A continuous preparation device and method of tetrafluoroethane-beta-sultone

Abstract

The application discloses a continuous preparation device for tetrafluoroethane-beta-sultone, which comprises a reactor, a sulfur trioxide supply device, a tetrafluoroethane-beta-sultone supply device, a tetrafluoroethylene supply device, a product buffer tank and a product tank. The application further discloses a method for continuously preparing tetrafluoroethane-beta-sultone by using the device. The application has the advantages of simple structure, high reaction efficiency and safety control.

Description

Technical Field

[0001] This invention relates to the field of tetrafluoroethane-β-sulfonyl lactone technology, and particularly to a continuous preparation apparatus and method for tetrafluoroethane-β-sulfonyl lactone. Background Technology

[0002] Tetrafluoroethane-β-sulfonyl lactone, CAS No.: 697-18-7, molecular formula: C2F4SO3, molecular weight: 180.08, boiling point: 41℃ (101.3KPa), liquid density: 1.6g / ml (25℃), is volatile, has a strong irritant effect, is a colorless and transparent liquid, and is readily soluble in ether solvents.

[0003] Perfluoroalkyl sulfonates are important fluorinated intermediates used to prepare sulfonic acid-containing functional compounds. Tetrafluoroethane-β-sulfonate is a widely used perfluoroalkyl sulfonate. Due to their unique structure, perfluoroalkyl sulfonates can react with various alkenes, cycloalkanes, nucleophiles, etc., to synthesize fluorinated compounds with various structures. These fluorinated compounds are mainly used in the synthesis of functional polymers and fine chemicals, such as PSVE, fluorinated surfactants, and fluorinated oils.

[0004] Tetrafluoroethane-β-sulfonyl lactone is mainly prepared by the addition reaction of sulfur trioxide (SO3) and tetrafluoroethylene (TFE). Currently, the synthesis of tetrafluoroethane-β-sulfonyl lactone usually adopts a batch reactor reaction. This reaction is highly exothermic, the raw materials and products are extremely corrosive, and there is also a risk of explosion. This poses significant safety risks in actual production. Furthermore, the residence time of materials in the reactor in traditional batch reactions is at least 30 minutes, resulting in low efficiency. To address these issues, researchers have made some improvements to the reaction apparatus.

[0005] For example, CN111072627A discloses a method for synthesizing tetrafluoroethane-β-sulfonyl lactone, in which sulfur trioxide and perfluoroolefin are continuously fed into a micromixer for mixing, and then the mixture is introduced into a microchannel reactor for reaction. This method improves the safety of the process, but due to the self-polymerization of TFE, the reactor is prone to clogging.

[0006] For example, CN114950320A discloses a continuous batch reactor, which consists of two batch reactors connected in series. The material from the first reactor overflows into the second reactor through its overflow port. This method has a high product yield, but there are still risks to its safety during scale-up. Summary of the Invention

[0007] The purpose of this invention is to solve the problems of the prior art and provide a continuous preparation device and method for tetrafluoroethane-β-sulfonolactone with simple structure, good mass and heat transfer effect, high reaction efficiency, and safe and controllable process.

[0008] To achieve the above objectives, the technical solution adopted by the present invention is as follows: a continuous preparation apparatus for tetrafluoroethane-β-sulfonyl lactone, comprising a reactor, a sulfur trioxide supply device, a tetrafluoroethane-β-sulfonyl lactone supply device, a tetrafluoroethylene supply device, a product buffer tank, and a product tank. The reactor is a hypergravity reactor, which includes a shell. An isolation component is provided inside the shell to divide the interior of the shell into an upper product chamber and a lower reaction chamber. The isolation component is provided with multiple reaction product conveying channels connecting the reaction chamber and the product chamber. A product overflow port is provided on the side of the product chamber, and the product overflow port is connected to the product buffer tank. The liquid phase outlet of the product buffer tank is connected to the product tank. A rotating packed bed is provided inside the reaction chamber, and a reaction chamber is provided at the center of the rotating packed bed. A packing chamber for placing packing is provided around the reaction chamber. The sulfur trioxide supply device and the tetrafluoroethane-β-sulfonyl lactone supply device are connected to the reaction chamber through liquid feed pipes, and the tetrafluoroethylene supply device is connected to the reaction chamber through a gas feed pipe.

[0009] Compared with existing technologies, the advantages of this invention are as follows: Utilizing the efficient mass and heat transfer characteristics of a hypergravity reactor, the heat generated by the reaction can be removed in a timely manner, reducing the self-polymerization of tetrafluoroethylene and the generation of byproducts; the powerful hypergravity field generated by the high-speed rotation of the rotating packed bed improves the mass transfer and reaction efficiency of the fluid reactants in the hypergravity field, ensuring stable material ratios and effective contact, resulting in uniform temperature distribution during the reaction and significantly enhanced reaction stability control; the mixed feeding of sulfur trioxide and tetrafluoroethane-β-sulfonyl lactone mother liquor further enhances the heat transfer efficiency of the reaction and improves the safety of the reaction.

[0010] The working principle of the hypergravity reactor in this invention is that the rotating packing layer, driven by a motor, generates a strong hypergravity field through high-speed rotation. This field enhances the mass and heat transfer efficiency and reaction rate of the fluid reactants, thereby increasing the reaction rate. The magnitude of the hypergravity field can be controlled by adjusting the motor speed. Gas is drawn in by the high-speed centrifugal liquid flow generated within the rotating packing bed. Through the centrifugal liquid flow and the secondary segmentation of the packing layer, the gas is broken into micron-sized microbubbles that are uniformly dispersed in the liquid, enabling efficient mixing, rapid mass transfer, and chemical reactions between the gas and liquid phases. The advantages of gas reacting with the liquid phase in the form of microbubbles are a large contact area, a small total amount of matter within the microbubbles, and the ability for mass transfer and chemical reactions to be completed instantaneously, thus improving conversion rate and reaction efficiency.

[0011] The apparatus for the continuous preparation of tetrafluoroethane-β-sulfonolactone of the present invention is small in size, requires less space, is more efficient, has a larger production capacity, and is easy to industrialize.

[0012] In order to better achieve gas-liquid separation of the product, as a preferred embodiment of the present invention, a gas outlet is provided at the top of the product chamber, and the gas outlet is connected to the product buffer tank.

[0013] In a preferred embodiment of the present invention, the preparation apparatus further includes a tetrafluoroethylene recovery device, wherein the gas phase outlet of the product buffer tank is connected to the tetrafluoroethylene recovery device.

[0014] In a preferred embodiment of the present invention, the tetrafluoroethylene recovery device is connected to the gas feed pipe.

[0015] In a preferred embodiment of the present invention, the liquid feed pipe and the gas feed pipe are connected to the reaction chamber through the isolation member from the top of the housing.

[0016] In a preferred embodiment of the present invention, the reaction product delivery channels are uniformly distributed along the axial direction.

[0017] The present invention also provides a method for the continuous preparation of tetrafluoroethane-β-sulfonolactone using the above-described apparatus, comprising the following steps: (1) Tetrafluoroethane-β-sulfonyl lactone and sulfur trioxide are continuously fed into the hypergravity reactor through the liquid feed pipe, while tetrafluoroethylene is continuously fed into the hypergravity reactor through the gas feed pipe, and the reaction takes place in the reaction chamber. (2) Under the centrifugal action of the rotating packed bed, the reaction products pass through the packing cavity and enter the reaction chamber, then enter the product chamber through the reaction product conveying channel, and flow into the product buffer tank through the product overflow port. (3) Tetrafluoroethane-β-sulfonolactone enters the product tank through the liquid phase outlet of the product buffer tank.

[0018] In a preferred embodiment of the present invention, the preparation apparatus further includes a tetrafluoroethylene recovery device, wherein unreacted tetrafluoroethylene enters the tetrafluoroethylene recovery device through the gas phase outlet of the product buffer tank.

[0019] In a preferred embodiment of the present invention, in the supergravity reactor, the amount of tetrafluoroethane-β-sulfonyl lactone is 20-60% of the volume of the supergravity reactor; the feed molar ratio of sulfur trioxide to tetrafluoroethylene is 1:1.5-2; the reaction temperature is 25-35°C; the reaction pressure is 0.05-0.3 MPa; and the residence time is 2-12 minutes.

[0020] In a preferred embodiment of the present invention, the liquid level in the product buffer tank is controlled at 30-60%.

[0021] This invention utilizes a hypergravity reactor and optimized process parameters to achieve the continuous addition reaction of sulfur trioxide and tetrafluoroethylene to prepare tetrafluoroethane-β-sulfonolactone. This simplifies the operation process and shortens the reaction time. Compared to traditional batch reactions where the material residence time is at least 30 minutes, the residence time of this invention is only 2–12 minutes, significantly simplifying the production process and improving reaction efficiency. Furthermore, the short residence time allows a large amount of reaction heat energy to be promptly removed from the hypergravity reactor, reducing the risk of tetrafluoroethylene self-polymerization due to localized overheating. Attached Figure Description

[0022] Figure 1 This is a schematic diagram of the apparatus for the continuous preparation of tetrafluoroethane-β-sulfonolactone according to the present invention.

[0023] Figure 2 This is a schematic diagram of the structure of the supergravity reactor in this invention.

[0024] In the diagram, 1 is a sulfur trioxide metering tank, 2 is a sulfur trioxide metering pump, 3 is a tetrafluoroethane-β-sulfonyl lactone tank, 4 is a transfer pump, 5 is a tetrafluoroethylene tank, 6 is a tetrafluoroethylene flow meter, 7 is a high-gravity reactor, 8 is a product buffer tank, 9 is a liquid level controller, 10 is a product tank, 11 is a tetrafluoroethylene recovery pump, 12 is a tetrafluoroethylene recovery tank, 13 is a recovery flow meter, 21 is a liquid feed pipe, 22 is a gas feed pipe, 23 is a product overflow port, 24 is a gas outlet port, 25 is a reaction product conveying channel, 26 is a packing cavity, 27 is a rotating shaft, 28 is a motor, 29 is a shell, 30 is an isolation component, 31 is a product bin, 32 is a reaction bin, and 33 is a reaction chamber. Detailed Implementation

[0025] As shown in the attached drawings, a continuous preparation apparatus for tetrafluoroethane-β-sulfonyl lactone according to the present invention includes a hypergravity reactor 7, a sulfur trioxide supply device consisting of a sulfur trioxide metering tank 1 and a sulfur trioxide metering pump 2, a tetrafluoroethane-β-sulfonyl lactone supply device consisting of a tetrafluoroethane-β-sulfonyl lactone tank 3 and a transfer pump 4, a tetrafluoroethylene supply device consisting of a tetrafluoroethylene tank 5 and a tetrafluoroethylene flow meter 6, a product buffer tank 8, a liquid level controller 9, and a product tank 10. The hypergravity reactor 7 includes a shell 29, and an isolation structure is provided inside the shell 29. The isolation component 30 divides the interior of the shell 29 into an upper product chamber 31 and a lower reaction chamber 32. The isolation component 30 is provided with multiple reaction product conveying channels 25 connecting the reaction chamber 32 and the product chamber 31. These channels 25 are evenly distributed axially. The product chamber 31 has a product overflow port 23 on its side, which is connected to the product buffer tank 8. The liquid phase outlet of the product buffer tank 8 is connected to the product tank 10 via the liquid level controller 9. A rotating packed bed is provided inside the reaction chamber 32, with a reaction chamber 33 at its center. A packing chamber 26 for placing packing material is provided around the reaction chamber 33. The rotating packed bed is connected to the motor 28 via the rotating shaft 27. The sulfur trioxide supply device and the tetrafluoroethane-β-sulfonyl lactone supply device are connected to the reaction chamber 33 via a liquid feed pipe 21. The tetrafluoroethylene supply device is connected to the reaction chamber 33 via a gas feed pipe 22. The liquid feed pipe 21 and the gas feed pipe 22 are connected to the reaction chamber 33 via the gas feed pipe 22. The feed pipe 22 passes through the isolation member 30 from the top of the shell 29 and communicates with the reaction chamber 33. The top of the product chamber 31 is provided with a gas outlet 24, which is connected to the product buffer tank 8. The preparation device also includes a tetrafluoroethylene recovery device consisting of a tetrafluoroethylene recovery pump 11, a tetrafluoroethylene recovery tank 12, and a recovery flow meter 13. The gas phase outlet of the product buffer tank 8 is connected to the tetrafluoroethylene recovery device; the tetrafluoroethylene recovery device is connected to the gas feed pipe 22.

[0026] The process flow for the continuous preparation of tetrafluoroethane-β-sulfonolactone using this device is as follows: (1) Tetrafluoroethane-β-sulfonyl lactone and sulfur trioxide are continuously fed into the hypergravity reactor 7 through the liquid feed pipe 21, while tetrafluoroethylene is continuously fed into the hypergravity reactor 7 through the gas feed pipe 22, and reacted in the reaction chamber 33. (2) Under the centrifugal force of the rotating packed bed, the reaction products enter the reaction chamber 32 after passing through the packing cavity 26, and then enter the product chamber 31 through the reaction product conveying channel 25, and flow into the product buffer tank 8 through the product overflow port 23; the unreacted tetrafluoroethylene enters the product buffer tank 8 through the gas outlet 24 of the supergravity reactor 7, and is then compressed to the tetrafluoroethylene recovery tank 12 by the tetrafluoroethylene recovery pump 11, and returned to the supergravity reactor 7 for recycling after being measured by the recovery flow meter 13; (3) Tetrafluoroethane-β-sulfonyl lactone enters the product tank 10 through the liquid phase outlet of the product buffer tank 8.

[0027] The present invention will be further described in detail below through embodiments. It should be understood that the embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.

[0028] Example 1 A continuous preparation apparatus for tetrafluoroethane-β-sulfonyl lactone includes a centrifugal reactor 7 (cylindrical, 5L volume, 316L material), a sulfur trioxide supply device consisting of a sulfur trioxide metering tank 1 and a sulfur trioxide metering pump 2, a tetrafluoroethane-β-sulfonyl lactone supply device consisting of a tetrafluoroethane-β-sulfonyl lactone tank 3 and a transfer pump 4, a tetrafluoroethylene supply device consisting of a tetrafluoroethylene tank 5 and a tetrafluoroethylene flow meter 6, a product buffer tank 8, a level controller 9, and a product tank 10. The centrifugal reactor 7 includes a shell 29, and an isolation device is provided inside the shell 29. Component 30 divides the interior of shell 29 into an upper product chamber 31 and a lower reaction chamber 32. Sixteen reaction product conveying channels 25, connecting the reaction chamber 32 and the product chamber 31, are provided on the isolation component 30. These sixteen channels are evenly distributed axially. A product overflow port 23 is provided on the side of the product chamber 31, and the product overflow port 23 is connected to the product buffer tank 8. The liquid phase outlet of the product buffer tank 8 is connected to the product tank 10 via a level controller 9. The level controller 9 uses a differential pressure level gauge and a regulating valve to interlock and control the liquid level in the product buffer tank 8. A rotating packed bed is installed inside the reaction chamber 32. A reaction chamber 33 is located at the center of the rotating packed bed. A packing chamber 26 (filled with φ1.5mm 316L triangular spiral packing) is arranged around the reaction chamber 33. The rotating packed bed is connected to a motor 28 via a rotating shaft 27. A sulfur trioxide supply device and a tetrafluoroethane-β-sulfonyl lactone supply device are connected to the reaction chamber 33 via a liquid feed pipe 21. A tetrafluoroethylene supply device is connected to the reaction chamber 33 via a gas feed pipe 22. The liquid feed pipe 21 and the gas feed pipe 22 pass through the top of the shell 29. The isolation component 30 is connected to the reaction chamber 33. The top of the product chamber 31 is provided with a gas outlet 24, which is connected to the product buffer tank 8 to maintain the pressure balance between the hypergravity reactor 7 and the product buffer tank 8 and prevent the reaction pressure fluctuation of the hypergravity reactor 7 from affecting the reaction effect. The preparation device also includes a tetrafluoroethylene recovery device consisting of a tetrafluoroethylene recovery pump 11, a tetrafluoroethylene recovery tank 12 and a recovery flow meter 13. The gas phase outlet of the product buffer tank 8 is connected to the tetrafluoroethylene recovery device; the tetrafluoroethylene recovery device is connected to the gas feed pipe 22.

[0029] The process parameters for the continuous preparation of tetrafluoroethane-β-sulcinolone using this apparatus are as follows: The amount of tetrafluoroethane-β-sulfonyl lactone pumped into the hypergravity reactor by the transfer pump is 20% of the volume of the hypergravity reactor; the feed molar ratio of sulfur trioxide to tetrafluoroethylene is 1:1.5; the operating temperature of the hypergravity reactor is 25℃, the pressure is 0.05Mpa, and the residence time is 2 minutes; the liquid level in the product buffer tank is controlled at 30%.

[0030] Example 2 A continuous preparation apparatus for tetrafluoroethane-β-sulfonyl lactone includes a centrifugal reactor 7 (cylindrical, 5L volume, 316L material), a sulfur trioxide supply device consisting of a sulfur trioxide metering tank 1 and a sulfur trioxide metering pump 2, a tetrafluoroethane-β-sulfonyl lactone supply device consisting of a tetrafluoroethane-β-sulfonyl lactone tank 3 and a transfer pump 4, a tetrafluoroethylene supply device consisting of a tetrafluoroethylene tank 5 and a tetrafluoroethylene flow meter 6, a product buffer tank 8, a level controller 9, and a product tank 10. The centrifugal reactor 7 includes a shell 29, and an isolation device is provided inside the shell 29. Component 30 divides the interior of shell 29 into an upper product chamber 31 and a lower reaction chamber 32. Fourteen reaction product conveying channels 25, connecting the reaction chamber 32 and the product chamber 31, are provided on the isolation component 30. These fourteen channels are evenly distributed axially. A product overflow port 23 is provided on the side of the product chamber 31, which is connected to a product buffer tank 8. The liquid phase outlet of the product buffer tank 8 is connected to the product tank 10 via a level controller 9. The level controller 9 uses a differential pressure level gauge and a regulating valve to interlock and control the liquid level in the product buffer tank 8. A rotating packed bed is installed inside the reaction chamber 32. A reaction chamber 33 is located at the center of the rotating packed bed. A packing chamber 26 (filled with φ1.5mm 316L triangular spiral packing) is arranged around the reaction chamber 33. The rotating packed bed is connected to a motor 28 via a rotating shaft 27. A sulfur trioxide supply device and a tetrafluoroethane-β-sulfonyl lactone supply device are connected to the reaction chamber 33 via a liquid feed pipe 21. A tetrafluoroethylene supply device is connected to the reaction chamber 33 via a gas feed pipe 22. The liquid feed pipe 21 and the gas feed pipe 22 pass through the top of the shell 29. The isolation component 30 is connected to the reaction chamber 33. The top of the product chamber 31 is provided with a gas outlet 24, which is connected to the product buffer tank 8 to maintain the pressure balance between the hypergravity reactor 7 and the product buffer tank 8 and prevent the reaction pressure fluctuation of the hypergravity reactor 7 from affecting the reaction effect. The preparation device also includes a tetrafluoroethylene recovery device consisting of a tetrafluoroethylene recovery pump 11, a tetrafluoroethylene recovery tank 12 and a recovery flow meter 13. The gas phase outlet of the product buffer tank 8 is connected to the tetrafluoroethylene recovery device; the tetrafluoroethylene recovery device is connected to the gas feed pipe 22.

[0031] The process parameters for the continuous preparation of tetrafluoroethane-β-sulcinolone using this apparatus are as follows: The amount of tetrafluoroethane-β-sulfonyl lactone pumped into the hypergravity reactor by the transfer pump is 30% of the volume of the hypergravity reactor; the feed molar ratio of sulfur trioxide to tetrafluoroethylene is 1:1.6; the operating temperature of the hypergravity reactor is 28℃, the pressure is 0.1 MPa, and the residence time is 5 minutes; the liquid level in the product buffer tank is controlled at 40%.

[0032] Example 3 A continuous preparation apparatus for tetrafluoroethane-β-sulfonyl lactone includes a centrifugal reactor 7 (cylindrical, 5L volume, 316L material), a sulfur trioxide supply device consisting of a sulfur trioxide metering tank 1 and a sulfur trioxide metering pump 2, a tetrafluoroethane-β-sulfonyl lactone supply device consisting of a tetrafluoroethane-β-sulfonyl lactone tank 3 and a transfer pump 4, a tetrafluoroethylene supply device consisting of a tetrafluoroethylene tank 5 and a tetrafluoroethylene flow meter 6, a product buffer tank 8, a level controller 9, and a product tank 10. The centrifugal reactor 7 includes a shell 29, and an isolation device is provided inside the shell 29. Component 30 divides the interior of shell 29 into an upper product chamber 31 and a lower reaction chamber 32. Twenty reaction product conveying channels 25, connecting the reaction chamber 32 and the product chamber 31, are provided on the isolation component 30. These twenty channels are evenly distributed axially. A product overflow port 23 is provided on the side of the product chamber 31, which is connected to a product buffer tank 8. The liquid phase outlet of the product buffer tank 8 is connected to the product tank 10 via a level controller 9. The level controller 9 uses a differential pressure level gauge and a regulating valve to interlock and control the liquid level in the product buffer tank 8. A rotating packed bed is installed inside the reaction chamber 32. A reaction chamber 33 is located at the center of the rotating packed bed. A packing chamber 26 (filled with φ1.5mm 316L triangular spiral packing) is arranged around the reaction chamber 33. The rotating packed bed is connected to a motor 28 via a rotating shaft 27. A sulfur trioxide supply device and a tetrafluoroethane-β-sulfonyl lactone supply device are connected to the reaction chamber 33 via a liquid feed pipe 21. A tetrafluoroethylene supply device is connected to the reaction chamber 33 via a gas feed pipe 22. The liquid feed pipe 21 and the gas feed pipe 22 pass through the top of the shell 29. The isolation component 30 is connected to the reaction chamber 33. The top of the product chamber 31 is provided with a gas outlet 24, which is connected to the product buffer tank 8 to maintain the pressure balance between the hypergravity reactor 7 and the product buffer tank 8 and prevent the reaction pressure fluctuation of the hypergravity reactor 7 from affecting the reaction effect. The preparation device also includes a tetrafluoroethylene recovery device consisting of a tetrafluoroethylene recovery pump 11, a tetrafluoroethylene recovery tank 12 and a recovery flow meter 13. The gas phase outlet of the product buffer tank 8 is connected to the tetrafluoroethylene recovery device; the tetrafluoroethylene recovery device is connected to the gas feed pipe 22.

[0033] The process parameters for the continuous preparation of tetrafluoroethane-β-sulcinolone using this apparatus are as follows: The amount of tetrafluoroethane-β-sulfonyl lactone pumped into the hypergravity reactor by the transfer pump is 50% of the volume of the hypergravity reactor; the feed molar ratio of sulfur trioxide to tetrafluoroethylene is 1:1.8; the operating temperature of the hypergravity reactor is 32℃, the pressure is 0.2 MPa, and the residence time is 9 minutes; the liquid level in the product buffer tank is controlled at 50%.

[0034] Example 4 A continuous preparation apparatus for tetrafluoroethane-β-sulfonyl lactone includes a centrifugal reactor 7 (cylindrical, 5L volume, 316L material), a sulfur trioxide supply device consisting of a sulfur trioxide metering tank 1 and a sulfur trioxide metering pump 2, a tetrafluoroethane-β-sulfonyl lactone supply device consisting of a tetrafluoroethane-β-sulfonyl lactone tank 3 and a transfer pump 4, a tetrafluoroethylene supply device consisting of a tetrafluoroethylene tank 5 and a tetrafluoroethylene flow meter 6, a product buffer tank 8, a level controller 9, and a product tank 10. The centrifugal reactor 7 includes a shell 29, and an isolation device is provided inside the shell 29. Component 30 divides the interior of shell 29 into an upper product chamber 31 and a lower reaction chamber 32. Eighteen reaction product conveying channels 25, connecting the reaction chamber 32 and the product chamber 31, are provided on the isolation component 30. These eighteen channels are evenly distributed axially. A product overflow port 23 is provided on the side of the product chamber 31, which is connected to a product buffer tank 8. The liquid phase outlet of the product buffer tank 8 is connected to the product tank 10 via a level controller 9. The level controller 9 uses a differential pressure level gauge and a regulating valve to interlock and control the liquid level in the product buffer tank 8. A rotating packed bed is installed inside the reaction chamber 32. A reaction chamber 33 is located at the center of the rotating packed bed. A packing chamber 26 (filled with φ1.5mm 316L triangular spiral packing) is arranged around the reaction chamber 33. The rotating packed bed is connected to a motor 28 via a rotating shaft 27. A sulfur trioxide supply device and a tetrafluoroethane-β-sulfonyl lactone supply device are connected to the reaction chamber 33 via a liquid feed pipe 21. A tetrafluoroethylene supply device is connected to the reaction chamber 33 via a gas feed pipe 22. The liquid feed pipe 21 and the gas feed pipe 22 pass through the top of the shell 29. The isolation component 30 is connected to the reaction chamber 33. The top of the product chamber 31 is provided with a gas outlet 24, which is connected to the product buffer tank 8 to maintain the pressure balance between the hypergravity reactor 7 and the product buffer tank 8 and prevent the reaction pressure fluctuation of the hypergravity reactor 7 from affecting the reaction effect. The preparation device also includes a tetrafluoroethylene recovery device consisting of a tetrafluoroethylene recovery pump 11, a tetrafluoroethylene recovery tank 12 and a recovery flow meter 13. The gas phase outlet of the product buffer tank 8 is connected to the tetrafluoroethylene recovery device; the tetrafluoroethylene recovery device is connected to the gas feed pipe 22.

[0035] The process parameters for the continuous preparation of tetrafluoroethane-β-sulcinolone using this apparatus are as follows: The amount of tetrafluoroethane-β-sulfonyl lactone pumped into the hypergravity reactor by the transfer pump is 60% of the volume of the hypergravity reactor; the feed molar ratio of sulfur trioxide to tetrafluoroethylene is 1:2; the operating temperature of the hypergravity reactor is 35℃, the pressure is 0.3Mpa, and the residence time is 12 minutes; the liquid level in the product buffer tank is controlled at 60%.

Claims

1. A continuous preparation apparatus for tetrafluoroethane-β-sulfanolactone, comprising a reactor, a sulfur trioxide supply device, a tetrafluoroethane-β-sulfanolactone supply device, a tetrafluoroethylene supply device, a product buffer tank, a product tank, and a tetrafluoroethylene recovery device, characterized in that, The reactor is a hypergravity reactor, comprising a shell. An isolation component within the shell divides the interior into an upper product chamber and a lower reaction chamber. The isolation component has multiple reaction product transport channels connecting the reaction chamber and the product chamber. A gas outlet is located at the top of the product chamber, and a product overflow outlet is located on its side. Both the gas outlet and the product overflow outlet are connected to a product buffer tank. The liquid phase outlet of the product buffer tank is connected to the product tank, and the gas phase outlet of the product buffer tank is connected to the tetrafluoroethylene recovery device. A rotating packed bed is located within the reaction chamber, with a reaction chamber at its center. A packing chamber for placing packing material is located around the reaction chamber. A sulfur trioxide supply device and a tetrafluoroethane-β-sulfonyl lactone supply device are connected to the reaction chamber via liquid feed pipes. The tetrafluoroethylene supply device is connected to the reaction chamber via a gas feed pipe, and the tetrafluoroethylene recovery device is connected to the gas feed pipe.

2. The continuous preparation apparatus for tetrafluoroethane-β-sulfanolactone according to claim 1, characterized in that, The liquid feed pipe and the gas feed pipe are connected to the reaction chamber through the isolation member from the top of the housing.

3. The continuous preparation apparatus for tetrafluoroethane-β-sulfanolactone according to claim 1 or 2, characterized in that, The reaction product transport channels are uniformly distributed along the axial direction.

4. A method for the continuous preparation of tetrafluoroethane-β-sulfanolactone using the apparatus of claim 1, characterized in that, Includes the following steps: (1) Tetrafluoroethane-β-sulfonyl lactone and sulfur trioxide are continuously fed into the hypergravity reactor through the liquid feed pipe, while tetrafluoroethylene is continuously fed into the hypergravity reactor through the gas feed pipe, and the reaction takes place in the reaction chamber. (2) Under the centrifugal action of the rotating packed bed, the reaction products pass through the packing cavity and enter the reaction chamber, then enter the product chamber through the reaction product conveying channel, and flow into the product buffer tank through the product overflow port. (3) Tetrafluoroethane-β-sulfonolactone enters the product tank through the liquid phase outlet of the product buffer tank.

5. The method for continuous preparation of tetrafluoroethane-β-sulfolactone according to claim 4, characterized in that, Unreacted tetrafluoroethylene enters the tetrafluoroethylene recovery unit through the gas phase outlet of the product buffer tank.

6. The method for continuous preparation of tetrafluoroethane-β-sulfanolactone according to claim 4, characterized in that, In the aforementioned hypergravity reactor, the amount of tetrafluoroethane-β-sulfonyl lactone is 20-60% of the volume of the hypergravity reactor; the feed molar ratio of sulfur trioxide to tetrafluoroethylene is 1:1.5-2; the reaction temperature is 25-35°C; the reaction pressure is 0.05-0.3 MPa; and the residence time is 2-12 minutes.

7. The method for continuous preparation of tetrafluoroethane-β-sulfolactone according to claim 4, characterized in that, The liquid level in the product buffer tank is controlled between 30% and 60%.

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