Potassium fluoride recovery device
By designing a fluoride recycling device that includes multiple centrifugal machines and processors, the problem of unable to effectively recycle potassium fluoride in existing technology, realize the efficient recycling and utilization of potassium fluoride, reduce the cost and cost of raw materials and the cost of raw materials Environmental pollution.
Patent Information
- Application Number
- CN202323537321.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-22
- Publication Date
- 2025-01-28
- Estimated Expiration
- 2033-12-22
AI Technical Summary
The prior art cannot effectively recover potassium fluoride mixed salts produced during the synthesis of fluorovinyl carbonate, resulting in waste of resources and increased raw material costs.
Designed a type of potassium fluoride recycling device, including a three -in -one filter, a mixed -salt dissolved kettle, a second centrifugal machine, a potassium concentrator, a third centrifugal machine and a flusher -flushing dryer. The solution is separated, dissolved, concentrated, and flashing to achieve the recovery and utilization of potassium fluoride.
Effective recycling and using undocumented potassium fluoride reduces the cost of potassium fluoride raw materials in fluoride reactions, and reduces environmental pollution and waste of resources.
Smart Images
Figure CN222400611U_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of chemical recovery, in particular to a potassium fluoride recovery device. Background Art
[0002] When synthesizing fluoroethylene carbonate, it is usually prepared by fluorination reaction of purified chloroethylene carbonate and a fluorinating agent, and potassium fluoride is often used as the fluorinating agent. In order to increase the conversion rate of chloroethylene carbonate, an excess of potassium fluoride is usually added to the reactor, so a large amount of potassium chloride and potassium fluoride mixed salt is generated in the reactor after the reaction is completed, and a large amount of organic matter is also entrained in the mixed salt.
[0003] If the mixed salt is discharged directly, it will not only cause environmental pollution, but also waste resources. The existing mixed salt treatment method mainly involves high-temperature calcination, defluorination treatment, and MVR treatment to convert the mixed salt into potassium chloride as a by-product for sale.
[0004] By using the above treatment method, fluoride ions in the mixed salt are removed, and potassium ions are all sold in the form of potassium chloride, resulting in that the excess potassium fluoride cannot be recycled, thereby increasing the cost of potassium fluoride raw materials in the fluoridation reaction. Utility Model Content
[0005] In order to recycle potassium fluoride and reduce the cost of potassium fluoride raw materials in fluoridation reactions, the present application provides a potassium fluoride recovery device.
[0006] The potassium fluoride recovery device provided in this application adopts the following technical solution:
[0007] A potassium fluoride recovery device, comprising:
[0008] A three-in-one filter press connected to the discharge port of the fluorination kettle, and a first centrifuge is arranged between the three-in-one filter press and the fluorination kettle;
[0009] A mixed salt dissolving kettle is connected to the three-in-one filter press, and the mixed salt dissolving kettle is connected to a water inlet pipe;
[0010] A second centrifuge connected to the mixed salt dissolving kettle;
[0011] a potash concentrator connected to the second centrifuge;
[0012] A third centrifuge is connected to the potassium salt concentrator, and the third centrifuge is connected to a potassium chloride collection tank;
[0013] The potassium fluoride flash dryer is connected to the third centrifuge, and the potassium fluoride flash dryer is connected to a potassium fluoride collecting tank.
[0014] By adopting the above technical scheme, after the fluorination reaction is completed, the unreacted potassium fluoride and the product are left in the fluorination kettle together, and the solid-liquid separation is carried out by the first centrifuge. The separated solid phase includes potassium fluoride, potassium chloride and impurities such as acetonitrile carried, and enters the three-in-one filter press to remove acetonitrile. Potassium fluoride and potassium chloride enter the mixed salt dissolution kettle, and fresh water is added through the water inlet pipe to dissolve potassium fluoride and potassium chloride. The impurities insoluble in water are separated by the second centrifuge, and the solid phase enters the potassium salt concentrator. A large amount of potassium chloride and a small amount of potassium fluoride are precipitated by heating and concentration. After separation by the third centrifuge, the solid phase enters the potassium chloride collection tank, and the liquid phase reaches the potassium fluoride flash dryer. The liquid phase is flashed to precipitate potassium fluoride and enter the potassium fluoride collection tank. Thereby, the recycling of potassium fluoride is realized, and the cost of potassium fluoride raw materials in the fluorination reaction is reduced.
[0015] Optionally, a condenser, an acetonitrile recovery tank and an acetonitrile transfer pump are sequentially connected to the top of the three-in-one filter press, and one end of the acetonitrile transfer pump away from the acetonitrile recovery tank is connected to the three-in-one filter press.
[0016] By adopting the above technical solution, in the three-in-one filter press, acetonitrile and other liquid impurities are vaporized by heat and reach the top of the three-in-one filter press, cooled by the condenser and enter the acetonitrile recovery tank, the acetonitrile transfer pump circulates the acetonitrile back to the three-in-one filter press, and the acetonitrile and other liquid phases are mixed to form a filtrate and discharged.
[0017] Optionally, the three-in-one filter press and the potassium salt concentrator are both provided with a jacket, and the jacket is provided with a steam inlet and a condensed water outlet.
[0018] By adopting the above technical solution, the jacket is used to pass steam, so as to heat the raw materials in the three-in-one filter press and the potassium salt concentrator.
[0019] Optionally, the end of the second centrifuge away from the mixed salt dissolution kettle is connected to a buffer tank, in which activated carbon for decolorization is placed, and the liquid in the buffer tank re-enters the second centrifuge.
[0020] By adopting the above technical solution, the activated carbon can adsorb impurities such as organic matter in the reaction liquid, and further separate them through the second centrifuge, so that the concentrations of potassium fluoride and potassium chloride in the reaction liquid are increased.
[0021] Optionally, the second centrifuge is configured as a bag plate centrifuge, and the second centrifuge is connected to an insoluble matter collection tank.
[0022] By adopting the above technical solution, the bag plate centrifuge can put the solid phase centrifuged into a cloth bag and transfer it to an insoluble matter collection tank for collection.
[0023] Optionally, one end of the third centrifuge away from the potassium salt concentrator is connected to a potassium fluoride aqueous solution tank, and a potassium fluoride aqueous solution transfer pump is provided between the potassium fluoride aqueous solution tank and the potassium fluoride flash dryer.
[0024] By adopting the above technical solution, the potassium fluoride aqueous solution pipe tank can be used for buffering and collection, and the potassium fluoride aqueous solution transfer pump transports the potassium fluoride aqueous solution to the potassium fluoride flash dryer.
[0025] Optionally, the three-in-one filter press and the potassium salt concentrator are commonly connected to a hot water tank, and the hot water tank is cyclically connected to the jacket via a hot water circulation pump.
[0026] By adopting the above technical solution, the hot water tank stores hot water, which can provide hot water heating to each hot spot.
[0027] Optionally, the potassium fluoride flash dryer, the potassium salt concentrator and the potassium fluoride aqueous solution tank are all connected to a steam exhaust pipe.
[0028] By adopting the above technical solution, the water vapor generated after heating is discharged outside the device through the steam exhaust pipe.
[0029] In summary, this application has the following beneficial effects:
[0030] After the fluorination reaction is completed, the unreacted potassium fluoride and the product are left in the fluorination kettle together, and the solid-liquid separation is carried out by the first centrifuge. The separated solid phase includes potassium fluoride, potassium chloride and impurities such as acetonitrile carried, and enters the three-in-one filter press to remove acetonitrile. Potassium fluoride and potassium chloride enter the mixed salt dissolution kettle, and fresh water is added through the water inlet pipe to dissolve potassium fluoride and potassium chloride. The impurities insoluble in water are separated by the second centrifuge. The solid phase enters the potassium salt concentrator, and a large amount of potassium chloride and a small amount of potassium fluoride are precipitated by heating and concentration. After separation by the third centrifuge, the solid phase enters the potassium chloride collection tank, and the liquid phase reaches the potassium fluoride flash dryer. The liquid phase is flashed to precipitate potassium fluoride and enter the potassium fluoride collection tank. In this way, the recycling of potassium fluoride is realized, and the cost of potassium fluoride raw materials in the fluorination reaction is reduced. BRIEF DESCRIPTION OF THE DRAWINGS
[0031] Figure 1 It is a schematic diagram of the overall structure of the embodiment of the present application;
[0032] Figure 2 It is a schematic diagram of the structure of a three-in-one filter press and a mixed salt dissolving kettle according to an embodiment of the present application;
[0033] Figure 3 It is a schematic diagram of the structure of the potassium salt concentrator and the potassium fluoride flash dryer in the embodiment of the present application;
[0034] Figure 4It is a schematic diagram of the structure of the hot water tank of the embodiment of the present application.
[0035] Description of reference numerals:
[0036] 1. Three-in-one filter press; 11. Fluorination kettle; 12. First centrifuge; 13. Condenser; 14. Acetonitrile recovery tank; 15. Acetonitrile transfer pump; 2. Mixed salt dissolving kettle; 21. Water inlet pipe; 3. Second centrifuge; 31. Insoluble matter collection tank; 32. Buffer tank; 4. Potassium salt concentrator; 41. Jacket; 42. Third centrifuge; 43. Potassium chloride collection tank; 5. Potassium fluoride flash dryer; 51. Potassium fluoride collection tank; 6. Potassium fluoride aqueous solution tank; 61. Potassium fluoride aqueous solution transfer pump; 7. Hot water tank; 71. Hot water circulation pump; 8. Steam discharge pipe. DETAILED DESCRIPTION
[0037] The following is combined with Figure 1-4 This application is described in further detail.
[0038] The present application embodiment discloses a potassium fluoride recovery device. Figure 1 A potassium fluoride recovery device includes a first centrifuge 12, a three-in-one filter press 1, a mixed salt dissolving kettle 2, a second centrifuge 3, a potassium salt concentrator 4, a third centrifuge 42 and a potassium fluoride flash dryer 5.
[0039] Reference Figure 1 and Figure 2 After the fluorination reaction is completed, the generated potassium chloride, unreacted potassium fluoride and liquid are left in the fluorination kettle 11 together. The first centrifuge 12 is connected to the discharge port of the fluorination kettle 11. The first centrifuge 12 is used to separate the solid and liquid, and the potassium fluoride, potassium chloride and liquid are initially separated. The separated solid phase includes potassium fluoride, potassium chloride and impurities such as acetonitrile and organic matter contained therein. The three-in-one filter press 1 is connected to the first centrifuge 12, and the solid phase enters the three-in-one filter press 1.
[0040] The outer sleeve of the three-in-one filter press 1 is provided with a jacket 41, and the jacket 41 is provided with a hot water inlet and a cold water outlet. Hot water can be introduced into the jacket 41 to heat the solid phase in the three-in-one filter press 1, and the acetonitrile solvent carried by the solid phase is vaporized to reach the top of the three-in-one filter press 1. The top of the three-in-one filter press 1 is sequentially connected with a condenser 13, an acetonitrile recovery tank 14 and an acetonitrile transfer pump 15, and the end of the acetonitrile transfer pump 15 away from the acetonitrile recovery tank 14 is connected to the three-in-one filter press 1. After acetonitrile is vaporized, it enters the condenser 13 for cooling and enters the acetonitrile recovery tank 14. The acetonitrile recovery tank 14 is connected with a nitrogen pipe, and the acidic gas in the acetonitrile is discharged into the tail gas absorption unit by blowing nitrogen. The acetonitrile transfer pump 15 returns the acetonitrile to the three-in-one filter press 1, and forms a liquid phase through acetonitrile and other organic impurities. The three-in-one filter press 1 filters the solid phase and liquid phase such as potassium fluoride and potassium chloride, and dries the solid phase. The mixed salt dissolving kettle 2 is connected to the three-in-one filter press 1, and the dried solid phase enters the mixed salt dissolving kettle 2.
[0041] The mixed salt dissolving kettle 2 is connected to a water inlet pipe 21, through which fresh water enters the mixed salt dissolving kettle 2, potassium fluoride and potassium chloride are dissolved in water to form a liquid phase, and water-insoluble impurities form a solid phase. The second centrifuge 3 is connected to the mixed salt dissolving kettle 2, and the aqueous solution enters the second centrifuge 3. The second centrifuge 3 uses a bag-type plate centrifuge, and the solid phase remains in the bag. The second centrifuge 3 is connected to a buffer tank 32, in which activated carbon is placed. The buffer tank 32 is reconnected to the second centrifuge 3, and the liquid phase of the second centrifuge 3 enters the buffer tank 32. The liquid phase is decolorized by the activated carbon to adsorb organic impurities. The decolorized liquid phase reenters the second centrifuge 3 for centrifugation to separate the water-insoluble substances from the aqueous solution of potassium fluoride and potassium chloride. The second centrifuge 3 is connected to an insoluble matter collection tank 31, and the solid phase remains in the bag of the bag-type plate centrifuge, so that the insoluble matter can be packaged.
[0042] Reference Figure 1 and Figure 3 The potassium salt concentrator 4 is connected to the second centrifuge 3, and the liquid phase of the second centrifuge 3, that is, the mixed aqueous solution of potassium fluoride and potassium chloride, enters the potassium salt concentrator 4. There is a difference in the solubility of potassium fluoride and potassium chloride in water. At the same temperature, the solubility of potassium fluoride in water is higher than that of potassium chloride. The outer sleeve of the potassium salt concentrator 4 is provided with a jacket 41, and the jacket 41 is provided with a hot water inlet and a cold water outlet, so that the mixed aqueous solution of potassium fluoride and potassium chloride can be heated by passing hot water into the jacket 41, and the water evaporates and becomes water vapor by gradually increasing the heating temperature, and the solution gradually reaches a saturated state, so that a large amount of potassium chloride and a small amount of potassium fluoride are precipitated.
[0043] The third centrifuge 42 is connected to the potassium salt concentrator 4. The precipitated large amount of potassium chloride and a small amount of potassium fluoride are separated from the potassium fluoride aqueous solution by centrifugation in the third centrifuge 42. The third centrifuge 42 is connected to a potassium chloride collecting tank 43. The precipitated large amount of potassium chloride and a small amount of potassium fluoride enter the potassium chloride collecting tank 43 and are packaged as potassium chloride by-products for sale.
[0044] The third centrifuge 42 is connected to a potassium fluoride aqueous solution tank 6, and a potassium fluoride aqueous solution transfer pump 61 is provided between the potassium fluoride aqueous solution tank 6 and the potassium fluoride flash dryer 5, and the potassium fluoride aqueous solution is transported to the potassium fluoride flash dryer 5 by the potassium fluoride aqueous solution transfer pump 61. The potassium fluoride flash dryer 5 comprises a heater, an induced draft fan, a cyclone separator, a spray gun, a drying chamber, etc., wherein the heater heats the potassium fluoride aqueous solution, the spray gun sprays potassium fluoride into microparticles and dries it in the drying chamber, the cyclone separator is used to concentrate the dried potassium fluoride particles, and the induced draft fan sucks the gas. The potassium fluoride aqueous solution is heated by the potassium fluoride flash dryer 5 under a slightly negative pressure environment to separate water vapor and solids, and the generated water vapor is discharged through high altitude, and the potassium fluoride flash dryer 5 is connected to a potassium fluoride collecting tank 51, and the potassium fluoride solid enters the potassium fluoride collecting tank 51, and is packaged or transported to the fluorination kettle 11 through a pipeline.
[0045] The potassium fluoride flash dryer 5, the potassium salt concentrator 4 and the potassium fluoride aqueous solution tank 6 are all connected to a steam exhaust pipe 8. When the aqueous solution is heated, the solvent water evaporates and becomes water vapor, and the water vapor can be discharged into the environment through the steam exhaust pipe 8.
[0046] Reference Figure 4 The potassium fluoride recovery device also includes a hot water tank 7, in which hot water is stored. The hot water is connected to the jacket 41 through a hot water circulation pump 71 and a pipeline, so that hot water is added to the jacket 41 through the hot water circulation pump 71 to heat the aqueous solution.
[0047] The implementation principle of a potassium fluoride recovery device in the embodiment of the present application is as follows: the solid-liquid separation of the material in the fluorination kettle 11 is carried out by the first centrifuge 12, and the solids such as potassium fluoride and potassium chloride enter the mixed salt dissolution kettle 2, and fresh water is added to dissolve potassium fluoride and potassium chloride in water to form a liquid phase. After the insoluble matter is separated by the second centrifuge 3, the liquid phase enters the buffer tank 32, and is decolorized by activated carbon, and then returns to the second centrifuge 3 to separate the insoluble solids and arrives at the potassium salt concentrator 4. By heating the water to volatilize, a large amount of potassium chloride and a small amount of potassium fluoride are precipitated, and the potassium chloride solid is separated by the third centrifuge 42 and enters the potassium chloride collection tank 43. The remaining potassium fluoride aqueous solution enters the potassium fluoride aqueous solution tank 6, and enters the potassium fluoride flash dryer 5 through the potassium fluoride aqueous solution transfer pump 61, and is heated to separate the water vapor and solid, and the potassium fluoride solid enters the potassium fluoride collection tank 51.
[0048] This specific implementation manner is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make non-creative modifications to the specific implementation manner as needed, but such modifications are protected by patent law as long as they are within the scope of the claims of the present application.
Claims
1. A potassium fluoride recovery device, characterized in that: include: A three-in-one filter press (1) is connected to the discharge port of the fluorination kettle (11), and a first centrifuge (12) is arranged between the three-in-one filter press (1) and the fluorination kettle (11); A mixed salt dissolving kettle (2) is connected to the three-in-one filter press (1), and the mixed salt dissolving kettle (2) is connected to a water inlet pipe (21); A second centrifuge (3) connected to the mixed salt dissolving kettle (2); a potassium salt concentrator (4), connected to the second centrifuge (3); A third centrifuge (42) is connected to the potassium salt concentrator (4), and the third centrifuge (42) is connected to a potassium chloride collection tank (43); The potassium fluoride flash dryer (5) is connected to the third centrifuge (42), and the potassium fluoride flash dryer (5) is connected to a potassium fluoride collecting tank (51).
2. A potassium fluoride recovery device according to claim 1, characterized in that: The top of the three-in-one filter press (1) is connected in sequence to a condenser (13), an acetonitrile recovery tank (14) and an acetonitrile transfer pump (15); one end of the acetonitrile transfer pump (15) away from the acetonitrile recovery tank (14) is connected to the three-in-one filter press (1).
3. A potassium fluoride recovery device according to claim 1, characterized in that: The three-in-one filter press (1) and the potassium salt concentrator (4) are both provided with a jacket (41), and the jacket (41) is provided with a hot water inlet and a cold water outlet.
4. A potassium fluoride recovery device according to claim 1, characterized in that The end of the second centrifuge (3) away from the mixed salt dissolving kettle (2) is connected to a buffer tank (32), in which activated carbon for decolorization is placed, and the liquid in the buffer tank (32) re-enters the second centrifuge (3).
5. A potassium fluoride recovery device according to claim 1, characterized in that: The second centrifuge (3) is configured as a bag-type plate centrifuge, and the second centrifuge (3) is connected to an insoluble matter collection tank (31).
6. A potassium fluoride recovery device according to claim 1, characterized in that: The end of the third centrifuge (42) away from the potassium salt concentrator (4) is connected to a potassium fluoride aqueous solution tank (6), and a potassium fluoride aqueous solution transfer pump (61) is provided between the potassium fluoride aqueous solution tank (6) and the potassium fluoride flash dryer (5).
7. A potassium fluoride recovery device according to claim 3, characterized in that: The three-in-one filter press (1) and the potassium salt concentrator (4) are commonly connected to a hot water tank (7), and the hot water tank (7) is cyclically connected to the jacket (41) via a hot water circulation pump (71).
8. A potassium fluoride recovery device according to claim 6, characterized in that: The potassium fluoride flash dryer (5), the potassium salt concentrator (4) and the potassium fluoride aqueous solution tank (6) are all connected to a steam discharge pipe (8).