A crude sulfur tower with regulating function for preparing hydrogen fluoride

Abstract

A crude sulfur column with regulating function for preparing hydrogen fluoride relates to a crude distillation column, a round hole (11) is arranged at the center of each plane tray (10), a plurality of liquid leakage holes A (12) are arranged around the round hole (11) of each plane tray (10), a silica gel material elastic tray is arranged between the plurality of supporting rings (25) and the slide bar (9), and a plurality of liquid leakage holes B (26) are arranged around the inner edge of each elastic tray; the silica gel material elastic tray is arranged between the interval arranged plane trays, the elastic tray is driven by the slide bar to form a tapered pipe tray with an expanding end at the lower end and a narrowing end at the upper end or an expanding end at the upper end and a narrowing end at the lower end, and the purpose of more thorough separation of the gas phase rising when the overhead product is too much and the liquid phase descending when the bottom product is too much is achieved.

Description

Technical Field

[0001] This invention relates to a crude distillation column, and more particularly to a crude sulfur column with conditioning function for the preparation of hydrogen fluoride. Background Technology

[0002] After drying and pulverizing, fluorite is mixed with 98% concentrated sulfuric acid and 105% fuming sulfuric acid in a certain proportion and then fed into a rotary kiln for reaction. The calcium sulfate produced by the reaction is discharged from the tail of the furnace, while the gas mixture produced by the reaction is discharged from the head of the furnace and enters the crude distillation column to remove most of the impurities such as sulfuric acid, water vapor, calcium sulfate, and fluorite dust. The remaining furnace gas, containing HF, SiF4, H2S, SO2, and small amounts of H2SO4 and H2O, enters the crude cooler for further cooling of the hydrogen fluoride gas. During the crude distillation in the column, the bottom temperature is controlled at 100-110℃ and the top temperature is controlled at 35-40℃. Because the proportions of each component in the gas mixture containing impurities entering the crude distillation column are not exactly the same from batch to batch, and the original plate structure of the crude sulfur column does not have an adjustment function, the separation of the top and bottom products during crude distillation is prone to incomplete separation when the feed ratio is different. Summary of the Invention

[0003] To overcome the shortcomings of the prior art, this invention discloses a crude sulfur tower with regulating function for preparing hydrogen fluoride. By setting elastic trays made of silicone between spaced planar trays, the elastic trays are driven by a sliding rod to form a conical tray with the expanding neck end at the bottom and the constricted neck end at the top or vice versa. This achieves the purpose of accelerating the rise of the gas phase when there is too much product at the top of the tower and accelerating the descent of the liquid phase when there is too much product at the bottom of the tower, thus achieving more thorough separation.

[0004] To achieve the aforementioned objective, the present invention employs the following technical solution:

[0005] A crude sulfur tower with regulating function for preparing hydrogen fluoride includes a tower body with a cavity inside. Multiple horizontally arranged planar trays, their outer edges fixed to the sidewalls of the cavity, are spaced apart in the middle of the cavity. Each planar tray has a central hole, and multiple drainage holes A are arranged around the hole on each tray. Horizontally arranged support rings are uniformly positioned between each pair of adjacent planar trays. The diameter of the support rings is larger than the diameter of the hole but smaller than the diameter of the cavity's cross-section. Multiple support rings are fixed to the sidewalls of the cavity via support rods. The middle section of a sliding rod passes through the multiple holes. Elastic towers made of silicone are positioned between the support rings and the sliding rods. Each flexible tray has multiple drain holes B spaced around its inner edge. When the flexible tray is not subjected to external force, it forms a planar disc tray. When the slide bar rises, the flexible tray forms a conical tray A with the expanded neck end at the bottom and the contracted neck end at the top. A conical cavity A is provided inside the conical tray A. The upper end of the conical tray A is located at the center of the circular hole provided in the planar tray above. When the slide bar falls, the flexible tray forms a conical tray B with the expanded neck end at the top and the contracted neck end at the bottom. The inner wall of the conical tray A forms the outer wall of the conical tray B. A conical cavity B is provided inside the conical tray B. The lower end of the conical tray B is located at the center of the circular hole provided in the planar tray below.

[0006] The crude sulfur tower for preparing hydrogen fluoride with regulating function has a collar A coaxial with the circular hole above the uppermost flat tray and a collar B coaxial with the circular hole below the lowermost flat tray. The diameter of collar A is smaller than the diameter of the circular hole and equal to the diameter of the sliding rod. The diameter of collar B is the same as that of collar A. The upper part of the sliding rod is slidably connected inside collar A, and the lower part of the sliding rod is slidably connected inside collar B.

[0007] The crude sulfur tower for preparing hydrogen fluoride with regulating function has multiple connecting rods A arranged around the collar A between the collar A and the side wall of the cavity, and multiple connecting rods B arranged around the collar B between the collar B and the side wall of the cavity.

[0008] The crude sulfur tower for preparing hydrogen fluoride with regulating function has multiple teeth spaced apart on a sliding rod located above the collar A. The motor is located outside the tower body, and its rotating shaft extends into the cavity. A gear is sleeved on the rotating shaft located in the cavity. The gear and teeth mesh. The rotation of the motor can drive the sliding rod to move up and down. When the gear is located at the lower part of the multiple teeth, the elastic tray forms a conical tray A. When the gear is located at the upper part of the multiple teeth, the elastic tray forms a conical tray B.

[0009] The crude sulfur tower for preparing hydrogen fluoride with regulating function has a bearing seat on the side wall of the cavity opposite to the motor. The end of the rotating shaft is rotatably sleeved in the shaft hole provided in the bearing seat. A shell is fixed to the outer wall of the tower body and covers the motor.

[0010] The crude sulfur tower with regulating function used to prepare hydrogen fluoride is equipped with a forward and reverse servo motor.

[0011] The crude sulfur tower with regulating function for preparing hydrogen fluoride has one end of the tower body connected to the top gas outlet pipe at the top, and the other end of the top gas outlet pipe connected to one end of the top reflux pipe and the top discharge pipe, respectively. A condenser is provided on the top gas outlet pipe, and the other end of the top reflux pipe is connected to the tower body above the uppermost flat tray.

[0012] The crude sulfur tower for preparing hydrogen fluoride with regulating function has one end of the bottom outlet pipe connected to the lower end of the tower body, and the other end of the bottom outlet pipe connected to one end of the bottom collection pipe and the bottom reflux pipe respectively. A reboiler 16 is provided on the bottom reflux pipe, and the other end of the bottom reflux pipe is connected to the tower body located below the lowest flat tray.

[0013] The crude sulfur tower for preparing hydrogen fluoride with regulating function has a feed pipe on the tower body located in the lower part of multiple planar trays.

[0014] Due to the adoption of the above technical solution, the present invention has the following beneficial effects:

[0015] The crude sulfur tower for preparing hydrogen fluoride with regulating function described in this invention uses elastic silica gel trays placed between spaced planar trays. These elastic trays, driven by sliding rods, form conical trays with either the expanding neck at the bottom and the contracted neck at the top, or vice versa. This achieves more thorough separation by accelerating the rise of the gas phase when there is excessive material at the top of the tower and accelerating the descent of the liquid phase when there is excessive material at the bottom. This invention features a simple structure, energy saving, and reduced consumption. The elastic silica gel trays are not easily damaged by heat at tower temperatures of 160-180 degrees Celsius and exhibit excellent elasticity, effectively improving separation accuracy and possessing strong potential for widespread application. Attached Figure Description

[0016] Figure 1 This is a schematic diagram of the structure of the elastic tray of the present invention when it is formed into a disc tray;

[0017] Figure 2 This is a schematic diagram of the structure of the elastic tray of the present invention when forming a tapered tray A;

[0018] Figure 3 This is a schematic diagram of the structure of the conical tray A and the planar tray of the present invention when they are combined;

[0019] Figure 4 This is a schematic diagram of the structure of the elastic tray of the present invention when forming the tapered tray B;

[0020] Figure 5 For the present invention Figure 2 A magnified structural diagram of point A in the middle.

[0021] In the diagram: 1. Top outlet pipe; 2. Condenser; 3. Top discharge pipe; 4. Top reflux pipe; 5. Tooth; 6. Gear; 7. Shaft seat; 8. Rotating shaft; 9. Sliding rod; 10. Flat tray; 11. Circular hole; 12. Drain hole A; 13. Tower body; 14. Cavity; 15. Bottom reflux pipe; 16. Bottom reboiler; 17. Bottom outlet pipe; 18. Shell; 19. Motor; 20. Connecting rod A; 21. Collar A; 22. Support rod; 23. Circular tray; 24. Feed pipe; 25. Support ring; 26. Drain hole B; 27. Connecting rod B; 28. Collar B; 29. ​​Bottom outlet pipe; 30. Conical tray A; 31. Conical cavity A; 32. Conical cavity B; 33. Conical tray B. Detailed Implementation

[0022] The present invention can be explained in more detail through the following embodiments. The present invention is not limited to the following embodiments. The purpose of disclosing the present invention is to protect all changes and modifications within the scope of the present invention.

[0023] Combined with appendix Figures 1-5The crude sulfur tower for preparing hydrogen fluoride with regulating function includes a tower body 13, a cavity 14 inside the tower body 13, and multiple horizontally arranged planar trays 10 spaced apart in the middle of the cavity 14, with their outer edges fixed to the side walls of the cavity 14. Each planar tray 10 has a circular hole 11 at its center, and multiple leakage holes A12 are arranged around the circular hole 11 on each planar tray 10. Horizontally arranged support rings 25 are evenly arranged between each pair of adjacent planar trays 10. The diameter of the support rings 25 is larger than the diameter of the circular hole 11 but smaller than the diameter of the cross-section of the cavity 14. Multiple support rings 25 are fixed to the side walls of the cavity 14 by support rods 22. The middle section of a sliding rod 9 passes through multiple circular holes 11. Silicon is disposed between the multiple support rings 25 and the sliding rod 9. The elastic trays made of rubber have multiple leakage holes B26 spaced around their inner edges. When the elastic trays are not subjected to external force, they form a planar disc tray 23. When the slide bar 9 rises, the elastic trays form a conical tray A30 with the expanding neck end at the bottom and the contracting neck end at the top. A conical cavity A31 is provided inside the conical tray A30, and the upper end of the conical tray A30 is located at the center of the circular hole 11 provided in the upper planar tray 10. When the slide bar 9 falls, the elastic trays form a conical tray B33 with the expanding neck end at the top and the contracting neck end at the bottom. The inner wall of the conical tray A30 forms the outer wall of the conical tray B33, and a conical cavity B32 is provided inside the conical tray B33. The lower end of the conical tray B33 is located at the center of the circular hole 11 provided in the lower planar tray 10. Positioned above the uppermost planar tray 10, a collar A21 coaxial with the circular hole 11 is provided. Below the lowermost planar tray 10, a collar B28 coaxial with the circular hole 11 is provided. The diameter of collar A21 is smaller than the diameter of the circular hole 11 and equal to the diameter of the sliding rod 9. The diameter of collar B28 is the same as that of collar A21. The upper part of the sliding rod 9 is slidably connected inside collar A21, and the lower part of the sliding rod 9 is slidably connected inside collar B28. Multiple connecting rods A20 are provided around collar A21 between collar A21 and the side wall of cavity 14. Multiple connecting rods B27 are provided around collar B28 between collar B28 and the side wall of cavity 14. Multiple teeth 5 are spaced apart on the sliding rod 9 located above collar A21. The motor 19 is located outside the tower body 13 and has... A rotating shaft 8 extends into the cavity 14. A gear 6 is fitted onto the rotating shaft 8 located inside the cavity 14. The gear 6 meshes with the teeth 5. The rotation of the motor 19 can drive the slide rod 9 to move up and down. When the gear 6 is located at the lower part of the teeth 5, the elastic tray forms a conical tray A30. When the gear 6 is located at the upper part of the teeth 5, the elastic tray forms a conical tray B33. A bearing seat 7 is provided on the side wall of the cavity 14 opposite to the motor 19. The end of the rotating shaft 8 is rotatably fitted into the shaft hole provided in the bearing seat 7. A housing 18 is fixed to the outer wall of the tower body 13 and covers the motor 19. The motor 19 is a forward and reverse servo motor. The upper end of the tower body 13 is connected to one end of the tower top outlet pipe 1. The other end of the tower top outlet pipe 1 is connected to one end of the tower top return pipe 4 and the tower top discharge pipe 3, respectively.A condenser 2 is installed on the top outlet pipe 1. The other end of the top reflux pipe 4 is connected to the column body 13 above the uppermost flat tray 10. The lower end of the column body 13 is connected to one end of the bottom liquid outlet pipe 29. The other end of the bottom liquid outlet pipe 29 is connected to one end of the bottom collection pipe 17 and one end of the bottom reflux pipe 15. A reboiler 16 is installed on the bottom reflux pipe 15. The other end of the bottom reflux pipe 15 is connected to the column body 13 below the lowermost flat tray 10. A feed pipe 24 is installed on the column body 13 located in the lower part of the multiple flat trays 10.

[0024] To implement the crude sulfur tower with regulating function for preparing hydrogen fluoride as described in this invention, the condenser 2, motor 19, and reboiler 16 are respectively connected to a switch and a power supply. The gas mixture generated by the reaction of fluorite powder and concentrated sulfuric acid in the rotary kiln flows out of the rotary kiln at a temperature of 160-180°C. The gas mixture enters the middle and lower part of the multiple planar trays 10 provided in the tower body 13 along the feed pipe 24. The condenser 2 and reboiler 16 are turned on.

[0025] When the proportions of the lighter component (hydrogen fluoride gaseous mixture) and the heavier component (sulfuric acid impurity mixture) in the gas mixture are sampled and tested before entering tower 13 and reach the preset normal values: (in conjunction with the attached...) Figure 1 The flexible tray, forming a planar structure, is a circular tray 23. In this gas mixture, the lighter hydrogen fluoride gaseous mixture rises, while the heavier sulfuric acid impurity liquid mixture descends. The labyrinth structure formed by the outer space between the circular tray 23 and the inner wall of the tower body 13, and the inner space of the planar tray 10 with its circular holes 11, facilitates the ascent of the hydrogen fluoride gaseous mixture. The multiple drain holes A12 on the planar tray 10, the edges of the circular holes 11 on the planar tray 10, the multiple drain holes B26 near the inner edge of the circular tray 23, and the outer edge of the circular tray 23 facilitate the descent of the sulfuric acid impurity liquid mixture. The hydrogen fluoride gaseous mixture and the descending liquid phase come into contact and separate, reaching the top of the column. It is then led out through the top outlet pipe 1 and condensed by the top condenser 2. Part of the hydrogen fluoride gaseous mixture is collected as the top product through the top outlet pipe 3, and part of the hydrogen fluoride gaseous mixture is returned to the column as top reflux through the top reflux pipe 4. The descending sulfuric acid impurity liquid mixture and the rising gas phase come into contact and separate, reaching the bottom of the column. It is led out through the bottom liquid outlet pipe 29. Part of the sulfuric acid impurity liquid mixture is collected as the bottom product through the bottom outlet pipe 17, and part of the sulfuric acid impurity liquid mixture is heated by the bottom reboiler 16 and turned into a gas phase, returning to the column through the bottom reflux pipe 15.

[0026] When the gas mixture entering tower 13 is sampled and tested, and the proportion of the heavier sulfuric acid impurity mixture is greater than the preset normal value, in order to facilitate the descent of the heavier sulfuric acid impurity mixture: (in conjunction with the attached...) Figure 2As the slide bar 9 rises, the elastic tray forms a conical tray A30 with the expanding neck at the bottom and the contracting neck at the top. A conical cavity A31 is provided within the conical tray A30. The upper end of the conical tray A30 is located at the center of the circular hole 11 provided in the upper planar tray 10. The lighter hydrogen fluoride gaseous mixture in the gas mixture rises, while the heavier sulfuric acid impurity liquid mixture in the gas mixture descends. Because the elastic tray forms a conical tray A30 with the expanding neck at the bottom and the contracting neck at the top, the lighter gaseous mixture is obstructed by the conical tray A30 as it rises. The gaseous mixture collected in the conical cavity A31 can only rise slowly through multiple drain holes B26 located near the inner edge of the conical tray A30. Therefore, the liquid phase mixed in the gas phase is more easily... The sulfuric acid impurity liquid mixture is easily separated from the gas phase, so the precipitation of the liquid phase sulfuric acid impurity liquid mixture is more thorough. After the rising hydrogen fluoride gas mixture and the falling liquid phase come into contact and separate, they reach the top of the column and are led out by the top outlet pipe 1. After being condensed by the top condenser 2, part of the hydrogen fluoride gas mixture is collected as the top product through the top outlet pipe 3, and part of the hydrogen fluoride gas mixture is returned to the column as the top reflux through the top reflux pipe 4. After the falling sulfuric acid impurity liquid mixture and the rising gas phase come into contact and separate, they reach the bottom of the column and are led out by the bottom liquid outlet pipe 29. Part of the sulfuric acid impurity liquid mixture is collected as the bottom product through the bottom outlet pipe 17, and part of the sulfuric acid impurity liquid mixture is heated into the gas phase by the bottom reboiler 16 and returned to the column by the bottom reflux pipe 15.

[0027] Before entering tower 13, if the proportion of the lighter component, hydrogen fluoride gaseous mixture, in the gas mixture is greater than the preset normal value after sampling and testing, in order to facilitate the ascent of the lighter component, hydrogen fluoride gaseous mixture: (in conjunction with the attached...) Figure 4As the slide bar 9 descends, the elastic tray forms a conical tray B33 with the expanding neck at the top and the contracting neck at the bottom. The inner wall of the conical tray A30 forms the outer wall of the conical tray B33. A conical cavity B32 is provided within the conical tray B33. The lower end of the conical tray B33 is located at the center of the circular hole 11 provided in the next layer of planar tray 10. The lighter hydrogen fluoride gaseous mixture in the gas mixture rises, while the heavier sulfuric acid impurity liquid mixture in the gas mixture descends. Because the elastic tray forms a conical tray B33 with the expanding neck at the top and the contracting neck at the bottom, the heavier liquid phase mixture in the gas mixture is obstructed by the conical tray B33 as it descends. The liquid phase mixture collected in the conical cavity B32 can only descend slowly through multiple leakage holes B26 provided near the inner edge of the conical tray B33. Since the gaseous phase mixed in the liquid phase is easier to separate from the liquid phase, the gaseous hydrogen fluoride mixture in the gaseous phase is released more completely. After the rising gaseous hydrogen fluoride mixture and the falling liquid phase come into contact and separate, they reach the top of the column and are led out by the top outlet pipe 1. After being condensed by the top condenser 2, part of the gaseous hydrogen fluoride mixture is collected as the top product through the top discharge pipe 3, and part of the gaseous hydrogen fluoride mixture is returned to the column as the top reflux through the top reflux pipe 4. After the falling liquid sulfuric acid impurity liquid mixture comes into contact and separates from the rising gas phase, it reaches the bottom of the column and is led out by the bottom liquid outlet pipe 29. Part of the liquid sulfuric acid impurity mixture is collected as the bottom product through the bottom collection pipe 17, and part of the liquid sulfuric acid impurity mixture is heated into the gaseous phase by the bottom reboiler 16 and returned to the column by the bottom reflux pipe 15.

[0028] In use, the motor 19 drives the rotating shaft 8 to rotate, which in turn drives the gear 6 to rotate. The rotation of the gear 6 drives the slide rod 9, which is meshed with the teeth 5, to slide up and down. The slide rod 9 drives multiple silicone disc trays 23, which are spaced and sleeved on the slide rod 9, to form either a flat surface, or a conical tray A30 with the expanded neck end at the bottom and the contracted neck end at the top, or a conical tray B33 with the expanded neck end at the top and the contracted neck end at the bottom, as needed. Since the specific gravity of the hydrogen fluoride gaseous mixture and the sulfuric acid impurity mixture in the gas mixture generated by the rotary kiln reaction is a frequently changing value, the multiple silicone disc trays 23 can be dynamically adjusted multiple times without stopping under the drive of the motor 19, so as to achieve the purpose of more thorough separation of the tower body 13 during use.

[0029] The parts of this invention not described in detail are prior art.

Claims

1. A crude sulfur tower with conditioning function for preparing hydrogen fluoride, characterized in that: The system includes a tower body (13), a cavity (14) inside the tower body (13), and multiple horizontally arranged flat trays (10) with their outer edges fixed to the side walls of the cavity (14) at intervals in the middle of the cavity (14). A circular hole (11) is provided at the center of each flat tray (10), and multiple leakage holes A (12) are provided around the circular hole (11) on each flat tray (10). Horizontally arranged support rings (25) are evenly arranged between each two adjacent flat trays (10). The diameter of the support rings (25) is larger than the diameter of the circular hole (11) and smaller than the diameter of the cross-section of the cavity (14). Multiple support rings (25) are fixed to the side walls of the cavity (14) through support rods (22). The middle section of the sliding rod (9) passes through multiple circular holes (11). A silicone elastic tower is provided between multiple support rings (25) and sliding rods (9). Each elastic tray has multiple leakage holes B (26) spaced around its inner edge. When the elastic tray is not subjected to external force, it forms a planar disc tray (23). When the slide bar (9) rises, the elastic tray forms a conical tray A (30) with the expanded neck end at the bottom and the contracted neck end at the top. A conical cavity A (31) is provided inside the conical tray A (30). The upper end of the conical tray A (30) is located at the center of the circular hole (11) provided in the upper planar tray (10). When the slide bar (9) falls, the elastic tray forms a conical tray B (33) with the expanded neck end at the top and the contracted neck end at the bottom. The inner wall of the conical tray A (30) forms the outer wall of the conical tray B (33). A conical cavity B (32) is provided inside the conical tray B (33). The lower end of the conical tray B (33) is located at the center of the circular hole (11) provided in the lower planar tray (10). A collar A (21) coaxial with the circular hole (11) is provided above the uppermost flat tray (10), and a collar B (28) coaxial with the circular hole (11) is provided below the lowermost flat tray (10). The diameter of the collar A (21) is smaller than the diameter of the circular hole (11) and equal to the diameter of the slide rod (9). The diameters of the collar B (28) and the collar A (21) are the same. The upper part of the slide rod (9) is slidably connected in the collar A (21), and the lower part of the slide rod (9) is slidably connected in the collar B (28). Multiple connecting rods A (20) are provided around the collar A (21) between the collar A (21) and the side wall of the cavity (14), and multiple connecting rods B (27) are provided around the collar B (28) between the collar B (28) and the side wall of the cavity (14). Multiple teeth (5) are spaced apart on the slide rod (9) located above the collar A (21). The motor (19) is located outside the tower body (13), and its rotating shaft (8) extends into the cavity (14). A gear (6) is sleeved on the rotating shaft (8) located in the cavity (14). The gear (6) and the teeth (5) mesh. The rotation of the motor (19) can drive the slide rod (9) to move up and down. When the gear (6) is located at the lower part of the multiple teeth (5), the elastic tray forms a conical tray A (30). When the gear (6) is located at the upper part of the multiple teeth (5), the elastic tray forms a conical tray B (33).

2. The crude sulfur tower with regulating function for preparing hydrogen fluoride according to claim 1, characterized in that: A bearing seat (7) is provided on the side wall of the cavity (14) opposite to the motor (19). The end of the rotating shaft (8) is rotatably sleeved in the shaft hole provided in the bearing seat (7). A housing (18) is covered outside the motor (19) and fixed to the outer wall of the tower body (13).

3. The crude sulfur tower with regulating function for preparing hydrogen fluoride according to claim 1, characterized in that: The motor (19) is a forward and reverse servo motor.

4. The crude sulfur tower with regulating function for preparing hydrogen fluoride according to claim 1, characterized in that: The upper end of the tower body (13) is connected to one end of the tower top outlet pipe (1), and the other end of the tower top outlet pipe (1) is connected to one end of the tower top reflux pipe (4) and the tower top discharge pipe (3), respectively. A condenser (2) is provided on the tower top outlet pipe (1), and the other end of the tower top reflux pipe (4) is connected to the tower body (13) located above the uppermost flat tray (10).

5. The crude sulfur tower with regulating function for preparing hydrogen fluoride according to claim 1, characterized in that: The lower end of the tower body (13) is connected to one end of the bottom liquid outlet pipe (29), and the other end of the bottom liquid outlet pipe (29) is connected to one end of the bottom collection pipe (17) and the bottom reflux pipe (15). A reboiler (16) is provided on the bottom reflux pipe (15), and the other end of the bottom reflux pipe (15) is connected to the tower body (13) located below the lowest flat tray (10).

6. The crude sulfur tower with regulating function for preparing hydrogen fluoride according to claim 1, characterized in that: A feed pipe (24) is provided on the tower body (13) located in the lower part of multiple planar tower trays (10).

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