Potassium tert-butoxide refining equipment

Abstract

The invention relates to the technical field of potassium tert-butoxide preparation, in particular to potassium tert-butoxide refining equipment which comprises a rectifying tower, a reboiler, a cooler and a phase splitter, the crystallization tower is located on the outer side of the rectifying tower, a rectifying chamber of the rectifying tower is connected with a crystallization chamber of the crystallization tower through the pre-filtering assembly, and the heater is installed at the bottom of the crystallization chamber of the crystallization tower; the input end of the low-pressure exhaust pipe is connected with the top of a crystallization chamber of the crystallization tower, the output end of the low-pressure exhaust pipe is connected with the input end of the cooler, the discharging pipe is installed on the side wall of the upper portion of the crystallization tower and communicated with the crystallization chamber of the crystallization tower, and the flashboard is inserted into the discharging pipe in a lifting mode. And the filter plate hopper is mounted in a crystallization chamber of the crystallization tower in a lifting and sliding manner. The azeotropic distillation kettle liquid can be subjected to efficient evaporation drying, redispersion, cooling crystallization and other processes after azeotropic distillation, potassium tert-butoxide can be efficiently discharged, and the practicability is good.

Description

Technical Field

[0001] The invention relates to the technical field of potassium tert-butoxide preparation, in particular to potassium tert-butoxide refining equipment. Background Art

[0002] Potassium tert-butoxide is an important organic base, and its alkalinity is greater than sodium hydroxide and potassium hydroxide. A variety of preparation methods of potassium tert-butoxide are proposed in the prior art, such as a process for preparing potassium tert-butoxide based on solid potassium hydroxide proposed by the Chinese invention patent of publication number CN118084615A, in which solid potassium hydroxide is placed in a low-temperature chamber filled with liquid nitrogen for grinding by cryogenic grinding, and ground to more than 100 meshes to obtain ultrafine potassium hydroxide powder, and then ultrafine potassium hydroxide powder is mixed with tert-butyl alcohol in a static mixer, and the amount and flow rate of the carrying agent are controlled, and the feeding is slowly fed when the tower top temperature reaches 65-75°C, and after reaching a certain liquid level, the feeding is stopped, and the whole reflux is performed until the moisture content is ≤0.35wt%, and the free alkali content is ≤0.5wt%, and the kettle liquid containing potassium tert-butoxide is obtained; then the kettle liquid is left to settle, and after reduced pressure evaporation, the evaporated solid obtained is dispersed in tetrahydrofuran, and high-purity potassium tert-butoxide is obtained after filtration and cooling crystallization.

[0003] The above-mentioned potassium tert-butoxide preparation process describes the preparation equipment of the azeotropic distillation stage of potassium tert-butoxide, but does not describe what kind of preparation equipment is used to evaporate, redisperse and cool and crystallize the kettle liquid after the azeotropic distillation. Therefore, on the basis of the existing technology, it is urgent to propose a potassium tert-butoxide refining equipment that adopts azeotropic distillation and efficient cooling and crystallization recovery. Summary of the invention

[0004] In order to solve the above technical problems, the present invention provides a potassium tert-butoxide refining device which can efficiently evaporate, redisperse and cool and crystallize the kettle liquid after azeotropic distillation, and discharge potassium tert-butoxide efficiently and has good practicality.

[0005] The invention discloses a potassium tert-butoxide refining device, comprising a distillation tower, a reboiler, a cooler and a phase separator; a distillation chamber is arranged inside the distillation tower, a feeding pipe communicating with the distillation chamber is arranged at the top of the distillation tower, and a plurality of trays are arranged in the distillation chamber; the reboiler is installed at the bottom of the distillation tower, the input end of the cooler is connected to the top of the distillation chamber of the distillation tower; the input end of the phase separator is connected to the output end of the cooler, a drain pipe is arranged at the bottom of the phase separator, a reflux pipe is arranged in the middle of the phase separator, and the output end of the reflux pipe extends into the top of the distillation chamber; and a crystallization tower is also provided. , heater, low-pressure exhaust pipe, discharge pipe, gate, filter plate bucket and pre-filtration assembly, the crystallization tower is located on the outside of the distillation tower, a crystallization chamber is arranged inside the crystallization tower, the distillation chamber of the distillation tower and the crystallization chamber of the crystallization tower are connected through the pre-filtration assembly, the heater is installed at the bottom of the crystallization chamber, the input end of the low-pressure exhaust pipe is connected to the top of the crystallization chamber of the crystallization tower, the output end of the low-pressure exhaust pipe is connected to the input end of the cooler, the discharge pipe is installed on the upper side wall of the crystallization tower, the discharge pipe is connected to the crystallization chamber of the crystallization tower, the gate is liftably inserted on the discharge pipe, and the filter plate bucket is liftably slidably installed in the crystallization chamber.

[0006] During operation, ultrafine potassium hydroxide powder and tert-butyl alcohol are added to the top of the distillation tower through a feeding pipe, and a carrier is continuously added to the distillation chamber of the distillation tower, so that the reaction solution of the carrier mixed with ultrafine potassium hydroxide powder and tert-butyl alcohol flows from top to bottom along the multi-layer tower plates, and the reboiler is turned on to heat the reaction liquid at the bottom of the distillation chamber of the distillation tower, so that the water produced by the reaction and the carrier boil together to generate mixed steam, and the mixed steam passes through the multi-layer tower plates from bottom to top in sequence, so that the mixed steam and the reaction solution are fully in contact between the multi-layer tower plates, promoting Ultrafine potassium hydroxide powder reacts with tert-butyl alcohol to generate potassium tert-butyl alcohol and water. After the mixed steam reaches the top of the distillation chamber of the distillation tower, it enters the cooler to cool and liquefy into a mixed liquid. The mixed liquid enters the phase separator and is layered. The water in the bottom layer is discharged from the phase separator. The carrier and tert-butyl alcohol in the upper oil phase are refluxed to the top of the distillation chamber of the distillation tower through the reflux pipe. When the water content in the reaction liquid is reduced to the set value, the kettle liquid in the distillation chamber of the distillation tower is input into the crystallization chamber of the crystallization tower through the pre-filter component. The pre-filter component performs primary filtration on the kettle liquid. Filtration, the kettle liquid is allowed to settle in the crystallization chamber of the crystallization tower, the filter plate bucket is raised from the bottom of the crystallization chamber of the crystallization tower to be aligned with the discharge pipe, the sediment and impurities in the kettle liquid are filtered, the gate is raised to open the discharge pipe, the sediment and impurities in the filter plate bucket are cleaned out through the discharge pipe, the gate closes the discharge pipe, the filter plate bucket descends back to the bottom of the crystallization chamber of the crystallization tower, the heater is turned on to evaporate the kettle liquid, the carrier and tert-butyl alcohol and n-butyl alcohol in the kettle liquid are evaporated into mixed steam 2, and the mixed steam 2 is input into the cooler and phase separator through the low-pressure exhaust pipe After cooling and stratification, the products are discharged for recovery respectively. After the kettle liquid is evaporated to dryness, tetrahydrofuran is added into the crystallization chamber of the crystallization tower for dispersion. The filter plate bucket is raised to filter the dispersion liquid again and then lowered to reset. The dispersion liquid is cooled to make potassium tert-butoxide crystals precipitate. The filter plate bucket is raised to fish out the potassium tert-butoxide crystals and align them with the discharge pipe. The gate is opened and the potassium tert-butoxide crystals in the filter plate bucket are discharged through the discharge pipe. Thus, the kettle liquid after azeotropic distillation is efficiently evaporated to dryness, redispersed and cooled for crystallization, and potassium tert-butoxide can be efficiently discharged, which has good practicality.

[0007] Preferably, the tower plate includes a sieve plate and a vertical plate, the sieve plate is installed at an angle in the distillation chamber of the distillation tower, a gap for the reaction liquid to pass through is provided between the high end of the sieve plate and the interior of the distillation tower, and the vertical plate is installed on the lower end surface of the high end of the sieve plate; the space between the sieve plate and the vertical plate gathers the mixed steam rising from the bottom of the distillation chamber of the distillation tower, and disperses the mixed steam to the top through the filter holes of the sieve plate, so that the mixed steam is fully mixed with the reaction liquid flowing on the sieve plate, and at the same time, the vertical plate and the inner wall of the distillation tower guide the reaction liquid flowing downward, and since the multiple sieve plates and the multiple vertical plates are arranged in a staggered and inclined manner in sequence, the upward inclined sieve plate slows down the flow speed of the reaction liquid and increases the contact time between the mixed steam and the reaction liquid, thereby improving the reaction efficiency.

[0008] Preferably, the interior of the distillation tower also includes multiple packing layers, and the lower end surfaces of multiple sieve plates are all installed with packing layers; by installing multiple packing layers, the mixed steam gathered between the sieve plates and the vertical plates is dispersed, so that the mixed steam passes through the filter holes of the sieve plates more evenly, which has good practicality.

[0009] Preferably, it also includes a receiving hopper, which is installed at the top of the distillation chamber of the distillation tower and is located below the feeding pipe of the distillation tower; the receiving hopper is used to carry the ultrafine potassium hydroxide powder added through the feeding pipe, reduce the flow of the ultrafine potassium hydroxide powder with the reaction liquid, thereby reducing the blockage of the filter holes of multiple sieve plates and the pipeline of the reboiler by the powdered sodium hydroxide, and improving reliability.

[0010] Preferably, it also includes a water jacket, a liquid replenishment pipe and a liquid return pipe, the water jacket is arranged on the top outer wall of the distillation tower, the output end of the phase separator is connected to the input end of the water jacket, the liquid replenishment pipe is installed on the water jacket, the liquid replenishment pipe is communicated with the inside of the water jacket, the output end of the water jacket is installed with the liquid return pipe, and the output end of the liquid return pipe extends into the top of the distillation chamber of the distillation tower; the carrier and tert-butyl alcohol etc. that flow back to the oil phase through the phase separator flow back to the water jacket through the reflux pipe, and the carrier is continuously transported to the water jacket through the liquid replenishment pipe, and the waste heat at the top of the distillation tower preheats the mixed liquid therein through the water jacket, and the preheated mixed liquid flows back to the distillation chamber of the distillation tower through the liquid return pipe, thereby reducing the influence of the mixed liquid on the temperature at the top of the distillation chamber of the distillation tower.

[0011] Preferably, it also includes a pressurized pipe, which is installed on the top of the distillation tower and is connected to the distillation chamber of the distillation tower; high-pressure air is input into the distillation chamber of the distillation tower through the pressurized pipe, and the high-pressure air presses the kettle liquid out of the distillation chamber of the distillation tower and inputs it into the crystallization chamber of the crystallization tower, thereby improving the liquid discharge efficiency.

[0012] Preferably, it also includes a screw, a bevel gear 1, a drive shaft, a bevel gear 2 and a motor 1. The screw is vertically rotatably installed in the middle of the crystallization chamber of the crystallization tower. The screw is transmission-connected to the filter plate bucket through a screw nut. The upper end of the screw is concentrically installed with a bevel gear 1, and the drive shaft is rotatably installed on the top of the crystallization chamber of the crystallization tower. The drive shaft is concentrically installed with a bevel gear 2, and the bevel gear 2 is meshed with the drive shaft. The motor 1 is installed on the crystallization tower, and the output shaft of the motor 1 is transmission-connected to the drive shaft; the motor 1 drives the drive shaft to rotate, and the drive shaft drives the bevel gear 2 to rotate, and the bevel gear 2 meshes with the bevel gear 1 to drive the screw to rotate. The screw drives the filter plate bucket to rise and fall in the crystallization chamber of the crystallization tower through the screw nut, and the driving effect is stable and reliable.

[0013] Preferably, it also includes a baffle and a spring, and an opening matching the discharge pipe is provided on the side wall of the filter plate bucket facing the discharge pipe, the inner end of the discharge pipe protrudes from the inner wall of the crystallization tower, the baffle is slidably inserted in the opening of the filter plate bucket, the upper end of the spring is connected to the filter plate bucket, and the lower end of the spring is connected to the baffle; when the filter plate bucket is raised to be aligned with the discharge pipe, the inner end of the discharge pipe blocks the baffle, thereby opening the opening of the filter plate bucket, making it convenient to discharge impurities or potassium tert-butoxide crystals in the filter plate bucket through the discharge pipe, and when the filter plate bucket is lowered, the elastic force of the spring pushes the baffle up and resets it, thereby closing the opening of the filter plate bucket, which has good practicality.

[0014] Preferably, it also includes a scraper, a slider, a hook rod, a second motor, a shaft rod and a lever, the scraper is slidably installed on the inner wall of the filter plate bucket, the slider is elastically lifted and slidably installed on the inner wall of the scraper, the slider is installed with the hook rod, the second motor is installed on the top outer wall of the crystallization tower, the shaft rod is rotatably installed on the top of the crystallization chamber of the crystallization tower, the shaft rod is transmission-connected to the output end of the second motor, one end of the lever is connected to the shaft rod, and a hook is provided on the other end of the lever, and the hook matches the hook rod; when the filter plate bucket is raised to be aligned with the discharge pipe, the second motor drives the shaft rod and the lever to rotate, so that the hook of the lever hooks the hook rod, and the lever rotates continuously, thereby pulling the scraper toward the opening of the filter plate bucket through the slider, thereby utilizing the scraper to push the impurities or potassium tert-butoxide crystals in the filter plate bucket through the opening into the discharge pipe for discharge, thereby improving the discharge efficiency.

[0015] Preferably, the pre-filter assembly includes a base, a filter cartridge, a top cover, a sealing wedge ring 1, a connecting pipe, a sealing wedge ring 2, a filter, a rotating shaft, an impeller and a propeller. The base is connected to the crystallization chamber of the crystallization tower through a flange tube, the left end of the filter cartridge is screwed and fastened to the base, the top cover is screwed and fastened to the right end of the filter cartridge, a through hole 1 is provided in the middle of the right end of the top cover, a sealing wedge ring 1 is provided on the inner side wall of the through hole, the right end of the connecting pipe is connected to the distillation chamber of the distillation tower through the flange tube, the left end of the connecting pipe extends into the through hole of the top cover, a sealing wedge ring 2 is provided on the left end of the connecting pipe, the sealing wedge ring 2 is squeezed and sealed with the sealing wedge ring 1, the filter is installed inside the filter cartridge, the inlet of the filter faces the connecting pipe, the middle part of the rotating shaft is rotatably connected to the bottom of the filter, and one end of the rotating shaft is provided with An impeller is installed, the impeller is located in the filter, and a propeller is installed at the other end of the rotating shaft, and the propeller is located at the flange pipe inlet of the base; when the base is connected to the crystallization tower and the connecting pipe is connected to the distillation tower, the sealing wedge ring 2 and the sealing wedge ring 1 are squeezed and sealed, and the kettle liquid in the distillation tower is input into the filter barrel through the connecting pipe, and the filter performs preliminary filtration on the kettle liquid, so that the filtered kettle liquid is input into the crystallization chamber of the crystallization tower through the flange pipe of the base, and the kettle liquid flowing through the flange pipe of the base and the propeller drive the rotating shaft to rotate, and the rotating shaft drives the impeller to rotate, and the impeller stirs the kettle liquid in the filter, so that the kettle liquid accelerates to collide with the filter, thereby improving the filtering efficiency of the filter, and the filter barrel is connected to the base and the top cover by screw connection, which is convenient for disassembling the filter barrel and cleaning the filter inside the filter barrel.

[0016] Compared with the prior art, the invention has the following beneficial effects: when working, ultrafine potassium hydroxide powder and tert-butyl alcohol are added to the top of the distillation tower through a feeding pipe, and a carrying agent is continuously added to the distillation chamber of the distillation tower, so that a reaction solution of the carrying agent mixed with the ultrafine potassium hydroxide powder and the tert-butyl alcohol flows from top to bottom along the multi-layer tower plates, and a reboiler is opened to heat the reaction liquid at the bottom of the distillation chamber of the distillation tower, so that the water generated by the reaction and the carrying agent boil together to generate mixed steam, and the mixed steam passes through the multi-layer tower plates in sequence from bottom to top, so that the mixed steam and the reaction solution are heated at the bottom of the distillation chamber of the distillation tower. The multiple layers of tower plates are in full contact with each other, promoting the reaction of ultrafine potassium hydroxide powder with tert-butanol to generate potassium tert-butoxide and water. After the mixed steam reaches the top of the distillation chamber of the distillation tower, it enters the cooler for cooling and liquefaction into a mixed liquid. The mixed liquid enters the phase separator and is layered. The water in the bottom layer is discharged from the phase separator, and the carrier and tert-butanol of the upper oil phase are refluxed to the top of the distillation chamber of the distillation tower through the reflux pipe. When the water content in the reaction liquid is reduced to the set value, the kettle liquid in the distillation chamber of the distillation tower is input into the crystallization chamber of the crystallization tower through the pre-filtration component. The pre-filtration The components perform primary filtration on the kettle liquid, and the kettle liquid is allowed to settle in the crystallization chamber of the crystallization tower. The filter plate bucket is raised from the bottom of the crystallization chamber of the crystallization tower to be aligned with the discharge pipe to filter the sediment and impurities in the kettle liquid. The gate is raised to open the discharge pipe, and the sediment and impurities in the filter plate bucket are cleaned out through the discharge pipe. The gate closes the discharge pipe, and the filter plate bucket descends back to the bottom of the crystallization chamber of the crystallization tower. The heater is turned on to evaporate the kettle liquid, and the carrier, tert-butyl alcohol and n-butyl alcohol in the kettle liquid are evaporated into mixed steam 2, and the mixed steam 2 is input to the cooling After cooling and stratification in the reactor and phase separator, the products are discharged for recovery respectively. After the kettle liquid is evaporated to dryness, tetrahydrofuran is added into the crystallization chamber of the crystallization tower for dispersion. The filter plate bucket is raised to filter the dispersion liquid again and then lowered to reset. The dispersion liquid is cooled to make potassium tert-butoxide crystals precipitate. The filter plate bucket is raised to fish out the potassium tert-butoxide crystals and align them with the discharge pipe. The gate is opened and the potassium tert-butoxide crystals in the filter plate bucket are discharged through the discharge pipe. Thus, the kettle liquid after azeotropic distillation is efficiently evaporated to dryness, redispersed and cooled for crystallization, and potassium tert-butoxide can be efficiently discharged, which has good practicality. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a schematic diagram of the structure of the present invention; Figure 2 It is a schematic diagram of the axonometric partial cross-sectional structure of the present invention; Figure 3 It is a front cross-sectional structural schematic diagram of the present invention; Figure 4 It is a schematic diagram of the structure of the distillation tower, reboiler, cooler and phase separator; Figure 5 It is a schematic diagram of the structure of the cooler, phase separator, low-pressure exhaust pipe and water jacket; Figure 6 It is a schematic diagram of the structure of the crystallization tower, heater, low-pressure exhaust pipe, discharge pipe, gate plate and filter plate bucket; Figure 7 It is a structural schematic diagram of filter plate bucket, screw, bevel gear 1, drive shaft, bevel gear 2, motor 1 and baffle; Figure 8 It is a schematic diagram of the structure of filter plate bucket, scraper, slider, hook rod, motor 2, shaft rod and lever; Fig. 9 is a schematic diagram of the structure of the pre-filtration component; Fig.10 It is a structural schematic diagram of the decomposed state of the pre-filtration component.

[0018] The symbols in the attached figure are: 1, distillation tower; 2, reboiler; 3, cooler; 4, phase separator; 5, crystallization tower; 6, heater; 7, low-pressure exhaust pipe; 8, discharge pipe; 9, gate; 10, filter plate bucket; 11, sieve plate; 12, vertical plate; 13, packing layer; 14, receiving hopper; 15, water jacket; 16, liquid replenishment pipe; 17, liquid return pipe; 18, pressurizing pipe; 19, screw; 20, bevel gear 1; 21, Drive shaft; 22, bevel gear 2; 23, motor 1; 24, baffle; 25, spring; 26, scraper; 27, slider; 28, hook rod; 29, motor 2; 30, shaft; 31, lever; 32, base; 33, filter cartridge; 34, top cover; 35, sealing wedge ring 1; 36, connecting pipe; 37, sealing wedge ring 2; 38, filter; 39, rotating shaft; 40, impeller; 41, propeller. DETAILED DESCRIPTION

[0019] In order to facilitate understanding of the present invention, the present invention will be described more fully below with reference to the relevant drawings. The present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present invention more thorough and comprehensive.

[0020] Example 1 like Figures 1 to 6As shown, a potassium tert-butoxide refining equipment comprises a distillation tower 1, a reboiler 2, a cooler 3 and a phase separator 4, wherein a distillation chamber is arranged inside the distillation tower 1, a feeding pipe connected to the distillation chamber is arranged at the top of the distillation tower 1, a multi-layer tower plate is arranged in the distillation chamber, the reboiler 2 is installed at the bottom of the distillation tower 1, the input end of the cooler 3 is connected to the top of the distillation chamber of the distillation tower 1, the input end of the phase separator 4 is connected to the output end of the cooler 3, a drain pipe is arranged at the bottom of the phase separator 4, a reflux pipe is arranged in the middle of the phase separator 4, and the output end of the reflux pipe extends into the top of the distillation chamber of the distillation tower 1; it also comprises a crystallization tower 5, a heater 6, a low-pressure exhaust pipe 7, a discharge pipe 8, a gate plate 9, a filter plate bucket 10 and a pre-filtration component, the crystallization tower 5 is located outside the distillation tower 1, a crystallization chamber is arranged inside the crystallization tower 5, and the distillation chamber of the distillation tower 1 and the crystallization chamber of the crystallization tower 5 are connected. The crystallization tower 1 is connected through a pre-filtering assembly, the heater 6 is installed at the bottom of the crystallization chamber of the crystallization tower 5, the input end of the low-pressure exhaust pipe 7 is connected to the top of the crystallization chamber of the crystallization tower 5, the output end of the low-pressure exhaust pipe 7 is connected to the input end of the cooler 3, the upper side wall of the crystallization tower 5 is installed with a discharge pipe 8, the discharge pipe 8 is communicated with the crystallization chamber of the crystallization tower 5, the gate 9 is liftably inserted on the discharge pipe 8, and the filter plate bucket 10 is liftably slidably installed in the crystallization chamber of the crystallization tower 5; it also includes a water jacket 15, a liquid replenishment pipe 16 and a liquid return pipe 17, the water jacket 15 is sleeved on the top outer wall of the distillation tower 1, the output end of the phase separator 4 is connected to the input end of the water jacket 15, the liquid replenishment pipe 16 is installed on the water jacket 15, the liquid replenishment pipe 16 is communicated with the inside of the water jacket 15, the output end of the water jacket 15 is installed with a liquid return pipe 17, and the output end of the liquid return pipe 17 extends into the top of the distillation chamber of the distillation tower 1.

[0021] During operation, ultrafine potassium hydroxide powder and tert-butanol are added to the top of the distillation tower 1 through a feeding pipe, and a carrying agent is continuously added to the distillation chamber of the distillation tower 1, so that the reaction solution of the carrying agent mixed with the ultrafine potassium hydroxide powder and the tert-butanol flows from top to bottom along the multi-layer tower plates, and the reboiler 2 is opened to heat the reaction liquid at the bottom of the distillation chamber of the distillation tower 1, so that the water produced by the reaction and the carrying agent boil together to produce mixed steam, and the mixed steam passes through the multi-layer tower plates from bottom to top in sequence, so that the mixed steam and the reaction solution are fully contacted between the multi-layer tower plates, so as to promote the reaction of the ultrafine potassium hydroxide powder with the tert-butanol to generate potassium tert-butoxide and water, and the mixed steam reaches the distillation tower 1. After reaching the top of the distillation chamber of the distillation tower 1, it enters the cooler 3 for cooling and liquefaction into a mixed liquid. The mixed liquid enters the phase separator 4 and is separated into layers. The water in the bottom layer is discharged from the phase separator 4. The carrier and tert-butyl alcohol in the upper oil phase are refluxed through the reflux pipe and refluxed into the water jacket 15. At the same time, the carrier is continuously transported to the water jacket 15 through the liquid replenishment pipe 16. The waste heat at the top of the distillation tower 1 preheats the mixed liquid therein through the water jacket 15. The preheated mixed liquid is refluxed into the distillation chamber of the distillation tower 1 through the liquid return pipe 17. When the water content in the reaction liquid is reduced to the set value, the kettle liquid in the distillation chamber of the distillation tower 1 is input into the crystallization tower 5 through the pre-filtration component. In the crystal chamber, the pre-filter assembly performs primary filtration on the kettle liquid, and the kettle liquid is allowed to settle in the crystallization chamber of the crystallization tower 5. The filter plate bucket 10 is raised from the bottom of the crystallization chamber of the crystallization tower 5 to be aligned with the discharge pipe 8, and the sediment and impurities in the kettle liquid are filtered. The gate plate 9 is raised to open the discharge pipe 8, and the sediment and impurities in the filter plate bucket 10 are cleaned out through the discharge pipe 8. The gate plate 9 closes the discharge pipe 8, and the filter plate bucket 10 descends back to the bottom of the crystallization chamber of the crystallization tower 5. The heater 6 is turned on to evaporate the kettle liquid, and the carrier, tert-butyl alcohol and n-butyl alcohol in the kettle liquid are evaporated into mixed steam 2, and the mixed steam 2 is input into the cooler 3 and the phase separator through the low-pressure exhaust pipe 7. After cooling and stratification in the device 4, they are discharged separately for recovery. After the kettle liquid is evaporated to dryness, tetrahydrofuran is added to the crystallization chamber of the crystallization tower 5 for dispersion. The filter plate bucket 10 is raised to filter the dispersion liquid again and then lowered to reset. The dispersion liquid is cooled to allow potassium tert-butoxide to crystallize out. The filter plate bucket 10 is raised to fish out the potassium tert-butoxide crystals and align them with the discharge pipe 8. The gate plate 9 is opened, and the potassium tert-butoxide crystals in the filter plate bucket 10 are discharged through the discharge pipe 8, thereby performing efficient evaporation, redispersion and cooling crystallization on the kettle liquid after azeotropic distillation, and potassium tert-butoxide can be efficiently discharged, which has good practicality and reduces the influence of the mixed liquid on the temperature at the top of the distillation chamber of the distillation tower 1.

[0022] Example 2 like Figures 1 to 4As shown, on the basis of Example 1, the tower plate includes a sieve plate 11 and a vertical plate 12, the sieve plate 11 is obliquely installed in the distillation chamber of the distillation tower 1, a gap for the reaction liquid to pass through is set between the high end of the sieve plate 11 and the interior of the distillation tower 1, and the vertical plate 12 is installed on the lower end surface of the high end of the sieve plate 11; it also includes a plurality of packing layers 13, and the lower end surfaces of the plurality of sieve plates 11 are all installed with the packing layers 13; it also includes a receiving hopper 14, which is installed at the top of the distillation chamber of the distillation tower 1, and the receiving hopper 14 is located below the feeding pipe of the distillation tower 1.

[0023] The space between the sieve plate 11 and the vertical plate 12 gathers the mixed steam rising from the bottom of the distillation chamber of the distillation tower 1, and disperses the mixed steam above it through the filter holes of the sieve plate 11, so that the mixed steam is fully mixed with the reaction liquid flowing on the sieve plate 11. At the same time, the vertical plate 12 and the inner wall of the distillation tower 1 guide the reaction liquid flowing downward. Since the multiple sieve plates 11 and the multiple vertical plates 12 are arranged in a staggered and inclined manner in sequence, the upwardly inclined sieve plate 11 slows down the flow rate of the reaction liquid and increases the contact time between the mixed steam and the reaction liquid, thereby improving the reaction efficiency. By installing multiple packing layers 13, the mixed steam gathered between the sieve plate 11 and the vertical plate 12 is dispersed, so that the mixed steam passes through the filter holes of the sieve plate 11 more evenly, which has good practicality. The receiving hopper 14 is used to carry the ultrafine potassium hydroxide powder added through the feeding pipe, reduce the ultrafine potassium hydroxide powder flowing with the reaction liquid, thereby reducing the blockage of the filter holes of the multiple sieve plates 11 and the pipeline of the reboiler 2 by the powdered sodium hydroxide, and improving reliability.

[0024] Example 3 like Figures 6 to 10As shown, on the basis of Example 1, it also includes a pressure pipe 18, which is installed on the top of the distillation tower 1, and the pressure pipe 18 is connected to the distillation chamber of the distillation tower 1; it also includes a screw 19, a bevel gear 1 20, a drive shaft 21, a bevel gear 22 and a motor 1 23, the screw 19 is vertically rotatably installed in the middle of the crystallization chamber of the crystallization tower 5, the screw 19 is transmission-connected to the filter plate bucket 10 through a screw nut, the upper end of the screw 19 is concentrically installed with a bevel gear 1 20, the drive shaft 21 is rotatably installed on the top of the crystallization chamber of the crystallization tower 5, the drive shaft 21 is concentrically installed with a bevel gear 22, the bevel gear 22 is meshed with the drive shaft 21, the motor 1 23 is installed on the crystallization tower 5, and the motor 1 23 is installed on the crystallization tower 5. The output shaft is connected to the drive shaft 21 in a transmission manner; it also includes a baffle 24 and a spring 25, an opening matching the discharge pipe 8 is set on the side wall of the filter plate bucket 10 facing the discharge pipe 8, the inner end of the discharge pipe 8 protrudes from the inner wall of the crystallization tower 5, the baffle 24 is slidably inserted into the opening of the filter plate bucket 10, the upper end of the spring 25 is connected to the filter plate bucket 10, and the lower end of the spring 25 is connected to the baffle 24; it also includes a scraper 26, a slider 27, a hook rod 28, a motor 29, a shaft rod 30 and a lever 31, the scraper 26 is slidably mounted on the inner side wall of the filter plate bucket 10, the slider 27 is elastically lifted and slidably mounted on the inner side wall of the scraper 26, the slider 27 is equipped with a hook rod 28, and the motor 29 is mounted on the crystallization tower 5 The shaft 30 is rotatably mounted on the top outer wall of the crystallization chamber of the crystallization tower 5, the shaft 30 is transmission-connected to the output end of the motor 29, one end of the lever 31 is connected to the shaft 30, and the other end of the lever 31 is provided with a hook, and the hook matches the hook rod 28; the pre-filtration assembly includes a base 32, a filter cartridge 33, a top cover 34, a sealing wedge ring 1 35, a connecting pipe 36, a sealing wedge ring 2 37, a filter 38, a rotating shaft 39, an impeller 40 and a propeller 41, the base 32 is connected to the crystallization chamber of the crystallization tower 5 through a flange pipe, the left end of the filter cartridge 33 is screwed and fastened to the base 32, the top cover 34 is screwed and fastened to the right end of the filter cartridge 33, and the middle of the right end of the top cover 34 A through hole 1 is provided, and a sealing wedge ring 1 35 is provided on the inner side wall of the through hole. The right end of the connecting pipe 36 is communicated with the distillation chamber of the distillation tower 1 through a flange pipe. The left end of the connecting pipe 36 extends into the through hole of the top cover 34. A sealing wedge ring 2 37 is provided on the left end of the connecting pipe 36. The sealing wedge ring 2 37 and the sealing wedge ring 1 35 are squeezed and sealed. The filter 38 is installed inside the filter cartridge 33, and the inlet of the filter 38 faces the connecting pipe 36. The middle part of the rotating shaft 39 is rotatably connected to the bottom of the filter 38. An impeller 40 is installed at one end of the rotating shaft 39, and the impeller 40 is located in the filter 38. A propeller 41 is installed at the other end of the rotating shaft 39, and the propeller 41 is located at the flange pipe inlet of the base 32.

[0025] High-pressure air is input into the distillation chamber of the distillation tower 1 through the pressure pipe 18, so that the high-pressure air presses the kettle liquid out of the distillation chamber of the distillation tower 1 and inputs it into the crystallization chamber of the crystallization tower 5, thereby improving the drainage efficiency. The motor 1 23 drives the drive shaft 21 to rotate, and the drive shaft 21 drives the bevel gear 22 to rotate. The bevel gear 22 meshes with the bevel gear 1 20 to drive the screw 19 to rotate. The screw 19 drives the filter plate bucket 10 to rise and fall in the crystallization chamber of the crystallization tower 5 through the screw nut. The driving effect is stable and reliable. When the filter plate bucket 10 When the filter plate bucket 10 is raised to align with the discharge pipe 8, the inner end of the discharge pipe 8 blocks the baffle 24, thereby opening the opening of the filter plate bucket 10, making it convenient to discharge impurities or potassium tert-butoxide crystals in the filter plate bucket 10 through the discharge pipe 8. When the filter plate bucket 10 is lowered, the elastic force of the spring 25 pushes the baffle 24 up and resets it to close the opening of the filter plate bucket 10, which is practical. When the filter plate bucket 10 is raised to align with the discharge pipe 8, the motor 29 drives the shaft 30 and the lever 31 to rotate, so that the hook of the lever 31 hooks the hook rod 28, and the lever 31 is rotated. 1 is continuously rotated, thereby pulling the scraper 26 toward the opening of the filter plate bucket 10 through the slider 27, so that the scraper 26 pushes the impurities or potassium tert-butoxide crystals in the filter plate bucket 10 through the opening into the discharge pipe 8 for discharge, thereby improving the discharge efficiency. When the base 32 is connected to the crystallization tower 5 and the connecting pipe 36 is connected to the distillation tower 1, the sealing wedge ring 2 37 and the sealing wedge ring 1 35 are squeezed and sealed, and the kettle liquid in the distillation tower 1 is input into the filter cylinder 33 through the connecting pipe 36, and the filter 38 performs preliminary filtration on the kettle liquid, so that the The filtered kettle liquid is input into the crystallization chamber of the crystallization tower 5 through the flange pipe of the base 32. The kettle liquid flowing through the flange pipe of the base 32 and the propeller 41 drive the rotating shaft 39 to rotate, and the rotating shaft 39 drives the impeller 40 to rotate. The impeller 40 stirs the kettle liquid in the filter 38, so that the kettle liquid accelerates to collide with the filter 38, thereby improving the filtering efficiency of the filter 38. The filter cartridge 33 is connected to the base 32 and the top cover 34 by screw connection, which is convenient for disassembling the filter cartridge 33 and cleaning the filter 38 inside the filter cartridge 33.

[0026] like Figures 1 to 10As shown, a potassium tert-butoxide refining device of the present invention, when working, firstly, ultrafine potassium hydroxide powder and tert-butanol are added to the top of the distillation tower 1 through the feeding pipe, and a carrying agent is continuously added to the distillation chamber of the distillation tower 1 through the liquid replenishing pipe 16, so that the reaction solution of the carrying agent mixed with the ultrafine potassium hydroxide powder and the tert-butanol flows from top to bottom along the multi-layer tower plate, and the reboiler 2 is opened to heat the reaction liquid at the bottom of the distillation chamber of the distillation tower 1, so that the water produced by the reaction and the carrying agent boil together to generate mixed steam, and the mixed steam passes through the multi-layer sieve plate 11 and the multi-layer packing layer 13 from bottom to top in sequence, so that the mixed steam and the reaction solution are fully contacted between the multi-layer sieve plate 11 and the vertical plate 12, so as to promote the reaction of the ultrafine potassium hydroxide powder with the tert-butanol to generate potassium tert-butoxide and Water, then the mixed steam reaches the top of the distillation chamber of the distillation tower 1 and enters the cooler 3 to be cooled and liquefied into a mixed liquid. The mixed liquid enters the phase separator 4 and then is separated into layers. The water in the bottom layer is discharged from the phase separator 4, and the carrier and tert-butyl alcohol in the upper oil phase are refluxed into the water jacket 15 through the reflux pipe. At the same time, the carrier is continuously transported to the water jacket 15 through the liquid replenishment pipe 16. The waste heat at the top of the distillation tower 1 is used to preheat the mixed liquid therein through the water jacket 15. The preheated mixed liquid is refluxed into the distillation chamber of the distillation tower 1 through the liquid return pipe 17. Then, when the water content in the reaction liquid is reduced to the set value, high-pressure air is input into the distillation chamber of the distillation tower 1 through the pressurizing pipe 18, so that the high-pressure air presses the kettle liquid out of the distillation chamber of the distillation tower 1 and inputs it into the crystallization tower 5. In the chamber, during this process, the kettle liquid in the distillation tower 1 is input into the filter cylinder 33 through the connecting pipe 36, and the filter 38 performs preliminary filtration on the kettle liquid, so that the filtered kettle liquid is input into the crystallization chamber of the crystallization tower 5 through the flange pipe of the base 32, and the kettle liquid flowing through the flange pipe of the base 32 and the propeller 41 drive the rotating shaft 39 to rotate, and the rotating shaft 39 drives the impeller 40 to rotate, and the impeller 40 stirs the kettle liquid in the filter 38, so that the kettle liquid accelerates to collide with the filter 38, thereby improving the filtration efficiency of the filter 38, and the kettle liquid is statically precipitated in the crystallization chamber of the crystallization tower 5, and the filter plate bucket 10 is raised from the bottom of the crystallization chamber of the crystallization tower 5 to be aligned with the discharge pipe 8, so as to filter the precipitate and impurities in the kettle liquid, and the gate plate 9 is raised to open the discharge pipe 8, and the filter plate bucket 10 is The precipitate and impurities are cleaned out through the discharge pipe 8, the gate plate 9 closes the discharge pipe 8, the filter plate bucket 10 descends back to the bottom of the crystallization chamber of the crystallization tower 5, the heater 6 is turned on to evaporate the kettle liquid, and the carrying agent, tert-butyl alcohol and n-butyl alcohol in the kettle liquid are evaporated into mixed steam 2, and the mixed steam 2 is input into the cooler 3 and the phase separator 4 through the low-pressure exhaust pipe 7 for cooling and stratification, and then discharged for recovery. After the kettle liquid is evaporated, tetrahydrofuran is added to the crystallization chamber of the crystallization tower 5 for dispersion, the filter plate bucket 10 is raised to filter the dispersion again and then descended to reset, and finally the dispersion is cooled to make potassium tert-butylate crystals precipitate, the filter plate bucket 10 is raised to fish out the potassium tert-butylate crystals and align them with the discharge pipe 8, the gate plate 9 is opened, and the motor 29 drives the shaft 30 and the lever 31 to rotate.The hook of the lever 31 hooks the hook rod 28, and the lever 31 rotates continuously, thereby pulling the scraper 26 toward the opening of the filter plate bucket 10 through the slider 27, so that the scraper 26 pushes the impurities or potassium tert-butoxide crystals in the filter plate bucket 10 through the opening into the discharge pipe 8 for discharge.

[0027] The main functions achieved by the present invention are: 1. It can efficiently evaporate, redisperse and cool and crystallize the kettle liquid after azeotropic distillation; 2. It can efficiently discharge potassium tert-butoxide and has good practicality; 3. The inclined tower plate can slow down the flow rate of the reaction liquid and increase the contact time between the mixed steam and the reaction liquid; 4. Use the waste heat to preheat the refluxed liquid to reduce the influence of the mixed liquid on the temperature at the top of the distillation chamber of the distillation tower 1; 5. It is capable of efficiently filtering the liquid. The filter cartridge 33 is connected to the base 32 and the top cover 34 by screw connection, so that the filter cartridge 33 can be easily disassembled and the filter 38 inside the filter cartridge 33 can be cleaned.

[0028] The potassium tert-butoxide refining equipment of the present invention has an installation mode, a connection mode or a setting mode which are all common mechanical modes, and can be implemented as long as the beneficial effects can be achieved; the potassium tert-butoxide refining equipment of the present invention has a distillation tower 1, a reboiler 2, a cooler 3, a phase separator 4, a crystallization tower 5, a heater 6, a low-pressure exhaust pipe 7, a gate plate 9, a filter plate bucket 10, a sieve plate 11, a vertical plate 12, a packing layer 13, a receiving hopper 14, a water jacket 15, a pressurizing pipe 18, a screw 19, a bevel gear 1 20, a drive shaft 21, a bevel gear 22, a motor 1 23, a spring 25, a slider 27, a motor 29, a shaft 30, a lever 31, a filter 38, a rotating shaft 39, an impeller 40, and a propeller 41 which are purchased on the market.

[0029] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the technical principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A potassium tert-butoxide refining device, comprising a distillation tower (1), a reboiler (2), a cooler (3) and a phase separator (4); a distillation chamber is arranged inside the distillation tower (1), a feeding pipe communicating with the distillation chamber is arranged at the top of the distillation tower (1), and a plurality of trays are arranged in the distillation chamber; the reboiler (2) is installed at the bottom of the distillation tower (1), an input end of the cooler (3) is connected to the top of the distillation chamber; an input end of the phase separator (4) is connected to the output end of the cooler (3), a drain pipe is arranged at the bottom of the phase separator (4), a reflux pipe is arranged in the middle of the phase separator (4), and the output end of the reflux pipe extends into the top of the distillation chamber; characterized in that It also comprises a crystallization tower (5), a heater (6), a low-pressure exhaust pipe (7), a discharge pipe (8), a gate plate (9), a filter plate bucket (10) and a pre-filtering assembly; the crystallization tower (5) is located outside the distillation tower (1); a crystallization chamber is arranged inside the crystallization tower (5); the distillation chamber of the distillation tower (1) and the crystallization chamber of the crystallization tower (5) are connected via the pre-filtering assembly; the heater (6) is installed at the bottom of the crystallization chamber; the input end of the low-pressure exhaust pipe (7) is connected to the top of the crystallization chamber; the output end of the low-pressure exhaust pipe (7) is connected to the input end of the cooler (3); the discharge pipe (8) is installed on the upper side wall of the crystallization tower (5); the discharge pipe (8) is connected to the crystallization chamber; the gate plate (9) is liftably inserted on the discharge pipe (8); and the filter plate bucket (10) is liftably slidably installed in the crystallization chamber.

2. A potassium tert-butoxide refining equipment as claimed in claim 1, characterized in that: The tower plate comprises a sieve plate (11) and a vertical plate (12); the sieve plate (11) is installed obliquely in the distillation chamber of the distillation tower (1); a gap for the reaction liquid to pass through is provided between the high end of the sieve plate (11) and the interior of the distillation tower (1); the vertical plate (12) is installed on the lower end surface of the high end of the sieve plate (11).

3. A potassium tert-butoxide refining equipment as claimed in claim 2, characterized in that, The distillation tower (1) further comprises a plurality of packing layers (13) inside, and the lower end surfaces of the plurality of sieve plates (11) are all equipped with the packing layers (13).

4. A potassium tert-butoxide refining equipment as claimed in claim 1, characterized in that: It also comprises a receiving hopper (14), wherein the receiving hopper (14) is installed at the top of the distillation chamber of the distillation tower (1), and the receiving hopper (14) is located below the feeding pipe of the distillation tower (1).

5. A potassium tert-butoxide refining equipment as claimed in claim 1, characterized in that: The invention also comprises a water jacket (15), a liquid replenishment pipe (16) and a liquid return pipe (17), wherein the water jacket (15) is sleeved on the top outer wall of the distillation tower (1), the output end of the phase separator (4) is connected to the input end of the water jacket (15), the liquid replenishment pipe (16) is installed on the water jacket (15), the liquid replenishment pipe (16) is communicated with the inside of the water jacket (15), the output end of the water jacket (15) is installed with the liquid return pipe (17), and the output end of the liquid return pipe (17) extends into the top of the distillation chamber of the distillation tower (1).

6. A potassium tert-butoxide refining equipment as claimed in claim 1, characterized in that: It also comprises a pressurizing pipe (18), wherein the pressurizing pipe (18) is installed at the top of the distillation tower (1), and the pressurizing pipe (18) is connected to the distillation chamber of the distillation tower (1).

7. A potassium tert-butoxide refining equipment as claimed in claim 1, characterized in that: The invention also comprises a screw (19), a bevel gear 1 (20), a drive shaft (21), a bevel gear 2 (22) and a motor 1 (23); the screw (19) is vertically rotatably mounted in the middle of the crystallization chamber of the crystallization tower (5); the screw (19) is transmission-connected to the filter plate bucket (10) via a screw nut; the bevel gear 1 (20) is concentrically mounted on the upper end of the screw (19); the drive shaft (21) is rotatably mounted on the top of the crystallization chamber of the crystallization tower (5); the bevel gear 2 (22) is concentrically mounted on the drive shaft (21); the bevel gear 2 (22) is meshed with the drive shaft (21); the motor 1 (23) is mounted on the crystallization tower (5); and the output shaft of the motor 1 (23) is transmission-connected to the drive shaft (21).

8. A potassium tert-butoxide refining equipment as claimed in claim 1, characterized in that: It also includes a baffle (24) and a spring (25); an opening matching the discharge pipe (8) is provided on the side wall of the filter plate bucket (10) facing the discharge pipe (8); the inner end of the discharge pipe (8) protrudes from the inner wall of the crystallization tower (5); the baffle (24) is slidably inserted into the opening of the filter plate bucket (10); the upper end of the spring (25) is connected to the filter plate bucket (10), and the lower end of the spring (25) is connected to the baffle (24).

9. A potassium tert-butoxide refining equipment as claimed in claim 1, characterized in that: It also includes a scraper (26), a slider (27), a hook rod (28), a second motor (29), a shaft rod (30) and a lever (31); the scraper (26) is slidably mounted on the inner side wall of the filter plate bucket (10); the slider (27) is elastically lifted and slidably mounted on the inner side wall of the scraper (26); the hook rod (28) is mounted on the slider (27); the second motor (29) is mounted on the top outer wall of the crystallization tower (5); the shaft rod (30) is rotatably mounted on the top of the crystallization chamber of the crystallization tower (5); the shaft rod (30) is transmission-connected to the output end of the second motor (29); one end of the lever (31) is connected to the shaft rod (30); the other end of the lever (31) is provided with a hook, and the hook matches the hook rod (28).

10. A potassium tert-butoxide refining equipment as claimed in claim 1, characterized in that: The pre-filter assembly comprises a base (32), a filter cartridge (33), a top cover (34), a sealing wedge ring 1 (35), a connecting pipe (36), a sealing wedge ring 2 (37), a filter (38), a rotating shaft (39), an impeller (40) and a propeller (41); the base (32) is connected to the crystallization chamber of the crystallization tower (5) through a flange pipe, the left end of the filter cartridge (33) is screwed and fastened to the base (32), the top cover (34) is screwed and fastened to the right end of the filter cartridge (33), a through hole 1 is provided in the middle of the right end of the top cover (34), a sealing wedge ring 1 (35) is provided on the inner side wall of the through hole 1, and the right end of the connecting pipe (36) is connected to the distillation tower (1) through the flange pipe. ), the left end of the connecting pipe (36) extends into the through hole 1 of the top cover (34), the left end of the connecting pipe (36) is provided with a sealing wedge ring 2 (37), the sealing wedge ring 2 (37) and the sealing wedge ring 1 (35) are squeezed and sealed, the filter (38) is installed inside the filter cartridge (33), the inlet of the filter (38) faces the connecting pipe (36), the middle part of the rotating shaft (39) is rotatably connected to the bottom of the filter (38), one end of the rotating shaft (39) is provided with an impeller (40), the impeller (40) is located in the filter (38), and the other end of the rotating shaft (39) is provided with a propeller (41), the propeller (41) is located at the flange pipe inlet of the base (32).

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