Extraction and purification equipment and extraction and purification method
By introducing a reflux pipe in the light-light-removal tower for gas-phase circulating heat exchange and condensation, and using a catalyst plate for multiple purifications in the hydrogenation reactor, the problem of insufficient purity of tetrahydrofuran in the existing technology is solved, achieving the effects of simplified process and improved purity.
Patent Information
- Application Number
- CN202411747858.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-02
- Publication Date
- 2025-01-10
AI Technical Summary
Existing technologies for extracting tetrahydrofuran from BDO tar have insufficient purity, requiring complex steps such as distillation, hydrogenation, and re-distillation to meet the requirements of chemical production. Furthermore, the multi-stage temperature control is complex and makes it difficult to further improve the purity.
By introducing a reflux pipe in the light-light product removal tower for gas-phase circulating heat exchange and condensation, combined with the catalyst plate and hydrogenation reaction in the hydrogenation reactor, multiple purification processes are achieved, simplifying the process and improving product purity.
The preparation process of tetrahydrofuran was simplified, the product purity was improved, and the system's thermal energy was effectively utilized, reducing energy consumption and enabling precise control of product purity.
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Figure CN119286556A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to extraction and purification equipment, in particular to extraction and purification equipment and an extraction and purification method. Background Art
[0002] BDO is an important chemical raw material. A large amount of tar by-product is generated in the production of BDO. Tar contains a large number of components with recycling value. Further extraction and recovery of tar can significantly increase the output of economic products and reduce the cost of hazardous waste treatment and the harm of waste emissions to the environment.
[0003] BDO tar contains a large amount of THF. In the prior art, tetrahydrofuran from BDO tar is extracted by using a BDO light removal tower, and effective components are extracted by using different condensation temperatures. However, this method can only obtain tetrahydrofuran with a purity of 99%. Tetrahydrofuran of this purity cannot be directly used in chemical production, and needs to be removed through subsequent complex distillation, hydrogenation, re-distillation and other steps to improve purity. If the existing BDO light removal tower can be effectively improved to minimize the water content of the output tetrahydrofuran product, the value of the tetrahydrofuran obtained in the process can be improved.
[0004] To this end, those skilled in the art have proposed an apparatus and a method for preparing polymerization-grade tetrahydrofuran from residue, and have made corresponding improvements to the structure of the existing BDO light-removal tower, which can not only effectively utilize the heat energy of the distilled gas phase as a heating source, but also facilitate the temperature control of the distilled gas phase, and facilitate minimizing the water content of the gas phase, so as to achieve the use effect of directly producing polymerization-grade tetrahydrofuran from the system. Summary of the invention
[0005] In view of the deficiencies in the prior art, the present invention provides an extraction and purification device and an extraction and purification method. The vaporized gas phase in the light removal tower is led out through a reflux pipe, heat exchanged with the feed room of the BDO reactor for condensation to obtain a target condensed liquid, and introduced into a hydrogenation reaction tank for hydrogenation reaction. The target condensed liquid is then purified by heat exchange evaporation through a condensation conduit and the feed room of the light removal tower. The liquid component purified by distillation is led out to a THF dehydration tower for subsequent dehydration and purification, which is beneficial to simplifying the preparation process of tetrahydrofuran and effectively recovering system heat energy to achieve energy saving.
[0006] To achieve the above objectives, the present invention is implemented through the following technical scheme: an extraction and purification device, including a BDO reactor, a light removal tower connected to the BDO reactor, and a THF dehydration tower connected to the light removal tower, wherein the BDO reactor and the light removal tower include a complete set of feeding and discharging and thermal evaporation systems.
[0007] In the production of the prior art, raw materials are introduced into the BDO reactor to react and generate a mixture, the mixture is introduced into the light removal tower to evaporate the gas phase for purification, and the purified gas phase is introduced into the THF dehydration tower for further distillation to obtain a tetrahydrofuran product with higher purity.
[0008] However, the light removal tower and THF dehydration tower in the prior art have many distillation steps, and the temperature range needs to be precisely controlled between each step to ensure the purity of the product. One factor that the prior art cannot improve the purity of the product is the complexity of multi-stage temperature control in a limited space, and the purification process is complicated, making it difficult to further improve the purity of the product. Therefore, technicians in this field improve the existing equipment, simplify the product purification process, and further precisely control the product purity.
[0009] A reflux pipe is fixed on the side of the light-removing tower, and both ends of the reflux pipe are respectively connected to the top and bottom ends of the BDO light-removing tower, and the evaporated gas phase in the BDO light-removing tower is circulated through the reflux pipe.
[0010] The side of the reflux pipe is fixedly connected with a heat exchange wing, and the gas phase in the reflux pipe is heat exchanged and condensed with the feed room of the BDO reactor through the heat exchange wing, and the effective components form condensate, while the remaining gas phase enters the light removal tower again through the reflux pipe for circulation.
[0011] A condensation conduit is fixed obliquely on the side of the reflux pipe, and one end of the condensation conduit away from the reflux pipe is connected to a hydrogenation reaction tank. The condensate is separated from the remaining gas phase and discharged into the hydrogenation reaction tank through the condensation conduit, and a hydrogenation reaction is carried out in the hydrogenation reaction tank to purify the tetrahydrofuran component.
[0012] A catalyst plate is arranged inside the hydrogenation reaction tank. Hydrogen is introduced into the hydrogenation reaction tank, and the hydrogen forms bubbles and moves along the surface of the catalyst plate. In the presence of the catalyst, furan reacts with the hydrogen, the double bonds are opened, and each carbon atom is combined with a hydrogen atom to generate tetrahydrofuran.
[0013] A distillation pipe is fixedly connected to the side of the hydrogenation reaction tank. The liquid after the hydrogenation reaction is passed into the distillation pipe for heating to evaporate the tetrahydrofuran component in the liquid. The end of the distillation pipe away from the hydrogenation reaction tank is connected to a reflux pipe. The remaining liquid is passed into the reflux pipe and returns to the light removal tower to obtain purified tetrahydrofuran.
[0014] Preferably, the middle section of the reflux pipe is connected to an inclined pipe section, and the condensation duct is connected to the side of the bottom end of the inclined pipe section. The condensation liquid is collected through the inclined pipe section to ensure that the condensation duct collects the condensation liquid.
[0015] An arc-shaped stopper is fixedly connected to the inner side of the inclined pipe section corresponding to the condensation conduit, and the arc-shaped stopper is used to ensure that the condensate enters the condensation conduit.
[0016] Preferably, the condensation duct includes a water storage section, which is vertically fixed to the reflux pipe. The condensate in the reflux pipe enters the water storage section. Only liquid of a certain depth can pass through the water storage section into the hydrogenation reaction tank, thereby preventing impurities in the mixed gas phase from entering and affecting the purity.
[0017] The end of the water storage section away from the reflux pipe is connected to a lead-out section, and a pressure valve is also provided at the connection between the lead-out section and the water storage section. When the liquid depth in the water storage section reaches a certain level, the condensate can enter the lead-out section through the pressure valve for discharge, thereby preventing the gas pressure of the gas phase transport in the reflux pipe from causing the mixed gas phase to enter the hydrogenation reaction tank.
[0018] Preferably, a main pipe is fixedly connected to the side of the hydrogenation reaction tank, and the main pipe is sleeved outside the light removal tower. The end of the condensation duct away from the reflux pipe is fixedly connected to the main pipe, and all condensation ducts are connected through the main pipe to improve the purification efficiency of the light removal tower.
[0019] A support rod is fixed on the side of the de-lightening tower corresponding to the main pipe, and the main pipe is fixed outside the de-lightening tower through multiple support rods to ensure the collection of condensed liquid in multiple groups of reflux pipes arranged in a ring outside the de-lightening tower.
[0020] Preferably, the feed pipe of the BDO reactor extends to the outside of the reflux pipe and is parallel to the reflux pipe in the opposite direction, and the heat exchange wing is fixedly connected between the feed pipe and the reflux pipe of the BDO reactor. The gas phase in the reflux pipe exchanges heat with the raw material of the BDO reactor through the heat exchange wing, effectively utilizing the heat energy of the gas phase to preheat the raw material, and also cooling and condensing the gas phase.
[0021] The feed pipe of the light removal tower extends to one side of the distillation pipe and is parallel to it in the opposite direction. A power pump and a control valve are provided on the side of each pipeline. The liquid in the distillation tank is heated by the output material in the BDO reactor, and the effective gas phase therein is evaporated for further purification.
[0022] Preferably, an aeration nozzle is fixed to the inner bottom of the hydrogenation reaction tank corresponding to the catalyst plate, and relatively uniform hydrogen bubbles are formed in the condensed liquid through the aeration nozzle.
[0023] The catalyst plate is coaxially fixed on the inner wall of the hydrogenation reaction tank in an inverted cone shape. The inverted cone-shaped catalyst plate can increase the contact area of the reactants and ensure the movement reaction of hydrogen along the catalyst plate.
[0024] The side of the catalyst plate is provided with a guide groove, and the hydrogen bubbles move along the guide groove on the surface of the catalyst plate after contacting the catalyst plate, thereby increasing the contact area between the hydrogen bubbles and the catalyst plate.
[0025] Preferably, honeycomb holes are penetrated through the side of the catalyst plate, and a wedge-shaped block is fixedly connected to the inner side of the guide groove corresponding to the honeycomb holes. When the hydrogen bubbles flow along the guide groove, they can also directly float up through the honeycomb holes, further increasing the contact area between the reactants. The wedge-shaped block has a certain interception effect on the bubbles, allowing the bubbles to float up through the honeycomb holes.
[0026] Preferably, a thin film evaporator is fixed on the inner wall of the distillation tube, and tetrahydrofuran in the condensed liquid is rapidly evaporated into a gas phase through heat exchange, thereby achieving the purpose of purification. The upper side wall of the distillation tube is provided with a gas phase cavity, and the evaporated gas phase enters the gas phase cavity on the upper side of the distillation tube.
[0027] Preferably, the top of the gas phase cavity is connected to a gas phase collecting pipe, through which the tetrahydrofuran gas phase is collected, and the other end of the gas phase collecting pipe is connected to a distillation tank, and the purified tetrahydrofuran gas phase is passed into the distillation tank, which is convenient for multiple purifications to improve the purity of the product.
[0028] An extraction and purification method of an extraction and purification device, the purification process is as follows:
[0029] S1. The mixed product outputted from the BDO reactor is passed into a light-removal tower for heating and evaporation. The evaporated gas phase is distilled and purified through the reflux pipe. It is not necessary to follow the purification process of the complex structure of the light-removal tower in the prior art. Only the gas phase needs to be evaporated, which reduces the difficulty of multi-stage temperature control in a small space in the prior art and can also improve the purity of the product.
[0030] S2, the gas phase is heat exchanged and condensed with the feed of the BDO reactor through the heat exchange wings on the side of the reflux pipe, and the condensed liquid enters the hydrogenation reaction tank through the condensation conduit, effectively utilizing the gas phase to cool down and condense, and using the heat energy of this part to preheat the reactants, thereby reducing energy loss;
[0031] S3, the condensed liquid is subjected to hydrogenation reaction in the hydrogenation reaction tank, and the THF component is purified by aeration and the action of the catalyst plate, the hydrogen is aerated and the catalyst plate arranged in an inverted cone is combined to increase the contact area of the reactants, the purified liquid is passed into the distillation tube for repeated distillation, and the product is purified multiple times in the distillation tube, and the product is exported to the THF dehydration tower after reaching the purity standard, so as to complete the purification of the tetrahydrofuran component.
[0032] The present invention discloses an extraction and purification device and an extraction and purification method, which have the following beneficial effects:
[0033] 1. The extraction and purification equipment and the extraction and purification method are different from the prior art purification method in which the tetrahydrofuran component is purified through multi-stage temperature control changes in the light removal tower. Only the gas phase is evaporated in the light removal tower, and the evaporated gas phase is circulated and discharged through a reflux pipe. The heat energy of the discharged gas phase is used to preheat the reactants, and the gas phase is cooled and condensed at the same time. The condensate is collected and hydrogenated, and then multiple evaporation and purification are performed. After multiple purifications to improve the purity of the product, it is introduced into the THF dehydration tower, which reduces the difficulty of multiple temperature controls in the light removal tower, is conducive to improving the purity of the product, and the purity of the output product can be artificially controlled by the equipment, which is more convenient to use.
[0034] 2. The extraction and purification equipment and extraction and purification method utilize a reflux pipe to discharge the gas phase in the light removal tower, exchange heat with the reactants through heat exchange wings, use the thermal energy of the gas phase to preheat the reactants, and simultaneously condense and liquefy the gas phase, thereby realizing effective utilization of the system's thermal energy. The heat exchange process can be precisely controlled by controlling the reactant input rate and the gas phase flow rate, thereby realizing purification and extraction of some products in the mixture.
[0035] 3. The extraction and purification equipment and the extraction and purification method, hydrogen is input into the hydrogenation reaction tank by aeration, and an inverted cone-shaped catalyst plate is provided to increase the contact area between the reactants, and guide grooves and honeycomb holes are further provided to increase the reaction effect and accelerate the progress of the hydrogenation reaction, and then the tetrahydrofuran component is purified by precise temperature control through a thin film evaporator, and the gas phase is collected and enters the distillation tube for multiple purifications to improve the purity, and the purity of the product is controlled by controlling the number of purifications. BRIEF DESCRIPTION OF THE DRAWINGS
[0036] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.
[0037] Figure 1 It is a schematic diagram of the overall structure of the present invention;
[0038] Figure 2 This is a schematic diagram of the installation structure of the side reflux pipe of the lightness removal tower of the present invention;
[0039] Figure 3 For the present invention Figure 2 A magnified schematic diagram of the condensation duct structure at center A;
[0040] Figure 4 It is a cross-sectional view of the structure of the hydrogenation reaction tank of the present invention;
[0041] Figure 5 This is a schematic diagram of the catalyst plate structure and installation of the present invention;
[0042] Figure 6 This is a schematic diagram of the distillation tube structure of the present invention;
[0043] Figure 7 For the present invention Figure 6 Enlarged schematic diagram of the structure at point B in the middle.
[0044] In the figure: 1. BDO reactor; 2. light removal tower; 3. THF dehydration tower; 4. reflux pipe; 5. heat exchange wings; 6. condensation duct; 601. water storage section; 602. outlet section; 7. hydrogenation reaction tank; 8. catalyst plate; 9. distillation pipe; 10. inclined pipe section; 11. arc-shaped block; 12. pressure valve; 13. main pipe; 14. support rod; 15. power pump; 16. control valve; 17. aeration nozzle; 18. guide groove; 19. honeycomb hole; 20. wedge block; 21. thin film evaporator; 22. gas phase cavity; 23. gas phase collecting pipe; 24. distillation tank. DETAILED DESCRIPTION
[0045] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described. Obviously, the described embodiments are 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 creative work are within the scope of protection of the present invention.
[0046] The embodiment of the present invention discloses an extraction and purification device and an extraction and purification method;
[0047] According to the attached Figure 1 As shown, it includes a BDO reactor 1, a light removal tower 2 connected to the BDO reactor 1, and a THF dehydration tower 3 connected to the light removal tower 2. The BDO reactor 1 and the light removal tower 2 include a complete set of feeding and discharging and thermal evaporation systems.
[0048] In the production of the prior art, raw materials are introduced into the BDO reactor 1 to react and generate a mixture, the mixture is introduced into the lightness removal tower 2 to evaporate the gas phase for purification, and the purified gas phase is introduced into the THF dehydration tower 3 for further distillation to obtain a tetrahydrofuran product with higher purity.
[0049] However, the light removal tower 2 and THF dehydration tower 3 of the prior art have many distillation steps, and the temperature range needs to be precisely controlled between each step to ensure the purity of the product. One factor that the prior art cannot improve the purity of the product is the complexity of multi-stage temperature control in a limited space, and the purification process is complicated, making it difficult to further improve the purity of the product. Therefore, technicians in this field improve the existing equipment, simplify the product purification process, and further precisely control the product purity.
[0050] According to the attached Figure 2 As shown, a reflux pipe 4 is fixed on the side of the BDO light-removal tower 2, and both ends of the reflux pipe 4 are respectively connected to the top and bottom ends of the BDO light-removal tower 2. The evaporating gas phase in the BDO light-removal tower 2 realizes internal and external heat exchange circulation through the reflux pipe 4.
[0051] A heat exchange wing 5 is fixedly connected to the side of the reflux pipe 4. The gas phase in the reflux pipe 4 is heat exchanged and condensed with the feed room of the BDO reactor 1 through the heat exchange wing 5, wherein the effective components form condensate, and the remaining gas phase enters the light removal tower 2 again through the reflux pipe 4 for circulation.
[0052] A condensation conduit 6 is fixed obliquely on the side of the reflux pipe 4, and one end of the condensation conduit 6 away from the reflux pipe 4 is connected to a hydrogenation reaction tank 7. The condensate is separated from the remaining gas phase through the condensation conduit 6 and discharged into the hydrogenation reaction tank 7, where a hydrogenation reaction is carried out to purify the tetrahydrofuran component.
[0053] According to the attached Figure 3 and attached Figure 4 As shown, a catalyst plate 8 is provided inside the hydrogenation reaction tank 7. Hydrogen is introduced into the hydrogenation reaction tank 7, and the hydrogen forms bubbles and moves along the surface of the catalyst plate 8. In the presence of the catalyst, furan reacts with the hydrogen, the double bonds are opened, and each carbon atom is combined with a hydrogen atom to generate tetrahydrofuran.
[0054] A distillation pipe 9 is fixedly connected to the side of the hydrogenation reaction tank 7. The liquid after the hydrogenation reaction is passed into the distillation pipe 9 for heating to evaporate the tetrahydrofuran component in the liquid. The end of the distillation pipe 9 away from the hydrogenation reaction tank 7 is connected to the reflux pipe 4, and the remaining liquid is passed into the reflux pipe 4 and returned to the light removal tower 2 to obtain purified tetrahydrofuran.
[0055] The middle section of the reflux pipe 4 is connected to an inclined pipe section 10 , and the condensation conduit 6 is connected to the side of the bottom end of the inclined pipe section 10 . The condensation liquid is collected through the inclined pipe section 10 , ensuring that the condensation conduit 6 collects the condensation liquid.
[0056] An arc-shaped stopper 11 is fixedly connected to the inner side of the inclined pipe section 10 corresponding to the condensation conduit 6 , and the arc-shaped stopper 11 ensures that the condensate enters the condensation conduit 6 .
[0057] The condensation conduit 6 includes a water storage section 601, which is vertically fixed to the reflux pipe 4. The condensate in the reflux pipe 4 enters the water storage section 601. Only liquid with a certain depth can pass through the water storage section 601 and enter the hydrogenation reaction tank 7 to avoid impurities in the mixed gas phase entering and affecting the purity.
[0058] The end of the water storage section 601 away from the reflux pipe 4 is connected to the outlet section 602, and a pressure valve 12 is also provided at the connection between the outlet section 602 and the water storage section 601. When the liquid depth in the water storage section 601 reaches a certain level, the condensate can enter the outlet section 602 through the pressure valve 12 for discharge, thereby preventing the gas pressure of the gas phase transport in the reflux pipe 4 from causing the mixed gas phase to enter the hydrogenation reaction tank 7.
[0059] According to the attached Figure 4 As shown, a main pipe 13 is fixedly connected to the side of the hydrogenation reaction tank 7, and the main pipe 13 is sleeved outside the light removal tower 2. One end of the condensation pipe 6 away from the reflux pipe 4 is fixedly connected to the main pipe 13. All condensation pipes 6 are connected through the main pipe 13 to improve the purification efficiency of the light removal tower 2.
[0060] A support rod 14 is fixed to the side of the de-lightening tower 2 corresponding to the main pipe 13. The main pipe 13 is fixed outside the de-lightening tower 2 through multiple support rods 14 to ensure the collection of condensed liquid in multiple groups of reflux pipes 4 arranged in a ring outside the de-lightening tower 2.
[0061] According to the attached Figure 5 As shown, the feed pipe of the BDO reactor 1 extends to the outside of the reflux pipe 4 and is parallel to the reflux pipe in the opposite direction. The heat exchange wings 5 are fixedly connected between the feed pipe of the BDO reactor 1 and the reflux pipe 4. The gas phase in the reflux pipe 4 exchanges heat with the raw material of the BDO reactor 1 through the heat exchange wings 5, effectively utilizing the heat energy of the gas phase to preheat the raw material, and also cooling and condensing the gas phase.
[0062] The feed pipe of the light removal tower 2 extends to one side of the distillation pipe 9 and is parallel to the opposite direction. A power pump 15 and a control valve 16 are provided on the side of each pipeline. The liquid in the distillation pipe 9 is heated by the output material in the BDO reactor 1, and the effective gas phase therein is evaporated for further purification.
[0063] An aeration nozzle 17 is fixed to the inner bottom of the hydrogenation reaction tank 7 corresponding to the catalyst plate 8. The aeration nozzle 17 forms relatively uniform hydrogen bubbles in the condensed liquid. The bubbles rotate and rise in the condensed liquid, and contact the catalyst plate 8 during the rising process to perform a catalytic reaction.
[0064] The catalyst plate 8 is coaxially fixed to the inner wall of the hydrogenation reaction tank 7 in an inverted cone shape. The inverted cone-shaped catalyst plate 8 can increase the contact area of the reactants and ensure the movement and reaction of hydrogen along the catalyst plate 8 .
[0065] A guide groove 18 is provided on the side of the catalyst plate 8 . After the hydrogen bubbles contact the catalyst plate 8 , they move along the guide groove 18 on the surface of the catalyst plate 8 , thereby increasing the contact area between the hydrogen bubbles and the catalyst plate 8 .
[0066] According to the attached Figure 6 and attached Figure 7As shown, a honeycomb hole 19 is penetrated through the side of the catalyst plate 8, and a wedge block 20 is fixedly connected to the inner side of the guide groove 18 corresponding to the honeycomb hole 19. When the hydrogen bubbles flow along the guide groove 18, they can also directly float up through the honeycomb hole 19, further increasing the contact area between the reactants. The wedge block 20 has a certain interception effect on the bubbles, allowing the bubbles to float up through the honeycomb hole 19.
[0067] A thin film evaporator 21 is fixed to the inner wall of the distillation tube 9, and tetrahydrofuran in the condensed liquid is quickly evaporated into a gas phase through heat exchange, thereby achieving the purpose of purification. A gas phase cavity 22 is provided on the upper side wall of the distillation tube 9, and the evaporated gas phase floats up into the gas phase cavity 22 on the upper side of the distillation tube 9.
[0068] The top of the gas phase chamber 22 is connected to a gas phase collecting pipe 23, through which tetrahydrofuran gas is collected. The other end of the gas phase collecting pipe 23 is connected to a distillation tank 24, and the purified tetrahydrofuran gas is passed into the distillation tank 24, which is convenient for multiple purifications to improve the purity of the product.
[0069] An extraction and purification method of an extraction and purification device, the purification process is as follows:
[0070] S1. The mixed product outputted from the BDO reactor 1 is passed into the light removal tower 2 for heating and evaporation. The evaporated gas phase is distilled and purified through the reflux pipe 4. It is not necessary to follow the purification process of the complex structure of the light removal tower 2 in the prior art. Only the gas phase needs to be evaporated, which reduces the difficulty of multi-stage temperature control in a small space in the prior art and can also improve the purity of the product.
[0071] S2, the gas phase is heat exchanged and condensed with the feed of the BDO reactor 1 through the heat exchange wings 5 on the side of the reflux pipe 4, and the condensed liquid enters the hydrogenation reaction tank 7 through the condensation conduit 6, effectively utilizing the gas phase to cool down and condense, and using the heat energy of this part to preheat the reactants, thereby reducing energy loss;
[0072] S3, the condensed liquid is subjected to hydrogenation reaction in the hydrogenation reaction tank 7, the hydrogen introduced is aerated through the aeration nozzle 17, and the THF component is purified by the catalyst plate 8, the hydrogen is aerated and the catalyst plate 8 with an inverted cone shape is used to increase the contact area of the reactants, the purified liquid is introduced into the distillation pipe 9 for repeated distillation, and the product is purified multiple times in the distillation pipe 9, and the product is exported to the THF dehydration tower 3 after reaching the purity standard, so as to complete the purification of the tetrahydrofuran component.
[0073] The extraction and purification equipment and the extraction and purification method are different from the prior art purification method in which the tetrahydrofuran component is purified through multi-stage temperature control changes in the light removal tower 2. Only the gas phase is evaporated in the light removal tower 2, and the evaporated gas phase is circulated and discharged through the reflux pipe 4. The heat energy of the discharged gas phase is used to preheat the reactants, and the gas phase is cooled and condensed at the same time. The condensate is collected and hydrogenated, and then multiple evaporation and purification are performed. After the multiple purifications improve the purity of the product, it is introduced into the THF dehydration tower 3, which reduces the difficulty of multiple temperature controls in the light removal tower 2, is conducive to improving the purity of the product, and the device can artificially control the purity of the output product, which is more convenient to use.
[0074] Furthermore, the gas phase in the light-removal tower 2 is discharged by means of the reflux pipe 4, and heat is exchanged with the reactants through the heat exchange wings 5. The reactants are preheated by means of the thermal energy of the gas phase, and the gas phase is condensed and liquefied at the same time, thereby realizing effective utilization of the thermal energy of the system. The heat exchange process can be precisely controlled by controlling the input speed of the reactants and the gas phase flow rate, thereby realizing purification and extraction of some products in the mixture.
[0075] Furthermore, hydrogen is introduced into the hydrogenation reaction tank 7 by aeration, and an inverted cone-shaped catalyst plate 8 is provided to increase the contact area between the reactants, and a guide groove 18 and a honeycomb hole 19 are further provided to increase the reaction speed and accelerate the progress of the hydrogenation reaction. The tetrahydrofuran component is then purified by precise temperature control through a thin film evaporator 21, and the gas phase is collected and enters the distillation tube 9 for multiple purifications to improve the purity, and the purity of the product is controlled by controlling the number of purifications.
[0076] The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention. It should be understood by those skilled in the art that the present invention is not limited to the above embodiments. The above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention to be protected. The scope of protection of the present invention is defined by the attached claims and their equivalents.
Claims
1. An extraction and purification device, comprising a BDO reactor (1), a lightness removal column (2) connected to the BDO reactor (1), and a THF dehydration column (3) connected to the lightness removal column (2), wherein the BDO reactor (1) and the lightness removal column (2) comprise a complete set of feeding and discharging and thermal evaporation systems, characterized in that: A reflux pipe (4) is fixed on the side of the light-removal tower (2), two ends of the reflux pipe (4) are respectively connected to the top and bottom ends of the BDO light-removal tower (2), a heat exchange wing (5) is fixedly connected to the side of the reflux pipe (4), a condensation pipe (6) is obliquely fixed on the side of the reflux pipe (4), and one end of the condensation pipe (6) away from the reflux pipe (4) is connected to a hydrogenation reaction tank (7); A catalyst plate (8) is arranged inside the hydrogenation reaction tank (7), a distillation pipe (9) is fixedly connected to the side of the hydrogenation reaction tank (7), and one end of the distillation pipe (9) away from the hydrogenation reaction tank (7) is connected to the reflux pipe (4).
2. The extraction and purification equipment according to claim 1, characterized in that: The middle section of the return pipe (4) is connected to an inclined pipe section (10), the condensation duct (6) is connected to the inner side of the bottom end of the inclined pipe section (10), and the inner side of the inclined pipe section (10) is fixedly connected to an arc-shaped stopper (11) corresponding to the condensation duct (6).
3. The extraction and purification equipment according to claim 2, characterized in that: The condensation conduit (6) comprises a water storage section (601), the water storage section (601) is vertically fixed to the return pipe (4), one end of the water storage section (601) away from the return pipe (4) is connected to a discharge section (602), and a pressure valve (12) is also provided at the connection between the discharge section (602) and the water storage section (601).
4. The extraction and purification equipment according to claim 1, characterized in that: A main pipe (13) is fixedly connected to the side of the hydrogenation reaction tank (7), and the main pipe (13) is sleeved and arranged outside the light removal tower (2). One end of the condensation conduit (6) away from the reflux pipe (4) is fixedly connected to the main pipe (13), and a support rod (14) is fixed to the side of the light removal tower (2) corresponding to the main pipe (13).
5. The extraction and purification equipment according to claim 1, characterized in that: The feed pipe of the BDO reactor (1) extends to the outside of the reflux pipe (4) and is parallel to the opposite direction thereof; the heat exchange wing (5) is fixedly connected between the feed pipe of the BDO reactor (1) and the reflux pipe (4); the feed pipe of the light removal tower (2) extends to one side of the distillation pipe (9) and is parallel to the opposite direction thereof; and a power pump (15) and a control valve (16) are arranged on the side of each pipeline.
6. The extraction and purification equipment according to claim 1, characterized in that: An aeration nozzle (17) is fixed to the inner bottom of the hydrogenation reaction tank (7) corresponding to the catalyst plate (8); the catalyst plate (8) is coaxially fixed to the inner wall of the hydrogenation reaction tank (7) in an inverted cone shape; and a guide groove (18) is provided on the side of the catalyst plate (8).
7. The extraction and purification equipment according to claim 6, characterized in that: A honeycomb hole (19) is formed through the side surface of the catalyst plate (8), and a wedge-shaped block (20) is fixedly connected to the inner side of the guide groove (18) corresponding to the honeycomb hole (19).
8. The extraction and purification equipment according to claim 1, characterized in that: A thin film evaporator (21) is fixed to the inner wall of the rectification tube (9), and a gas phase cavity (22) is provided on the upper side wall of the rectification tube (9).
9. The extraction and purification equipment according to claim 8, characterized in that: The top of the gas phase cavity (22) is connected to a gas phase collecting pipe (23), and the other end of the gas phase collecting pipe (23) is connected to a distillation tank (24).
10. The extraction and purification method based on the extraction and purification equipment according to any one of claims 1 to 9, characterized in that: The purification process is as follows: S1, the mixture output from the BDO reactor (1) is passed into a light removal tower (2) for heating and evaporation, and the evaporated gas phase is distilled and purified through the reflux pipe (4); S2, the gas phase is heat exchanged and condensed with the feed of the BDO reactor (1) through the heat exchange wings (5) on the side of the reflux pipe (4), and the condensed liquid enters the hydrogenation reaction tank (7) through the condensation conduit (6); S3, the condensed liquid is subjected to a hydrogenation reaction in the hydrogenation reaction tank (7), and the THF component is purified by aeration and the action of the catalyst plate (8). The purified liquid is passed into the distillation pipe (9) for repeated distillation, and is led out to the THF dehydration tower (3) after reaching the purity standard, thereby completing the purification of the tetrahydrofuran component.
Citation Information
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