technologies for strengthening the gas-liquid mass transfer process.
Aiming at the gas-liquid mass transfer process involving indissolvable gases such as hydrogen, oxygen, carbon monoxide and the like, the problem of poor gas-liquid mass transfer often exists, 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 crushed to form micro bubbles, so that the mass transfer area between gas and liquid phases is increased, the gas-liquid mass transfer process is strengthened, the gas-liquid mass transfer rate is matched with the intrinsic reaction rate, 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 supergravity nano-micro bubble generation device and a reaction system, which are difficult to realize large-scale preparation of micro bubbles with small size and uniform size distribution while realizing effective regulation and control of the micro bubble size at present. Therefore, the device for preparing the microbubbles with small size and uniform size distribution is developed, which has simple equipment structure, large gas flux, high speed and controllable preparation, and has important practical application value for improving the problems of high energy consumption, high material consumption and high pollution of three highs in the chemical industry and realizing national energy conservation and emission reduction.
Disclosure of Invention
The first technical problem to be solved by the application is to provide a supergravity air mixing device for cutting bubbles step by step; the device mainly aims at the gas-liquid mass transfer process of indissolvable gases such as hydrogen, oxygen, carbon monoxide and the like, wherein a liquid phase is used as a continuous phase, a gas phase is used as a disperse phase, the liquid phase and part of the gas phase enter the hypergravity device through a gas-liquid inlet at the lower part of a shell, the other part of the gas is subjected to repeated gas supplementing through a gas supplementing port, the gas content is improved, a gas-liquid mixture entering the hypergravity device through the gas-liquid inlet is driven by a motor to rotate at a high speed, a gas crushing part loaded in the rotor shears the gas-liquid mixture, the sheared gas-liquid mixture enters the rotor at the next stage together with the gas entering through the gas supplementing port, the aperture of the gas crushing part loaded in the rotor is smaller and smaller from bottom to top, and finally the gas-liquid mixture leaves the device from a gas-liquid outlet. Finally, the rapid and large-scale controllable preparation of 10-300 mu m micro-bubbles is realized, and the size distribution of the micro-bubbles is uniform.
The second technical problem to be solved by the application is to provide an application of a supergravity air mixing device for cutting bubbles step by step.
In order to solve the first technical problem, the application adopts the following technical scheme:
a supergravity air mixing device for cutting bubbles step by step comprises a motor, a rotating shaft, a shell, an air-liquid inlet, an air-supplementing port, an air-liquid outlet, a multistage rotor and bubble crushing parts;
the rotating shaft is used as an output shaft of the motor, extends from the center of the top end of the shell to the inside of the shell, and is connected with the rotor to drive the rotor to rotate;
a plurality of guide pieces are fixedly arranged on the inner wall of the shell and positioned between each stage of rotor and the shell;
the gas crushing parts are loaded in the multistage rotor, and the aperture of the gas crushing parts loaded in the multistage rotor is smaller and smaller from bottom to top;
the upper part outside the shell is provided with a gas-liquid outlet; the shell transversely corresponding to the gaps among the rotors at all levels is provided with an air supplementing port;
the bottom of the shell is provided with a gas-liquid inlet;
the bottom of the rotor is provided with a plurality of pore canals which are convenient for gas and liquid to pass through.
Preferably, the multistage rotor in the shell is 3-30 layers, and the interval between each layer is 10-50mm; more preferably, the multistage rotor in the housing has 3-5 layers.
Preferably, the number of the air supplementing openings is 2-29.
Preferably, the gap between the flow guiding piece and the rotor is 2-10mm.
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 porous filler with nano-micro holes and a sintered film with nano-micro holes.
Preferably, the aperture of the gas crushing part loaded in the multistage rotor is reduced from bottom to top in equal proportion.
Preferably, a plurality of pore canals arranged at the bottom of each stage of rotor are symmetrically and uniformly distributed around the axis of the rotary shaft.
Preferably, a gas flow control valve is arranged at the gas-liquid inlet.
Preferably, the air supplementing ports are provided with one-way valves.
In order to solve the second technical problem, the application adopts the following technical scheme:
the application of the supergravity gas mixing device for cutting bubbles step by step comprises the gas-liquid mixing process in the gas-liquid mixing process or the 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 poorly soluble gas is one of hydrogen, oxygen, ozone, carbon monoxide, carbon dioxide, nitric oxide, and lower hydrocarbons.
Any range recited in the application includes any numerical value between the endpoints and any sub-range of any numerical value between the endpoints or any numerical value between the endpoints.
Unless otherwise indicated, all starting materials herein are commercially available, and the equipment used in the present application may be conventional in the art or may be conventional in the art.
Compared with the prior art, the application has the following beneficial effects：
The application provides a supergravity gas mixing device for cutting bubbles step by step, which mainly aims at the gas-liquid mass transfer process involving indissolvable gases such as hydrogen, oxygen, carbon monoxide and the like, wherein a liquid phase is used as a continuous phase, a gas phase is used as a disperse phase, the liquid phase and part of the gas phase enter the supergravity device through a gas-liquid inlet at the lower part of a shell, the other part of the gas is supplemented with gas for a plurality of times through a gas supplementing port, so that the gas content of the gas is improved, a gas-liquid mixture entering the supergravity device through the gas-liquid inlet drives a rotor to rotate at a high speed, a gas crushing part loaded in the rotor shears the gas-liquid mixture, the sheared gas-liquid mixture enters the next rotor together with the gas entering through the gas supplementing port, the aperture of the gas crushing part loaded in the rotor is smaller and smaller from bottom to top, and the final gas-liquid mixture leaves the device from a gas-liquid outlet; finally, the rapid and large-scale controllable preparation of 10-300 mu m micro-bubbles is realized, and the size distribution of the micro-bubbles is uniform; on the other hand, for the gas-liquid mixing process in the gas-liquid and gas-liquid-solid catalytic reaction process, 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 describes the embodiments of the present application in further detail with reference to the drawings
FIG. 1 shows a schematic structure of a supergravity air mixing device for cutting bubbles step by step;
FIG. 2 shows a schematic diagram of the distribution of the channels at the bottom of the rotor of FIG. 1 in accordance with the present application;
figure 3 shows a schematic bore of a gas breaker element loaded by the rotor of each stage in figure 1 according to the application.
FIG. 4 is a schematic view showing the structure of a reaction system in example 1 of the present application;
FIG. 5 is a schematic view showing the structure of a reaction system in example 2 of the present application;
FIG. 6 is a schematic diagram showing the structure of a reaction system in example 3 of the present application.
Detailed Description
In order to more clearly illustrate the present application, the present application will be further described with reference to preferred embodiments and the accompanying drawings. Like parts in the drawings 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 that this application is not limited to the details given herein.
Various cross-sectional views according to disclosed embodiments of the application are shown in the accompanying drawings. The figures are not drawn to scale, wherein certain details are exaggerated for clarity of presentation and may have been omitted. The shapes of the various regions, layers and relative sizes, positional relationships between them shown in the drawings are merely exemplary, may in practice deviate due to manufacturing tolerances or technical limitations, and the skilled person may additionally design regions/layers having different shapes, sizes, relative positions as actually required.
Aiming at the gas-liquid mass transfer process involving indissolvable gases such as hydrogen, oxygen, carbon monoxide and the like, the problem of poor gas-liquid mass transfer often exists, 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 crushed to form micro bubbles, so that the mass transfer area between gas and liquid phases is increased, the gas-liquid mass transfer process is strengthened, the gas-liquid mass transfer rate is matched with the intrinsic reaction rate, the macroscopic reaction rate is improved, the reaction time is shortened, and the intrinsic safety of the system is improved. However, at present, the method still has certain difficulty in realizing the effective regulation and control of the size of the microbubbles and simultaneously realizing the mass preparation of the microbubbles with small size and uniform size distribution.
Therefore, as one aspect of the application, the application provides a supergravity gas mixing device for cutting bubbles step by step, which is characterized in that a traditional supergravity reactor is modified, on one hand, a multistage rotor structure is adopted, parts with nano-micro holes are placed in a rotating environment to reduce coalescence, meanwhile, the pore diameter 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, on the other hand, the surface of the bubble crushing part is subjected to hydrophilic or hydrophobic surface modification, and the dispersing process of the gas crushing part on the gas is further enhanced.
It is well known to those skilled in the art that the centrifugal force acceleration generated in the hypergravity field should be greater than 10g (i.e. more than 10 times the gravity acceleration), 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 micrometer scale, generally considered to be between 1 μm and 1000 μm.
Referring to fig. 1, the present application provides a supergravity air mixing device for cutting bubbles step by step, comprising:
a motor 1 for powering the rotation of the rotor in the device of the application;
a rotation shaft 2; for power transmission and for fixing the rotor 4 of each stage in the housing 3
A housing 3 for accommodating the components and the reaction liquid of the apparatus of the present application;
a gas-liquid inlet 6 for the ingress of gas and liquid material to form a gas-liquid mixture;
a gas supplementing port 8 for supplementing gas to the device;
a gas-liquid outlet 9 for outputting a gas-liquid mixture;
a multistage rotor 4 for loading gas crushing parts to crush gas; and
a bubble breaking part 5 for breaking the gas;
the rotating shaft 2 is used as an output shaft of the motor, extends from the center of the top end of the shell 3 to the inside of the shell 3, is fixed with each stage of rotor 4, and drives the rotor 4 to rotate;
a plurality of guide pieces 10 are fixedly arranged on the inner wall of the shell 3 and positioned between each stage of rotor and the shell; the flow guiding piece 10 is used for enabling the gas-liquid mixture and the gas newly supplemented from the air supplementing port 8 to sequentially pass through the rotor according to the design requirement;
the multistage rotor 4 is internally provided with a gas crushing part 5, and the aperture of the gas crushing part 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 and 3000r/min; the size of the nano-micro bubbles is controlled by the rotational speed of the rotor, for example, the higher the rotational speed of the rotor, the smaller the bubbles.
The upper part of the outer part of the shell 3 is provided with a gas-liquid outlet 9; the shell 3 transversely corresponding to the gaps among the rotors 4 at each stage is provided with an air supplementing port 8;
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 pore canals which facilitate the gas-liquid to pass through, as shown in fig. 3.
According to certain embodiments of the application, the multistage rotor in the shell 3 is formed by 3-30 layers, and the interval between each layer is 10-50mm; more preferably, the multistage rotor in the housing 3 has 3-5 layers. The rotor structure shown for example in fig. 1 is provided with 4 layers.
According to some embodiments of the application, the number of the air supplementing ports 8 is 2-29. For example, 3 make-up ports are shown in fig. 1.
According to some embodiments of the application, the gap between the baffle 10 and the rotor 4 is 2-10mm.
According to certain embodiments of the application, the gas disruption element surface is a hydrophilic skin or a hydrophobic skin. The size of the microbubbles can be controlled by the hydrophilic/hydrophobic surface modification of the gas disruption elements, e.g., the better the hydrophilicity, the smaller the bubbles, the better the hydrophobicity, the smaller the bubbles, for an oil phase system.
According to some embodiments of the application, the bubble breaking member 5 is a porous filler of nano-micro holes, a sintered film of nano-micro holes.
According to some embodiments of the application, the aperture of the gas-crushing elements 5 loaded in the multistage rotor 4 is reduced from bottom to top in equal proportion. The gas-crushing elements loaded in the rotor are described in detail below in connection with fig. 2. Fig. 2 shows a side view of the gas-crushing part loaded in each stage of the rotor, and it can be seen from fig. 2 that the pore diameter of the gas-liquid crushing part becomes smaller and smaller as the gas-liquid mixture flows.
In a preferred embodiment, the gas crushing part should be matched with the pore diameter of the pore canal at the bottom of the rotor in view of the gas crushing part loaded in the rotor, the gas-liquid ratio of the inlet device and the actual application process, and the pore diameter of the pore canal at the bottom of the rotor should be smaller and smaller as the pore diameter of the gas crushing part is reduced. Thus, the diameter of the pore canal increases or decreases along the direction of the gas flow; or the pore diameter of the pore canal increases or decreases gradually along the flowing direction of the outer cavity liquid. Thus, the pore diameter of the gas crushing part and the size of the bottom pore canal of the rotor are more matched with the specific system.
According to some embodiments of the present application, the plurality of holes provided at the bottom of each stage of rotor 4 are symmetrically and uniformly distributed around the axis of the rotary shaft, for example, as shown in fig. 3.
According to some embodiments of the application, the gas-liquid inlet is provided with a gas flow control valve. Thus, the flow rate of the gas can be controlled to further control the mixing ratio of the gas and the liquid, and the application does not limit whether the gas flow control valve is arranged on the shell, for example, the gas flow control valve can be arranged on a gas source (generally, each gas steel cylinder is provided with the gas flow control valve), but for a system with a longer pipeline, the error of controlling the gas flow from the gas source is larger, the direct control error at the gas inlet is small, and the influence caused by the pressure difference of the pipeline can be eliminated.
According to some embodiments of the application, the air supply ports are provided with one-way valves.
The average particle size of microbubbles formed in the supergravity gas mixing device for cutting bubbles step by step is between 10 and 300 microns, and the detection can be specifically performed by a visualization and X-ray imaging technology and a method of an optical fiber probe or a conductivity probe, and the application is not limited to the method.
Based on the inventive concept of the supergravity gas mixing device for stepwise cutting bubbles according to the first aspect of the present application, as a second aspect of the present application, there is provided the use of the above-mentioned supergravity gas mixing device for stepwise cutting bubbles, the use comprising 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 involving a poorly soluble gas; more preferably, the poorly soluble 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 a 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, a reaction system device comprises a supergravity gas mixing device-41 for cutting bubbles step by step, a nitrogen gas steel bottle-11, a hydrogen gas steel bottle-12, a gas mass flowmeter-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 supergravity gas mixing device for cutting bubbles step by step, the fixed bed reactor and the raw material tank are all provided with electric heating jackets, and the reaction process comprises the following steps:
1) The gas-liquid inlet of the supergravity gas mixing device for cutting bubbles step by step is respectively connected with a gas steel bottle and a raw material tank, the gas-liquid outlet of the supergravity gas mixing device for cutting bubbles step by step is connected with a fixed bed reactor, the fixed bed outlet 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. 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 supergravity gas mixing device for cutting bubbles step by step and form liquid-phase circulation, starting a gas steel cylinder to introduce hydrogen after the system is stable, regulating the gas flow by using a gas mass flowmeter, regulating to a preset pressure by using a back pressure valve to perform gas-liquid-solid three-phase catalytic reaction, controlling the pressure of a reaction system by the back pressure valve, and controlling the temperature 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 a vent valve, and flowing the liquid into a raw material tank; in addition, the system can be controlled to be single-pass catalytic reaction or circulating catalytic reaction by controlling the switch of the ball valve, when the ball valve is opened, the system is circulating catalytic reaction, and when the ball valve is closed, the system is single-pass catalytic reaction; the reacted sample was separated and further tested.
Taking the hydrogenation of alpha-methylstyrene (AMS) as an example: pd/Al with equivalent diameter of 3mm is filled in the fixed bed layer 2 O 3 The catalyst, cut the rotor stage number of the supergravity air mixing device of the bubble step by step to be 3, pack the porous filler of the hydrophilic nanometer micron pore in the rotor; the volume fraction is prepared by taking isopropylbenzene as a solventThe time-space reaction rate (STY) of 20% AMS working solution reaches 5.2mmolAMS gPd under the condition that the temperature is 50 ℃, the pressure is 0.3MPa and the rotating speed of a supergravity air mixing device for cutting bubbles step by step is 800r/min -1 ·s -1 The method comprises the steps of carrying out a first treatment on the surface of the Under the same temperature and pressure, the rotating speed of the supergravity air mixing device for cutting bubbles step by step is only changed to 1500r/min, and the time-space reaction rate (STY) reaches 7.8mmolAMS gPd -1 ·s -1 Under the same experimental conditions, a supergravity air 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 supergravity gas mixing device for cutting bubbles step by step is used as gas-liquid mixing equipment to be applied to a catalytic reaction process of a stirred tank, and comprises the following steps:
referring to FIG. 5, the device shown in FIG. 1 is applied to a catalytic reaction process, a reaction system device comprises a supergravity gas mixing device-41 for cutting bubbles step by step, a nitrogen steel bottle-21, a hydrogen steel bottle-22, a gas mass flowmeter-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 supergravity gas mixing device for cutting bubbles step by step and the raw material tank are both provided with an electric heating sleeve, and the stirred tank reactor is provided with a cooling system, and the reaction process comprises the following steps:
1) The gas-liquid inlet of the supergravity gas mixing device for cutting bubbles step by step is respectively connected with a gas steel bottle and a raw material tank, the gas-liquid outlet of the supergravity gas mixing device for cutting 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 supergravity gas mixing device for cutting bubbles step by step and form liquid-phase circulation, starting a gas steel cylinder to introduce hydrogen after the system is stable, regulating the gas flow by using a gas mass flowmeter, regulating to a preset pressure by using a back pressure valve to perform gas-liquid-solid three-phase catalytic reaction, controlling the pressure of a reaction system by the back pressure valve, and controlling the temperature 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 a vent valve, and flowing the liquid into a raw material tank; in addition, the system can be controlled to be single-pass catalytic reaction or circulating catalytic reaction by controlling the switch of the ball valve, when the ball valve is opened, the system is circulating catalytic reaction, and when the ball valve is closed, the system is single-pass catalytic reaction; the reacted sample was separated and further tested.
Taking catalytic hydrogenation of paranitroanisole to prepare paraaminoanisole as an example: and adding a Raney nickel catalyst into the stirred tank reactor, wherein the rotor stage number of the supergravity gas mixing device for cutting bubbles step by step is 3, and porous filler with hydrophilic nano-micro holes is filled in the rotor. Methanol is used as a solvent to prepare the working solution of the p-nitroanisole with the mass fraction of 35 percent. Under the conditions that the temperature is 75 ℃ and the pressure is 1.2MPa, and the rotating speed of a supergravity air mixing device for cutting bubbles step by step is 800r/min, the reaction is carried out for 1h, and the conversion rate of the paranitroanisole reaches more than 90%; under the same temperature, pressure and reaction time, the rotating speed of the supergravity air mixing device for cutting bubbles step by step is only changed to 1500r/min, the conversion rate of the paranitroanisole reaches more than 95%, and under the same experimental conditions, the supergravity air 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 a slurry bed catalytic reaction process, and comprises the following steps:
referring to fig. 6, the device shown in fig. 1 is used in a catalytic reaction process, a reaction system device comprises a supergravity gas mixing device-41 for cutting bubbles step by step, a nitrogen gas steel bottle-31, a hydrogen gas steel bottle-32, a gas mass flowmeter-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 supergravity gas mixing device for cutting bubbles step by step and the raw material tank are both provided with an electric heating sleeve, and a slurry bed reactor is provided with a cooling system, and the reaction process comprises the following steps:
1) The gas-liquid inlet of the supergravity gas mixing device for cutting bubbles step by step is respectively connected with a gas steel bottle and a raw material tank, the gas-liquid outlet of the supergravity gas mixing device for cutting 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 supergravity gas mixing device for cutting bubbles step by step and form liquid-phase circulation, starting a gas steel cylinder to introduce hydrogen after the system is stable, regulating the gas flow by using a gas mass flowmeter, regulating to a preset pressure by using a back pressure valve to perform gas-liquid-solid three-phase catalytic reaction, controlling the pressure of a reaction system by the back pressure valve, and controlling the temperature 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 a vent valve, and flowing the liquid into a raw material tank; in addition, the system can be controlled to be single-pass catalytic reaction or circulating catalytic reaction by controlling the switch of the ball valve, when the ball valve is opened, the system is circulating catalytic reaction, and when the ball valve is closed, the system is single-pass catalytic reaction; the reacted sample was separated and further tested.
Taking 2-nitro-4-acetamido anisole as an example for preparing 2-amino-4-acetamido anisole by catalytic hydrogenation: and adding Raney nickel catalyst into the slurry bed reactor, wherein the rotor stage number of the supergravity gas mixing device for cutting bubbles step by step is 3, and porous filler with hydrophilic nano-micro holes is filled in the rotor. Methanol is used as a solvent to prepare the 2-nitro-4-acetamido anisole working solution with the solid content of 30 percent. Under the conditions that the temperature is 100 ℃ and the pressure is 1.5MPa, and the rotating speed of a supergravity gas mixing device for cutting bubbles step by step is 800r/min, the conversion rate of the 2-nitro-4-acetamido anisole reaches more than 85 percent; under the same temperature, pressure and reaction time, the rotating speed of the supergravity air mixing device for cutting bubbles step by step is only changed to 1500r/min, the conversion rate of the paranitroanisole reaches over 92 percent, and under the same experimental conditions, the supergravity air 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 for cutting bubbles step by step can be used as gas-liquid mixing equipment for catalytic reaction processes participated in by reactors such as fixed beds, stirred tanks, slurry beds and the like, and the gas-liquid contact area in the hydrogenation/oxidation reaction process is increased due to the existence of a large number of microbubbles, and the gas content of a solution to be reacted is improved, 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 scenario is merely illustrative, and the present apparatus may be applied to various gas-liquid mixing processes, or gas-liquid mixing reactions in hydrogenation/oxidation reactions, which are not exhaustive herein, but it is understood that the substitution of the reaction system based on the concept of the present application, although not necessarily one of hydrogenation or oxidation, still falls within the scope of the present application.
It is to be understood that the above examples of the present application are provided by way of illustration only and not by way of limitation of the embodiments of the present application. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. Not all embodiments are exhaustive. All obvious changes or modifications which come within the spirit of the application are desired to be protected.
Claims (11)
1. The supergravity air mixing device for cutting bubbles step by step is characterized by comprising a motor, a rotating shaft, a shell, an air-liquid inlet, an air-supplementing port, an air-liquid outlet, a multistage rotor and bubble crushing parts;
the rotating shaft is used as an output shaft of the motor, extends from the center of the top end of the shell to the inside of the shell, and is connected with the rotor to drive the rotor to rotate;
a plurality of 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 provided with a plurality of layers of gas crushing parts, and the aperture of the gas crushing part of the upper layer is smaller than that of the gas crushing part of the lower layer along with the flowing direction of the gas-liquid mixture;
the upper part outside the shell is provided with a gas-liquid outlet; the shell transversely corresponding to the gaps among the rotors at all levels is provided with an air supplementing port;
the bottom of the shell is provided with a gas-liquid inlet;
the bottom of the rotor is provided with a plurality of pore canals which are convenient for gas and liquid to pass through.
2. The supergravity air mixing device for cutting bubbles step by step according to claim 1, wherein: the multistage rotor in the shell is 3-30 layers, and the interval between each two layers is 10-50 mm.
3. The supergravity air mixing device for cutting bubbles step by step according to claim 2, wherein: the multistage rotor in the shell is 3-5 layers.
4. The supergravity air mixing device for cutting bubbles step by step according to claim 2, wherein: the number of the air supplementing openings is 2-29.
5. The supergravity air mixing device for cutting bubbles step by step according to claim 1, wherein: the gap between the flow guiding piece and the rotor is 2-10mm.
6. The supergravity air mixing device for cutting bubbles step by step according to claim 1, wherein: the surface of the gas crushing part is a hydrophilic surface layer or a hydrophobic surface layer.
7. The supergravity air mixing device for cutting bubbles step by step according to claim 1, wherein: the bubble breaking part is a porous filler with nano-micro holes and a sintered film with nano-micro holes.
8. The supergravity air mixing device for cutting bubbles step by step according to claim 1, wherein: the aperture of the gas crushing part loaded in the multistage rotor is decreased from bottom to top according to equal proportion.
9. The supergravity air mixing device for cutting bubbles step by step according to claim 1, wherein: the pore channels arranged at the bottom of each stage of rotor are symmetrically and uniformly distributed around the axis of the rotary shaft.
10. The supergravity air mixing device for cutting bubbles step by step according to claim 1, wherein: and a gas flow control valve is arranged at the gas-liquid inlet.
11. Use of a supergravity gas mixing device for stepwise cutting of gas bubbles according to any of the claims 1-10, wherein: the application includes a gas-liquid mixing process during a gas-liquid mixing process or during a gas-liquid-solid catalytic reaction;
the gas-liquid mixing process refers to a gas-liquid mixing process involving insoluble gas; the indissolvable gas is one of hydrogen, oxygen, ozone, carbon monoxide, carbon dioxide, nitric oxide and low-carbon hydrocarbon.
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