A method for synthesizing potassium fluoride by using potassium hydroxide as by-product of organic fluorination reaction

By adding hydrofluoric acid to the potassium hydroxide solution and using a homogenizing component and heating vacuum technology, the problem of low purity in the preparation of potassium fluoride is solved, and high-purity potassium fluoride is efficiently generated.

CN117466310BActive Publication Date: 2025-10-10INNER MONGOLIA XINGHAN FUDU CHEM CO LTD
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Patent Information

Application Number
CN202311442443.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-11-01
Publication Date
2025-10-10
Estimated Expiration
2043-11-01

AI Technical Summary

Technical Problem

In the prior art, hydrofluoric acid has a poor dispersion effect when added to the by-product potassium hydroxide solution, resulting in low reaction efficiency and low purity of the prepared potassium fluoride.

Method used

A feeding mechanism is used to add hydrofluoric acid to the by-product potassium hydroxide solution, and the solution is evenly dispersed through a homogenizing component. The solution is then processed with a vacuum pump and a heating mechanism to generate high-purity potassium fluoride.

Benefits of technology

The reaction efficiency of hydrofluoric acid and potassium hydroxide solution is improved, the contact area is increased, and the purity of potassium fluoride is ensured to reach more than 99%.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a method for synthesizing potassium fluoride by using by-product potassium hydroxide of organic fluorination reaction, and relates to the technical field of potassium fluoride, and comprises the following steps: adding hydrofluoric acid into the by-product potassium hydroxide solution; when the solution reaches neutral, continue adding the hydrofluoric acid, stop adding the hydrofluoric acid when the pH value of the solution reaches 3-5, and obtain the potassium fluoride solution; the potassium fluoride solution is evaporated and crystallized under reduced pressure to obtain the first solid potassium fluoride; the first solid potassium fluoride is calcined at a temperature of 500-700 DEG C for different lengths of time to obtain the second solid potassium fluoride. According to the method, the by-product can be reused, and the resource loss is reduced; through the cooperation between the vacuumizing mechanism and the heating mechanism, the evaporation efficiency of the potassium fluoride solution can be improved, and the purity of the generated potassium fluoride is higher.
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Description

Technical Field

[0001] The present invention relates to the technical field of potassium fluoride, and more particularly to a method for synthesizing potassium fluoride by utilizing potassium hydroxide produced as a by-product of an organic fluorination reaction. Background Art

[0002] With the development of science and technology, the status of organic fluorine chemicals in the chemical industry has been significantly improved. The production scale of various fluorine chemical products has increased year by year. The production scale of some products has already occupied an important position in the world. However, in terms of the overall production technology of organic fluorine chemicals, my country's overall technical level is still not very high. The level of comprehensive utilization of by-products is far behind the advanced level abroad, and the resulting environmental pollution problems are very obvious.

[0003] In the prior art, when hydrofluoric acid is added to the by-product potassium hydroxide solution, the dispersion effect of the hydrofluoric acid is poor, and the hydrofluoric acid cannot fully react with the potassium hydroxide solution, resulting in low reaction efficiency and low purity of the prepared potassium fluoride.

[0004] Therefore, it is necessary to propose a method for synthesizing potassium fluoride by utilizing potassium hydroxide produced as a by-product of an organic fluorination reaction to solve the above problems. Summary of the Invention

[0005] The present invention aims to solve the problems in the prior art of poor dispersion of hydrofluoric acid when it is added to a by-product potassium hydroxide solution, inability to fully react with the potassium hydroxide solution, low reaction efficiency, and low purity of potassium fluoride.

[0006] In order to achieve the above-mentioned purpose, the present invention specifically adopts the following technical solutions:

[0007] A method for synthesizing potassium fluoride from potassium hydroxide produced as a by-product of an organic fluorination reaction comprises the following steps:

[0008] Step 1: adding hydrofluoric acid to the by-product potassium hydroxide solution stored in the reaction cylinder by controlling the feeding mechanism to remove carbonate ions in the by-product potassium hydroxide solution to obtain a first solution;

[0009] Step 2: When the first solution reaches neutrality, continue to control the feeding mechanism to add hydrofluoric acid. When the pH value of the solution reaches between 3 and 5, stop adding hydrofluoric acid to generate a potassium fluoride solution;

[0010] Step 3: evacuating the gas in the reaction cylinder by a vacuum mechanism, and then controlling the heating mechanism to evaporate and crystallize the potassium fluoride solution in the reaction cylinder to obtain a first solid potassium fluoride;

[0011] Step 4: calcining the first solid potassium fluoride at a temperature of 500-700° C. for different lengths of time to obtain a second solid potassium fluoride with a purity of more than 99%.

[0012] Furthermore, the feeding mechanism includes a feeding component and a homogenization component, the feeding component includes a cylindrical barrel, an addition barrel and a liquid storage barrel, the cylindrical barrel is fixedly connected to the upper end of the reaction barrel, the addition barrel is fixedly connected to the inner side of the cylindrical barrel, the liquid storage barrel is fixedly connected to the upper end of the addition barrel, the upper end of the liquid storage barrel is provided with an opening for adding hydrofluoric acid, the lower end of the addition barrel is a discharge port for hydrofluoric acid, and the homogenization component is used to evenly disperse the hydrofluoric acid flowing out of the discharge port in the potassium hydroxide solution in the reaction barrel.

[0013] Furthermore, the homogenization assembly includes a driving mechanism, a rotating shaft, a plug, an umbrella-shaped plate and a dividing strip. A shaft connector for the rotating shaft to pass through is provided in the middle of the adding cylinder. The lower end of the rotating shaft passes through the bottom of the adding cylinder to the reaction cylinder. The umbrella-shaped plate is fixedly connected to the lower end of the rotating shaft. The driving mechanism is used to drive the rotating shaft to rotate and lift. The plug is fixedly connected to the middle of the rotating shaft. An adding hole for the plug to be plugged in is provided at the lower end of the adding cylinder. The dividing strip is evenly arranged along the upper side of the umbrella-shaped plate.

[0014] Furthermore, the driving mechanism includes a first driving assembly for driving the rotating shaft to rotate and a second driving assembly for driving the rotating shaft to rise and fall.

[0015] Furthermore, the second drive assembly includes a first electric push rod and a mounting plate, the first electric push rod is fixedly connected to the upper end of the reaction cylinder, the mounting plate is fixedly connected to the output end of the first electric push rod, and a shaft hole for rotating the mounting shaft is opened in the middle of the mounting plate.

[0016] Furthermore, the first driving assembly includes a driven gear, a motor and a driving gear, the driven gear is fixedly connected to the upper end of the rotating shaft, the motor is fixedly connected to the upper end of the mounting plate, the driving gear is fixedly connected to the output shaft of the motor, and the driving gear and the driven gear are meshed and connected.

[0017] Furthermore, a through hole is provided in the middle of the bottom of the reaction cylinder, an isolation cylinder is inserted into the through hole, the isolation cylinder is a hollow cylinder, the space between the outer side of the isolation cylinder and the reaction cylinder is used to store potassium hydroxide solution, the middle part of the isolation cylinder is used to install a heating mechanism, an annular limiting plate is provided at the bottom of the isolation cylinder, and two limiting handles are symmetrically connected to the bottom of the reaction cylinder on both sides of the limiting plate, and the upper end of the limiting handle is used to place the heating mechanism.

[0018] Furthermore, a slide groove is provided on the inner side surface of the isolation cylinder, a placement plate is slidably connected to the slide groove, a stabilizing ring is fixedly connected to the lower side surface of the umbrella-shaped plate, the outer side surface diameter of the stabilizing ring is equal to the inner side surface diameter of the isolation cylinder, and the lower end of the umbrella-shaped plate is symmetrically fixedly connected to a stirring plate extending into the potassium hydroxide solution storage space.

[0019] Furthermore, a plurality of support rods are fixedly connected to the lower end of the reaction cylinder, a second electric push rod with an output end facing downward is symmetrically fixedly connected to the outer side surface of the reaction cylinder, the output end of the second electric push rod is fixedly connected to a transmission rod, the end of the transmission rod away from the second electric push rod is fixedly connected to a right-angle plate, the upper end surface of the right-angle plate is fixedly connected to a positioning block, and the lower end of the annular limit plate is provided with a positioning groove for the positioning block to be inserted.

[0020] Furthermore, a plug-in rod is inserted into the side of the right-angle plate. When the two limit handles are rotated away from the hinged end with the reaction cylinder to the axis of the reaction cylinder, the limit handles and the transmission rod form a cross shape. A notch is provided at the lower end of the limit handle away from the hinged end. The two notches relatively form a space consistent with the width of the plug-in rod for the plug-in rod to be inserted.

[0021] Compared with the prior art, the present invention has the following beneficial effects:

[0022] 1. The present invention adopts a method of adding hydrofluoric acid to the by-product potassium hydroxide solution to prepare potassium fluoride, so that the by-product can be reused, reducing resource loss. The coordination between the vacuuming mechanism and the heating mechanism can improve the evaporation efficiency of the potassium fluoride solution, ensuring that the generated potassium fluoride has a higher purity.

[0023] 2. The present invention, through the provision of a homogenizing mechanism, can ensure that hydrofluoric acid can be fully added to the potassium hydroxide solution in the reaction cylinder during addition, thereby increasing the contact area between the hydrofluoric acid and the potassium hydroxide solution and thereby improving the reaction rate.

[0024] 3. The present invention, through the coordination among the second drive assembly, the addition hole, the rotating shaft and the plug, can adjust the distance between the addition hole and the plug by driving the second drive assembly, thereby controlling the feeding rate of hydrofluoric acid.

[0025] 4. The present invention, on the one hand, facilitates the installation and removal of the heating mechanism through the coordination between the limiting handle and the isolation tube, and on the other hand, can collect the first solid potassium fluoride in the reaction tube by controlling the descent of the isolation tube.

[0026] 5. In the present invention, the position of the placement plate can be adjusted by setting the chute and the placement plate. On the one hand, this does not affect the installation of the heating mechanism, and on the other hand, more first solid potassium fluoride can be stored in the isolation cylinder. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is a schematic diagram of the main view of the structure of the present invention;

[0028] Figure 2 It is a three-dimensional bottom view schematic diagram of the structure of the present invention;

[0029] Figure 3 It is a three-dimensional cross-sectional schematic diagram of the structure of the present invention;

[0030] Figure 4 It is a three-dimensional top view schematic diagram of the structure of the present invention;

[0031] Figure 5 This is a three-dimensional schematic diagram of the connection structure between the homogenizing assembly and the adding cylinder in the present invention;

[0032] Figure 6 It is a cross-sectional schematic diagram of the connection structure in the figure of the present invention;

[0033] Figure 7 For the present invention Figure 2 A in the middle is an enlarged schematic diagram;

[0034] Figure 8 For the present invention Figure 3 The enlarged schematic diagram of point B in the middle;

[0035] Figure 9 For the present invention Figure 3 Enlarged schematic diagram at point C in the middle;

[0036] Figure 10 For the present invention Figure 3 Enlarged schematic diagram at point D in the middle.

[0037] Figure numerals: 1. reaction cylinder; 2. cylindrical cylinder; 3. adding cylinder; 4. liquid storage cylinder; 5. shaft connecting part; 6. first electric push rod; 7. mounting plate; 8. rotating shaft; 9. driven gear; 10. motor; 11. driving gear; 12. umbrella-shaped plate; 13. dividing strip; 14. plug; 15. adding hole; 16. stirring plate; 17. stabilizing ring; 18. isolation cylinder; 19. slide; 20. placement plate; 21. thermal insulation pad; 22. tubular heating furnace; 23. limiting handle; 24. second electric push rod; 25. transmission rod; 26. positioning block; 27. plug rod; 28. support rod; 29. ​​vacuum tube; 30. vacuum pump. DETAILED DESCRIPTION

[0038] With reference to the drawings of the embodiments of the present application, the technical solutions in the embodiments of the present application will be clearly and completely described. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments of the present application, all the other embodiments obtained by a person of ordinary skill in the art without creative work fall within the protection scope of the present application.

[0039] Please refer to Figure 1-10 A method for synthesizing potassium fluoride by using by-product potassium hydroxide of organic fluorination reaction, comprising the following steps:

[0040] Step one, by controlling the feeding mechanism to add hydrofluoric acid to the by-product potassium hydroxide solution stored in the reaction cylinder 1, remove carbonate ions in the by-product potassium hydroxide solution, and obtain a first solution;

[0041] Step two, when the first solution reaches neutral, continue to control the feeding mechanism to add hydrofluoric acid, and stop adding hydrofluoric acid when the pH value of the solution reaches between 3-5, to generate a potassium fluoride solution;

[0042] Step three, by the vacuum pumping mechanism, the gas in the reaction cylinder 1 is pumped out, and then the heating mechanism is controlled to evaporate and crystallize the potassium fluoride solution in the reaction cylinder 1, to obtain a first solid potassium fluoride, wherein the vacuum pumping mechanism is a vacuum pump 30, the gas inlet of the vacuum pump 30 is connected to the reaction cylinder 1 through a vacuum pipe 29, and the heating mechanism is a tubular heating furnace 22, but is not limited to the heating furnace;

[0043] Step four, the first solid potassium fluoride is calcined at a temperature of 500-700℃ for different lengths of time, to obtain a second solid potassium fluoride with a purity of more than 99%, and when the calcination temperature is 650℃ and the calcination time is 20 min, the prepared second solid potassium fluoride has a higher purity.

[0044] In the embodiment, by using the method of adding hydrofluoric acid to the by-product potassium hydroxide solution to prepare potassium fluoride, the by-product can be reused, and resource loss is reduced. By the cooperation between the vacuum pumping mechanism and the heating mechanism, the evaporation efficiency of the potassium fluoride solution can be improved, and the purity of the generated potassium fluoride is higher.

[0045] Specifically, in combination with Figure 1-4 the feeding mechanism includes a feeding assembly and a homogenizing assembly. The feeding assembly includes a cylindrical barrel 2, an adding barrel 3, and a liquid storage barrel 4. The shape of the liquid storage barrel 4 is not limited to Figure 1-6In the shape shown in the figure, the cylindrical barrel 2 is fixedly connected to the upper end of the reaction barrel 1, the adding barrel 3 is fixedly connected to the inner side of the cylindrical barrel 2, the liquid storage barrel 4 is fixedly connected to the upper end of the adding barrel 3, and the upper end of the liquid storage barrel 4 is provided with an opening for adding hydrofluoric acid. The lower end of the adding barrel 3 is a discharge port for hydrofluoric acid, and the homogenizing component is used to uniformly disperse the hydrofluoric acid flowing out of the discharge port in the potassium hydroxide solution in the reaction barrel 1.

[0046] Specific, combined Figure 5 and Figure 6 As shown, the homogenization assembly includes a driving mechanism, a rotating shaft 8, a plug 14, an umbrella plate 12 and a dividing strip 13. A shaft connector 5 for the rotating shaft 8 to pass through is provided in the middle of the adding cylinder 3. At the same time, the inner wall of the shaft connector 5 must also fit the outer wall of the rotating shaft 8. The purpose is to provide stability to the rotating shaft 8 on the one hand, and to reduce the contact area between the rotating shaft 8 and the solution in the adding cylinder 3 on the other hand, thereby reducing the occurrence of adhesion. The lower end of the rotating shaft 8 passes through the bottom of the adding cylinder 3 to the reaction cylinder 1, and the umbrella plate 12 is fixedly connected to the lower end of the rotating shaft 8. The driving mechanism is used to drive the rotating shaft 8 to rotate and lift. The head 14 is fixedly connected to the middle part of the rotating shaft 8, and an adding hole 15 for plugging the plug 14 is opened at the lower end of the adding cylinder 3. The fitting surface of the adding hole 15 and the plug 14 fits tightly, and the adding hole 15 is conical, matching the cross-sectional shape of the plug 14. As the rotating shaft 8 moves downward, the distance between the plug 14 and the adding hole 15 gradually increases, which is used to control the feeding rate of hydrofluoric acid. The dividing strips 13 are evenly arranged along the upper side of the umbrella plate 12, and the umbrella plate 12 and the dividing strips 13 are coated with a lubricating layer to ensure that the solution does not adhere to the umbrella plate 12 and the dividing strips 13.

[0047] Specific, combined Figure 5 and Figure 6 As shown, the driving mechanism includes a first driving assembly for driving the rotating shaft 8 to rotate and a second driving assembly for driving the rotating shaft 8 to lift. The second driving assembly includes a first electric push rod 6 and a mounting plate 7. The first electric push rod 6 is fixedly connected to the upper end of the reaction cylinder 1. The mounting plate 7 is fixedly connected to the output end of the first electric push rod 6, and the middle of the mounting plate 7 is provided with an axial hole for rotating the rotating shaft 8. When the attached Figure 1-6 When the liquid storage cylinder 4 is shown in the figure, the mounting plate 7 is located in the gap in the middle of the liquid storage cylinder 4, and the gap can meet the lifting range required by the rotating shaft 8.

[0048] Specific, combined Figure 1-4As shown, the first drive assembly includes a driven gear 9, a motor 10 and a driving gear 11, the driven gear 9 is fixedly connected to the upper end of the rotating shaft 8, the motor 10 is fixedly connected to the upper end of the mounting plate 7, the driving gear 11 is fixedly connected to the output shaft of the motor 10, and the driving gear 11 and the driven gear 9 are meshed and connected. By controlling the start of the motor 10, the rotation of the rotating shaft 8 is driven by the transmission of the driving gear 11 and the driven gear 9. Since the first drive assembly is arranged on the mounting plate 7, the gap of the liquid storage cylinder 4 must also meet the range in which the first drive assembly can move up and down.

[0049] Specific, combined Figure 2 and Figure 3 As shown, the middle of the bottom of the reaction tube 1 is set as a through hole, and the isolation tube 18 is inserted into the through hole. In order to further ensure the sealing effect, a sealing gasket can be set at the position where the isolation tube 18 fits the through hole, but this setting will increase the friction between the isolation tube 18 and the reaction tube 1, and human assistance is required when removing the isolation tube 18. The isolation tube 18 is a hollow tube, and the space between the outer side of the isolation tube 18 and the reaction tube 1 is used to store potassium hydroxide solution. The middle part of the isolation tube 18 is used to install a heating mechanism. An annular limit plate is provided at the bottom of the isolation tube 18. The bottom of the reaction tube 1 on both sides of the limit plate is symmetrically connected to two limit handles 23, and the upper end of the limit handle 23 is used to place a tubular heating furnace 22. In order to prevent the tubular heating furnace 22 from being scalded, an insulation pad 21 is provided at the lower end of the tubular heating furnace 22. A wire hole is opened on the insulation pad to facilitate the wiring on the tubular heating furnace 22 to pass through.

[0050] Specific, combined Figure 3-9 As shown, a chute 19 is provided on the inner side of the isolation cylinder 18, and a placement plate 20 is slidably connected in the chute 19. The placement plate 20 and the chute 19 fit tightly together to prevent the first solid potassium fluoride from falling from the gap. A stabilizing ring 17 is fixedly connected to the lower side of the umbrella-shaped plate 12. The outer diameter of the stabilizing ring 17 is equal to the inner diameter of the isolation cylinder 18. The setting of the stabilizing ring 17 can ensure that the umbrella-shaped plate 12 is more stable when it is driven to rotate. At the same time, when the first electric push rod 6 is extended to the upper limit, the bottom of the stabilizing ring 17 just comes out of the upper limit. The upper end of the isolation cylinder 18 is moved out, and when the first electric push rod 6 is extended to the lower limit, the lower end of the stabilizing ring 17 does not interfere with the movement of the placement plate 20. The lower end of the umbrella plate 12 is symmetrically fixedly connected with a stirring plate 16 extending into the storage space of the potassium hydroxide solution. By adopting the cooperation of the stirring plate 16 and the homogenizing mechanism, potassium hydroxide and hydrofluoric acid can be fully contacted and reacted. In addition, the bottom of the reaction cylinder 1 is set to an inclined surface facing the center of the reaction cylinder 1, and the bottom of the stirring plate 16 matches the inclined surface, thereby promoting the sliding of the first solid potassium fluoride.

[0051] Specific, combined Figure 2 and Figure 9As shown, the lower end of the reaction tube 1 is fixedly connected to a plurality of support rods 28, and the outer side surface of the reaction tube 1 is symmetrically fixedly connected to a second electric push rod 24 with the output end facing downward, the height of the support rod 28 is greater than the maximum extension stroke of the second electric push rod 24, the output end of the second electric push rod 24 is fixedly connected to a transmission rod 25, and the end of the transmission rod 25 away from the second electric push rod 24 is fixedly connected to a right-angle plate, the horizontal plate of the right-angle plate is on the top, and the vertical plate is on the bottom, and the upper end surface of the horizontal plate of the right-angle plate is fixedly connected to a positioning block 26, and the lower end of the annular limit plate is provided with a positioning groove for the positioning block 26 to be inserted. Through the cooperation of the positioning block 26 and the positioning groove, the isolation tube 18 can be positioned in advance before installation.

[0052] Specific, combined Figure 1 、 Figure 7 and Figure 9 As shown, a plug-in rod 27 is inserted into the side surface of the longitudinal plate of the right-angle plate. When the two limit handles 23 are rotated away from the hinged end with the reaction cylinder 1 to the axis of the reaction cylinder 1, the limit handles 23 and the transmission rod 25 form a cross shape, which can ensure that the limit handles 23 will not interfere with the transmission rod 25 when rotating. A notch is provided at the lower end of the limit handle 23 away from the hinged end. The two notches relatively form a space consistent with the width of the plug-in rod 27 for the plug-in rod 27 to be inserted. When the plug-in rod 27 is inserted into the space, the side surface of the plug-in rod 27 will fit into the notch, and under the restriction of the plug-in rod 27, the rotation of the limit handle 23 is avoided.

[0053] The first electric push rod 6, the motor 10, the tubular heating furnace 22, the vacuum pump 30 and the second electric push rod 24 are all controlled by an industrial computer.

[0054] Working principle: First, when using, follow Figure 3 The state in is described, the by-product potassium hydroxide solution is introduced into the reaction tube 1 through the upper end of the liquid storage cylinder 4. After the introduction is completed, the first electric push rod 6 is controlled by the industrial computer to extend, so that the first electric push rod 6 drives the mounting plate 7 to rise, and then drives the rotating shaft 8 to move upward, so that the plug 14 enters the addition hole 15, and then the motor 10 is controlled by the industrial computer to rotate, so that the driving gear 11 drives the driven gear 9 to rotate, and then drives the rotating shaft 8 to rotate, and the potassium hydroxide solution on the umbrella plate 12 is thrown into the reaction tube 1, and then the hydrofluoric acid is poured into the liquid storage cylinder 4, so that the hydrofluoric acid is stored in the liquid storage cylinder 4 and the addition cylinder 3;

[0055] When it is necessary to add hydrofluoric acid to the potassium hydroxide solution, the stroke of the first electric push rod 6 retraction is controlled by the industrial computer, and the motor 10 is started by the industrial computer, thereby driving the plug 14 to move down a certain distance from the addition hole 15, driving the rotating shaft 8 to rotate, thereby changing the feeding rate of the hydrofluoric acid. After the first electric push rod 6 stops retracting, the lower end of the stabilizing ring 17 extends into the isolation cylinder 18. As the rotating shaft 8 rotates, when the hydrofluoric acid is discharged along the addition hole 15, it falls into the gap between the dividing strips 13. As the umbrella plate 12 rotates, the hydrofluoric acid can be driven to disperse in the reaction cylinder 1, so that the hydrofluoric acid is fully dispersed in the potassium hydroxide solution, and the carbonate ions in the by-product potassium hydroxide solution are removed to obtain the first solution. When the first solution reaches neutrality, the feeding mechanism is continued to be controlled to add hydrofluoric acid. When the pH value of the solution reaches between 3 and 5, the addition of hydrofluoric acid is stopped to generate a potassium fluoride solution.

[0056] Then, the industrial computer controls the vacuum pump 30 to evacuate the gas in the reaction tube 1, so that the reaction tube 1 is in a negative pressure state, and then controls the heating mechanism to start, evaporates and crystallizes the potassium fluoride solution in the reaction tube 1, and produces the first solid potassium fluoride;

[0057] Then, after the heating is completed, first, the plug rod 27 is pulled out, and after it is pulled out, the limit handle 23 can be rotated to remove the tubular heating furnace 22 installed on the insulation pad 21 from the isolation tube 18. As the tubular heating furnace 22 is taken out, the placement plate 20 will slide down along the slide 19. After the tubular heating furnace 22 is taken out, the extension of the second electric push rod 24 is controlled by the industrial computer to drive the transmission rod 25 to move downward. At this time, the isolation tube 18 moves downward. When the uppermost end of the isolation tube 18 is lower than the height of the first solid potassium fluoride in the reaction tube 1, the first solid potassium fluoride will fall into the isolation tube 18. At the same time, in order to ensure the first solid potassium fluoride is dropped, the start of the motor 10 can be controlled to drive the stirring plate 16 to push the first solid potassium fluoride into the isolation tube 18, thereby completing the collection of the first solid potassium fluoride.

[0058] After the material is taken out, the first solid potassium fluoride in the isolation cylinder 18 is transferred to a roasting device for roasting to obtain a second solid potassium fluoride with a purity of more than 99%.

[0059] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. The scope of patent protection of the present invention shall be based on the claims. Any equivalent structural changes made using the description and drawings of the present invention should also be included in the scope of protection of the present invention.

Claims

1. A method for synthesizing potassium fluoride using potassium hydroxide as a by-product of an organic fluorination reaction, characterized in that: The following steps are involved: Step 1: adding hydrofluoric acid to the by-product potassium hydroxide solution stored in the reaction cylinder by controlling the feeding mechanism to remove carbonate ions in the by-product potassium hydroxide solution to obtain a first solution; Step 2: When the first solution reaches neutrality, continue to control the feeding mechanism to add hydrofluoric acid. When the pH value of the solution reaches between 3 and 5, stop adding hydrofluoric acid to generate a potassium fluoride solution; Step 3: evacuating the gas in the reaction cylinder by a vacuum mechanism, and then controlling the heating mechanism to evaporate and crystallize the potassium fluoride solution in the reaction cylinder to obtain a first solid potassium fluoride; Step 4: calcining the first solid potassium fluoride at a temperature of 500-700° C. for different lengths of time to obtain a second solid potassium fluoride with a purity of more than 99%; The feeding mechanism includes a feeding assembly and a homogenizing assembly, the feeding assembly includes a cylindrical barrel, an adding barrel and a liquid storage barrel, the cylindrical barrel is fixedly connected to the upper end of the reaction barrel, the adding barrel is fixedly connected to the inner side of the cylindrical barrel, the liquid storage barrel is fixedly connected to the upper end of the adding barrel, the upper end of the liquid storage barrel is provided with an opening for adding hydrofluoric acid, the lower end of the adding barrel is a discharge port for hydrofluoric acid, and the homogenizing assembly is used to uniformly disperse the hydrofluoric acid flowing out of the discharge port in the potassium hydroxide solution in the reaction barrel; The homogenization assembly includes a driving mechanism, a rotating shaft, a plug, an umbrella-shaped plate and a dividing strip. A shaft connector for the rotating shaft to pass through is provided in the middle of the adding cylinder. The lower end of the rotating shaft passes through the bottom of the adding cylinder to the reaction cylinder. The umbrella-shaped plate is fixedly connected to the lower end of the rotating shaft. The driving mechanism is used to drive the rotating shaft to rotate and lift. The plug is fixedly connected to the middle of the rotating shaft. An adding hole for the plug to be plugged in is provided at the lower end of the adding cylinder. The dividing strips are evenly arranged along the upper side of the umbrella-shaped plate.

2. The method for synthesizing potassium fluoride from potassium hydroxide produced as a by-product of an organic fluorination reaction according to claim 1, wherein: The driving mechanism includes a first driving assembly for driving the rotating shaft to rotate and a second driving assembly for driving the rotating shaft to rise and fall.

3. The method for synthesizing potassium fluoride from potassium hydroxide produced as a by-product of an organic fluorination reaction according to claim 2, wherein: The second driving assembly includes a first electric push rod and a mounting plate. The first electric push rod is fixedly connected to the upper end of the reaction cylinder. The mounting plate is fixedly connected to the output end of the first electric push rod, and a shaft hole for rotating the mounting shaft is opened in the middle of the mounting plate.

4. The method for synthesizing potassium fluoride from potassium hydroxide produced as a by-product of an organic fluorination reaction according to claim 3, wherein: The first driving assembly includes a driven gear, a motor and a driving gear, the driven gear is fixedly connected to the upper end of the rotating shaft, the motor is fixedly connected to the upper end of the mounting plate, the driving gear is fixedly connected to the output shaft of the motor, and the driving gear and the driven gear are meshed and connected.

5. The method for synthesizing potassium fluoride from potassium hydroxide produced as a by-product of an organic fluorination reaction according to claim 4, wherein: A through hole is provided in the middle of the bottom of the reaction cylinder, and an isolation cylinder is inserted into the through hole. The isolation cylinder is a hollow cylinder. The space between the outer side of the isolation cylinder and the reaction cylinder is used to store potassium hydroxide solution. The middle part of the isolation cylinder is used to install a heating mechanism. An annular limiting plate is provided at the bottom of the isolation cylinder. Two limiting handles are symmetrically connected to the bottom of the reaction cylinder on both sides of the limiting plate, and the upper end of the limiting handle is used to place the heating mechanism.

6. The method for synthesizing potassium fluoride from potassium hydroxide produced as a by-product of an organic fluorination reaction according to claim 5, wherein: A chute is provided on the inner side of the isolation cylinder, a placement plate is slidably connected to the chute, a stabilizing ring is fixedly connected to the lower side of the umbrella-shaped plate, the outer side diameter of the stabilizing ring is equal to the inner side diameter of the isolation cylinder, and the lower end of the umbrella-shaped plate is symmetrically fixedly connected to a stirring plate extending into the potassium hydroxide solution storage space.

7. The method for synthesizing potassium fluoride from potassium hydroxide produced as a by-product of an organic fluorination reaction according to claim 6, wherein: A plurality of support rods are fixedly connected to the lower end of the reaction cylinder, a second electric push rod with an output end facing downward is symmetrically fixedly connected to the outer side of the reaction cylinder, the output end of the second electric push rod is fixedly connected to a transmission rod, an end of the transmission rod away from the second electric push rod is fixedly connected to a right-angle plate, a positioning block is fixedly connected to the upper end surface of the right-angle plate, and a positioning groove for the positioning block to be inserted is provided at the lower end of the annular limit plate.

8. The method for synthesizing potassium fluoride from potassium hydroxide produced as a by-product of an organic fluorination reaction according to claim 7, wherein: A plug-in rod is inserted into the side of the right-angle plate. When the two limit handles are rotated away from the hinged end with the reaction cylinder to the axis of the reaction cylinder, the limit handles and the transmission rod form a cross shape. A notch is provided at the lower end of the limit handle away from the hinged end. The two notches form a space consistent with the width of the plug-in rod for the plug-in rod to be inserted.

Citation Information

Patent Citations

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