A high gravity microwave coupling reaction system and method

The supergravity microwave coupled reaction system solves the problem of high viscosity and high melting point materials being prone to agglomeration and blockage in supergravity equipment, realizes timely heat replenishment and efficient mass transfer of materials, and improves reaction efficiency.

CN116617977BActive Publication Date: 2025-10-17BEIJING UNIV OF CHEM TECH
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Patent Information

Application Number
CN202310361038.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-04-06
Publication Date
2025-10-17
Estimated Expiration
2043-04-06

AI Technical Summary

Technical Problem

Existing supergravity equipment has difficulty in handling high-viscosity and high-melting-point materials, resulting in problems such as easy agglomeration, easy clogging, and difficulty in flowing the materials.

Method used

A supergravity microwave coupled reaction system is used. By setting a shearing unit in the supergravity device, the material is sheared into micro-nano scale fluid elements. The fluid elements are then heated by a microwave device, and heated and excited by an electromagnetic induction coil.

Benefits of technology

Under strong centrifugal force, timely heat replenishment of materials is achieved, improving the efficiency of mass transfer process and the stability of chemical reaction. Molecular-level molecular surface contact opportunities are increased, and reaction efficiency is improved by more than 50%.

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Abstract

The application provides a supergravity microwave coupling reaction system and method, which can overcome the defects of the prior art, solve the problem that current supergravity equipment is difficult to process high-melting-point and high-viscosity materials, and cause the materials to be prone to caking, blocking and difficult to flow, and keep the material temperature from falling by the way of microwave device coupling supergravity device for heat compensation. The supergravity device designed in the application can complete the mass transfer process under the condition of timely heat compensation in a strong centrifugal force environment, and the molecular diffusion and interphase mass transfer process is much faster than that under a conventional gravity field, the huge shear force can tear the liquid into micron or even nanometer liquid film, liquid line and liquid drop, generate a huge and rapidly updated phase interface, strengthen the mass transfer process, and can make the separation efficiency of the product increased by more than 50%.
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Description

TECHNICAL FIELD

[0001] The present application relates to the field of reactor technology, more particularly, to a supergravity microwave coupling reaction system and method. BACKGROUND

[0002] Supergravity technology is a new generation of chemical process intensification technology. It can simulate supergravity environment through strong centrifugal field generated by high-speed rotation, so as to realize great intensification of mass transfer and mixing. Supergravity technology has been successfully and widely applied in chemical processes such as intensification of mass transfer and mixing. Supergravity technology utilizes rotation to create a stable and adjustable centrifugal field. It uses a rotating annular porous packing bed instead of a vertical stationary packing tower, so that gas and liquid phases can fully contact in the rotating packing layer, thereby completing mass transfer and heat transfer. Microwave heating, as a new heating method, has the advantages of fast heating speed, strong controllability, cleanliness and no pollution, and is getting more and more attention. Microwave heating belongs to bulk heating, that is, microwaves directly act on polar molecules, making the molecules produce heat through vibration and collision, thereby directly converting electromagnetic energy into heat energy. During microwave heating, heat is generated directly from the inside of the material, rather than being transferred from the surface of the material to the inside through heat conduction as in traditional heating. This can greatly improve the heating efficiency and avoid the temperature gradient from the surface to the inside of the material in traditional heating methods, achieving a more uniform heating effect and improving the reliability of the reaction. By combining supergravity technology and microwave technology to make a supergravity microwave coupling reactor, the advantages and characteristics of both technologies can be combined to further reduce energy consumption, improve efficiency, and reduce pollution. However, the current supergravity microwave reactor has problems when dealing with materials that need to be preheated. The heat of the fluid itself is lost through heat conduction when it comes into contact with the packing. Some high-melting-point, high-viscosity fluids are prone to solidification, caking, and blockage under such conditions. SUMMARY

[0003] The technical problem to be solved by the present application is to provide a supergravity device that can be used to process high-melting-point, high-viscosity fluids. The device solves the problem of current supergravity devices that are difficult to process high-viscosity, high-melting-point materials. It can ensure that the material temperature does not drop in the supergravity device. It solves the problem of high-viscosity, high-melting-point materials that are prone to caking, blocking, and difficult to flow in the supergravity device, making the supergravity device capable of processing high-viscosity, high-melting-point material processes.

[0004] To solve at least one of the above problems, in a first aspect, the present application provides a supergravity microwave coupling reaction system, comprising: a supergravity device and a microwave device.

[0005] The super gravity device comprises a reaction cavity and a shearing unit arranged inside the reaction cavity, the shearing unit is used for shearing a reaction material introduced into the super gravity device into fluid micro elements of micro-nano scale, and the reaction material has a viscosity and a melting point higher than a set threshold value.

[0006] The microwave device is fixed on the outer surface of the shell of the super gravity device, and the microwave generator can feed microwaves into the super gravity device for heating the fluid micro elements.

[0007] Further, the super gravity microwave coupling reaction system further comprises an electromagnetic induction coil connected with the shearing unit, and used for heating the shearing unit and the reaction material in the shearing unit.

[0008] Further, the microwave device further comprises a microwave controller used for controlling the power of the microwave generator.

[0009] Further, the shearing unit comprises:

[0010] a pair of rotating discs arranged oppositely, a ring-shaped shearing space being formed between the rotating discs and surrounding a central region of the shearing space, and the electromagnetic induction coil being arranged on the outer surface of the rotating discs;

[0011] shearing fillers each fixed on one side surface of one of the rotating discs and filled in the shearing space;

[0012] a liquid distributor inserted into the central region and capable of spraying the reaction material into the shearing space.

[0013] Further, the shearing unit further comprises a rotating shaft and a motor, the motor drives the rotating shaft to rotate, and one of the rotating discs is fixedly combined with the free end of the rotating shaft.

[0014] Further, the microwave device comprises one or more.

[0015] Further, a vacuum pump is connected to the gas outlet of the super gravity device.

[0016] Further, the power of the microwave generator is 100W-6000W.

[0017] Further, the heating threshold value of the electromagnetic induction coil is 200KW.

[0018] In a second aspect, the present application provides a super gravity microwave coupling reaction method based on the above super gravity microwave coupling reaction system, comprising:

[0019] starting the electromagnetic induction coil and the microwave device to heat the super gravity device;

[0020] injecting a reaction material, which has a viscosity and a melting point higher than a set threshold, to the heated shearing packing through a heated liquid distributor;

[0021] The reaction material is sheared into fluid micro-units of micro-nano scale by the shearing packing and is guided out from a liquid outlet.

[0022] Advantages of the invention

[0023] The present application provides a supergravity microwave coupling reaction system and method, which can overcome the shortcomings of the prior art, solve the problem that the current supergravity equipment is difficult to process high-melting-point and high-viscosity materials, and cause the materials to be prone to caking, blocking and difficult to flow. The present application maintains the temperature of the materials from falling by the way of heating the materials by the microwave device coupled with the supergravity device. The supergravity device designed in the present application can complete the mass transfer process under the condition of timely heating in the strong centrifugal force environment. The molecular diffusion and interphase mass transfer process is much faster than that under the conventional gravity field. The huge shear force can tear the liquid into micron or even nanometer liquid film, liquid line and liquid droplet, generate a huge and rapidly updated phase interface, strengthen the mass transfer process, and improve the separation efficiency of the product by more than 50%.

[0024] At the same time, the electromagnetic induction coil coupled with the microwave can help control the electromagnetic field in the reactor, thereby enhancing the stability of the reactor. In addition, the microwave and the electromagnetic induction coil can provide additional excitation energy, thereby accelerating the chemical reaction in the reactor. At the same time, with the help of the supergravity super-strong mass transfer effect, the excitation energy can be transmitted to every local area in the reactor in an instant, greatly improving the reaction efficiency and making the reaction molecules in a sustained active state. At the same time, due to the energy excited by the single excitation source, most of the molecules have resonance effect, so although the molecules vibrate at the molecular level, the vibration frequency and direction are uniform, resulting in less opportunity for molecular contact. The present application couples the microwave through the electromagnetic induction coil 1-5, forms multiple excitation sources, and the types and parameters of the excitation sources are different, thereby avoiding the resonance effect. The vibration of each molecule is more random, greatly improving the opportunity for molecular surface contact at the molecular level and greatly improving the reaction efficiency. BRIEF DESCRIPTION OF DRAWINGS

[0025] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings needed to be used in the embodiments or prior art description will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without creative labor.

[0026] Figure 1Schematic diagram of the structure of the supergravity microwave coupled reaction system in an embodiment of the present invention;

[0027] Figure 2 This is a schematic diagram of the overall structure of the supergravity microwave coupled reaction system in an embodiment of the present invention;

[0028] Description of the drawings: 1-1, housing; 1-2, motor; 1-3, liquid distributor; 1-4, material inlet; 1-5, electromagnetic induction coil; 1-6, reaction chamber; 1-7, shear filler; 1-8, microwave generator; 1-9, microwave controller; 1-10, liquid outlet; 1-11, gas outlet. DETAILED DESCRIPTION

[0029] The following will be combined with the accompanying drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0030] For ease of description, the descriptions of "first", "second", etc. in the present invention are provided for descriptive purposes only and should not be understood as indicating or implying their relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" or "second" may explicitly or implicitly include at least one of such features. In addition, the technical solutions between the various embodiments can be combined with each other, but this must be based on the fact that they can be implemented by ordinary technicians in this field. When the combination of technical solutions is contradictory or cannot be implemented, it should be deemed that such a combination of technical solutions does not exist and is not within the scope of protection required by the present invention.

[0031] The current high-gravity equipment is difficult to handle the problem of high viscosity and high melting point materials. Based on this, the present invention provides a high-gravity microwave coupled reaction system, such as Figure 1 As shown, including: supergravity device and microwave device;

[0032] The hypergravity device includes a reaction chamber 1-6 and a shearing unit provided inside the reaction chamber 1-6, wherein the shearing unit is used to shear the reaction material introduced into the hypergravity device into micro-nano-scale fluid elements, and the viscosity and melting point of the reaction material are higher than a set threshold;

[0033] The microwave device is fixed on the outer surface of the shell of the hypergravity device, and the microwave generator can feed microwaves into the hypergravity device to supplement heat for the fluid micro-element.

[0034] In the embodiment, the reactant is a high-viscosity and high-melting-point fluid, and the reaction cavity 1-6 of the supergravity device is provided with a shearing unit, which includes a rotor provided with shearing fillers. The reactant introduced into the supergravity device is sheared and dispersed in the filler layer, and the microwave device continuously reheats the reactant to maintain the temperature of the reactant from falling, thereby strengthening the mass transfer process of the reactant. The microwave device is fixed outside the shell 1-1 of the supergravity device, and one or more microwave devices can be provided according to different systems of the reactant. The microwave device includes a microwave generator 1-8 and a microwave controller 1-9. The microwave controller 1-9 controls the power of the microwave generator according to different systems of the reactant. The power of the microwave generator is 100-6000 W. The specific power is not limited according to different systems.

[0035] As can be seen from the above description, the supergravity microwave coupling reaction system provided by the application can overcome the shortcomings of the prior art, solve the problem that the current supergravity equipment is difficult to process high-melting-point and high-viscosity materials, and cause the materials to be prone to caking, blocking and difficult to flow. The application maintains the temperature of the material from falling by the way of reheating the material by the microwave device coupled with the supergravity device. The supergravity device designed by the application can complete the mass transfer process under the condition of timely reheating in a strong centrifugal force environment. The molecular diffusion and interphase mass transfer process is much faster than that in a conventional gravitational field. The huge shear force can tear the liquid into micron or even nanometer liquid film, liquid line and liquid droplet, generate a huge and rapidly updated phase interface, strengthen the mass transfer process, and improve the separation efficiency of the product by more than 50%.

[0036] At the same time, the electromagnetic induction coil coupled with the microwave can help control the electromagnetic field in the reactor, thereby enhancing the stability of the reactor. In addition, the microwave and the electromagnetic induction coil can provide additional excitation energy, thereby accelerating the chemical reaction in the reactor. At the same time, with the help of the supergravity and the strong mass transfer effect, the excitation energy can be transmitted to every local area in the reactor in an instant, greatly improving the reaction efficiency and making the reaction molecules in a continuous active state. At the same time, since the energy excited by a single excitation source makes most of the molecules have a resonance effect, although the molecules vibrate at the molecular level, the vibration frequency and direction are uniform, so that the contact opportunity between the molecules is small. The application couples the microwave with the electromagnetic induction coil 1-5 to form multiple excitation sources, and the types and parameters of the excitation sources are different, thereby avoiding the resonance effect. The vibration of each molecule is more random, greatly improving the opportunity of contact between the molecules at the molecular level, and greatly improving the reaction efficiency.

[0037] In some specific embodiments, the application also provides another reheating method, such as Figure 1As shown, the high gravity microwave coupling reaction system further comprises: an electromagnetic induction coil 1-5 connected with the shearing unit for heating the shearing unit and the reaction material in the shearing unit.

[0038] In the embodiment, the electromagnetic induction coil 1-5 is divided into two parts, each part is divided into two blocks, and is arranged on the upper part and the lower part of the reaction cavity 1-6. The lower electromagnetic induction coil is close to the shearing unit, and the maximum heating power of the electromagnetic induction coil can reach 200 KW. The specific power selection is not limited according to different systems.

[0039] The microwave coupled by the electromagnetic induction coil 1-5 can help to control the electromagnetic field in the reactor, thereby enhancing the stability of the reactor. In addition, the microwave and the electromagnetic induction coil can provide additional excitation energy, thereby accelerating the chemical reaction in the reactor. At the same time, by means of the super strong mass transfer effect of the high gravity, the excitation energy can be transmitted to every local area in the reactor in an instant, greatly improving the reaction efficiency, making the reaction molecules in a continuous active state, and because the energy excited by the single excitation source makes most of the molecules have resonance effect, although molecular level vibration is generated, the vibration frequency and direction are uniform, so that the contact opportunity between molecules is small. The present application couples the microwave by the electromagnetic induction coil 1-5, forms multiple excitation sources, and the types and parameters of the excitation sources are different, so as to avoid resonance effect, the vibration of each molecule is more random, greatly improving the opportunity of molecular surface contact at the molecular level, and greatly improving the reaction efficiency.

[0040] In some specific embodiments, the shearing unit comprises:

[0041] A pair of rotating discs, and the pair of rotating discs are oppositely arranged, and a ring-shaped shearing space is formed between the pair of rotating discs and arranged around the central region. The outer surface of the rotating disc is provided with the electromagnetic induction coil 1-5;

[0042] Shearing fillers 1-7 are respectively fixed on one side surface of one of the rotating discs and filled in the shearing space;

[0043] A liquid distributor 1-3 is inserted into the central region and can spray the reaction material to the shearing space.

[0044] In the embodiment, the electromagnetic induction coils 1-5 can be arranged on a pair of rotating discs, which heat the rotating discs, the shearing fillers 1-7 and the liquid distributors 1-3, and the rotating discs rotate at a speed of 100-2500 r / min, preferably 600-2000 r / min. The shearing fillers 1-7 are made of stainless steel and can be in the shape of a cylinder or a prism, or other shapes to enhance the contact with the materials. In the application, the shearing fillers 1-7 can be vertical column fillers or other rotating fillers such as wire mesh fillers.

[0045] In some other embodiments, the shearing unit further comprises a rotating shaft and a motor 1-2, the motor 1-2 drives the rotating shaft to rotate, and one of the pair of rotating discs is fixedly connected to the free end of the rotating shaft.

[0046] In the embodiment, the rotating shaft of the motor 1-2 extends through the lower surface of the shell 1-1 into the interior of the shell 1-1, and the upper end of the rotating shaft of the motor 1-2 is fixedly connected to the rotating disc; the liquid distributor 1-3 is fixedly connected to the rotating shaft.

[0047] In some other embodiments, as shown in Figure 1 The gas outlet 1-11 of the supergravity device is connected to a vacuum pump.

[0048] In the embodiment, the vacuum pump can draw the reaction system to be close to vacuum to ensure the smooth feeding of the reaction materials, and the vacuum degree of the vacuum pump ranges from -0.70 MPa to -0.99 MPa in terms of gauge pressure, preferably from -0.080 MPa to -0.099 MPa in terms of gauge pressure.

[0049] The application provides an application method of the supergravity microwave coupling reaction system, which comprises the following steps:

[0050] S1, power on the four electromagnetic induction heating devices to heat the rotor and the fillers through heat conduction and heat radiation, i.e. heat the rotating discs, the liquid distributors and the vertical column filler layers.

[0051] S2, start the vacuum pump to draw the reactor to be close to vacuum to ensure the smooth feeding;

[0052] S3, turn on the microwave generating device;

[0053] S4, turn on the motor to start the rotating discs and the liquid distributors;

[0054] S5, feed the materials into the reaction cavity 1-6, and the materials leave the edge of the distributor at a high speed through the heated rotating discs and the liquid distributors;

[0055] S6, the leaving materials are sheared and stretched by the heated vertical column filler layers, and are broken into micro units to complete the mass transfer process;

[0056] S7, discharging the material from the liquid outlet 1-10.

[0057] In some embodiments of the present application, in step S1, the electromagnetic induction coil heating power is up to 200 KW, and the specific power is not limited according to different systems.

[0058] In some embodiments of the present application, in step S2, the vacuum degree is in the range of-0.70MPa to-0.99MPa in terms of gauge pressure. Preferably, the vacuum degree is in the range of-0.080MPa to-0.099MPa in terms of gauge pressure.

[0059] In some embodiments of the present application, in step S3, the power of the microwave generating device is in the range of 100-6000W; and the specific power is not limited according to different systems.

[0060] In some embodiments of the present application, in step S4, the rotating disc rotation speed is in the range of 100-2500r / min; preferably, the rotation speed is in the range of 600-2000r / min.

[0061] As can be seen from the above description, the supergravity microwave coupling reaction system and method provided by the present application can overcome the shortcomings of the prior art, solve the problem that the current supergravity equipment is difficult to process high-melting-point and high-viscosity materials, and lead to the problems of easy caking, easy blocking and difficult flowing of the materials. The present application maintains the temperature of the material from falling by the way of heating by coupling the microwave device with the supergravity device. The supergravity device designed in the present application can complete the mass transfer process under the condition of timely heating in the strong centrifugal force environment. The molecular diffusion and interphase mass transfer process is much faster than that under the conventional gravity field. The huge shear force can tear the liquid into micron or even nanometer liquid film, liquid line and liquid droplet, produce huge and rapidly updated phase interface, strengthen the mass transfer process, and can make the separation efficiency of the product increase by more than 50%.

[0062] The present application will be described below in conjunction with specific examples.

[0063] Example 1

[0064] As Figure 2This device is used to remove volatile TDI from polyurethane prepolymers. The material is preheated in a raw material tank and then fed into the reactor through a peristaltic pump via a feed pipe. Passing through a heated rotating disc distributor at a speed of 800 rpm, it exerts a significant centrifugal force. Upon exiting the disc, the heated packing layer is sheared and stretched, breaking it into microelements, completing the mass transfer process. Throughout the process, a microwave generator provides supplemental heat to the material, ensuring that the temperature remains constant. The microwave power is controlled at 700W, maintaining the material temperature at approximately 100°C. After the devolatilization process, the product is obtained through a liquid outlet. Testing has shown a volatile matter removal rate of 85%.

[0065] Example 2

[0066] like Figure 2 This device is used to remove volatile acetone from dimethyl silicone oil. The material is preheated in a feed tank, and the reactor is simultaneously evacuated to -0.090 MPa. Driven by the pressure differential of a vacuum pump, the material enters the reactor through a feed pipe. Passing through a heated rotating disc distributor, which exerts a significant centrifugal force at a speed of 1000 r / min, the heated packing layer is sheared and stretched upon exiting the disc, breaking it into microelements and completing the mass transfer process. Throughout the process, a microwave generator provides supplemental heating to maintain temperature. The microwave power is controlled at 500W, maintaining the material at approximately 80°C. After the devolatilization process, the product is obtained through a liquid outlet. Testing has shown a volatile matter removal rate of 82%.

[0067] In the description of this specification, reference to the terms "one embodiment," "some embodiments," "example," "specific example," or "some examples" means that the specific features, structures, materials, or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the embodiment of this specification. In this specification, the exemplary expressions of the above terms do not necessarily refer to the same embodiment or example.

[0068] In addition, those skilled in the art may combine and combine the different embodiments or examples described in this specification, as well as the features of the different embodiments or examples, unless they are mutually inconsistent. The above description is merely an embodiment of the embodiment of this specification and is not intended to limit the embodiment of this specification. For those skilled in the art, various changes and modifications may be made to the embodiment of this specification. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the embodiment of this specification shall be included within the scope of the claims of the embodiment of this specification.

Claims

1. A supergravity microwave coupled reaction device, characterized in that: include: Hypergravity devices and microwave devices; The hypergravity device includes a reaction chamber and a shearing unit disposed inside the reaction chamber, the shearing unit being used to shear the reaction material introduced into the hypergravity device into micro-nano-scale fluid microelements, wherein the viscosity and melting point of the reaction material are higher than a set threshold value; the microwave device is fixed to the outer surface of the hypergravity device housing, and the microwave generator is capable of feeding microwaves into the hypergravity device to supplement the heat of the fluid microelements; The supergravity microwave coupled reaction system also includes: an electromagnetic induction coil, which is connected to the shear unit and is used to heat the shear unit and the reaction material in the shear unit; the microwave device also includes a microwave controller, which is used to control the power of the microwave generator; the power of the microwave generator is between 100W and 6000W, and the microwave device is provided in multiples; the shear unit includes: a pair of turntables, and the pair of turntables are arranged opposite to each other, forming an annular shear space arranged around the central area between the pair of turntables, and the electromagnetic induction coil is arranged on the outer surface of the turntable; shear fillers, each fixed on a side surface of one of the turntables, and filled in the shear space; a liquid distributor, inserted into the central area, and capable of spraying the reaction material into the shear space.

2. The ultra-gravity microwave coupled reaction device according to claim 1, characterized in that: The shearing unit further includes a rotating shaft and a motor, wherein the motor drives the rotating shaft to rotate, and one of the pair of rotating disks is fixedly coupled to a free end of the rotating shaft.

3. The ultra-gravity microwave coupled reaction device according to claim 1, characterized in that: The gas outlet of the supergravity device is connected to a vacuum pump.

4. The ultra-gravity microwave coupled reaction device according to claim 1, characterized in that: The heating threshold of the electromagnetic induction coil is 200KW.

5. An application method of the ultra-gravity microwave coupled reaction device according to any one of claims 1 to 4, characterized in that: include: The electromagnetic induction coil and the microwave device are started to heat the supergravity device; the reaction material is sprayed onto the heated shear filler through the heated liquid distributor, and the viscosity and melting point of the reaction material are higher than the set threshold value; the reaction material is sheared into micro-nano-scale fluid elements by the shear filler and then discharged from the liquid outlet.

Citation Information

Patent Citations

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