Ultrasonic-assisted extraction device for fluoride recovery

Abstract

The extraction device comprises a stone crusher, a reaction extraction pool, a vacuum evaporator and a waste liquid pool, the outlet end of the stone crusher is communicated with the inlet end of the closed reaction extraction pool through a conveying belt, and an injection opening is formed in the top of the reaction extraction pool; a plurality of rows of ultrasonic probes arranged in the generatrix direction of the inner wall are arranged in the circumferential direction of the inner wall of the reaction extraction pool at intervals, at least two ultrasonic probes are further arranged at the bottom of the reaction extraction pool at intervals, and the outlet end of the reaction extraction pool is communicated with the inlet end of the waste liquid pool through a blow-off pipeline; the other outlet end of the reaction extraction pool is communicated with the inlet end of a vacuum evaporator through a first conveying pipeline, and the vacuum evaporator is provided with a plurality of outlet ends which are correspondingly communicated with the inlet ends of a first condensation pipe, a second condensation pipe and a third liquid storage tank through a second conveying pipeline, a third conveying pipeline and a fourth conveying pipeline respectively; and the outlet ends of the first condenser pipe and the second condenser pipe are correspondingly communicated with the inlet ends of the first liquid storage tank and the second liquid storage tank through pipelines respectively.

Description

Technical Field

[0001] The utility model belongs to the technical field of resource recovery, and in particular relates to an ultrasonic-assisted fluoride recovery extraction device. Background Art

[0002] Fluorine is an element widely distributed in nature, accounting for about 0.072wt.% in the earth's crust. Fluorine resources in nature mainly exist in cryolite, fluorite, and fluorophosphate ore. Since the reserves of cryolite in nature are very low and only exist in a few countries, cryolite is generally not used as a raw material for fluorine chemical products. Therefore, the fluorine sources of fluorine chemical products are mainly fluorite and fluorophosphate ore.

[0003] In the process of extracting fluorophosphate ore with concentrated sulfuric acid, the existing equipment is to put concentrated sulfuric acid and fluorophosphate ore into a reaction extraction tank for extraction through an extraction device, and then recover the fluorine resources through a vacuum circulation evaporation device. However, the existing equipment has a long precipitation time for fluorine element, low precipitation efficiency and needs to remove impurities attached to the surface of the fluorophosphate ore in advance, which greatly affects the production efficiency, reduces the precipitation amount of fluorine element, and causes waste of resources. Utility Model Content

[0004] The utility model aims to provide an ultrasonic-assisted fluoride recovery extraction device, aiming to solve the problems raised in the background technology.

[0005] In order to achieve the above purpose, the utility model provides the following technical solutions:

[0006] An ultrasonic-assisted fluoride recovery extraction device comprises a stone crusher, a reaction extraction tank, a vacuum evaporator, and a waste liquid tank. The outlet end of the stone crusher is connected to the inlet end of the closed reaction extraction tank through a conveyor belt. The top of the reaction extraction tank is provided with an injection port. The inner wall of the reaction extraction tank is provided with a plurality of rows of ultrasonic probes arranged along the inner wall generatrix direction at intervals in the circumferential direction. The bottom of the reaction extraction tank is also provided with at least two ultrasonic probes at intervals. The outlet end of the reaction extraction tank is connected to the inlet end of the waste liquid tank through a sewage pipe. The other outlet end of the reaction extraction tank is connected to the inlet end of the vacuum evaporator through a first conveying pipe. The vacuum evaporator is provided with a plurality of outlet ends and is respectively connected to the inlet ends of a first condenser, a second condenser, and a third liquid storage tank through a second conveying pipe, a third conveying pipe, and a fourth conveying pipe. The outlet ends of the first condenser and the second condenser are respectively connected to the inlet ends of a first liquid storage tank and a second liquid storage tank through pipes.

[0007] Compared with the prior art, the beneficial effects of the utility model are:

[0008] 1. In the reaction process of fluorophosphate ore and concentrated sulfuric acid, the application of ultrasound can help increase the mass transfer rate between fluoride in fluorophosphate ore and concentrated sulfuric acid, so that fluoride can be better dissolved and dispersed in dilute phosphoric acid;

[0009] 2. During the reaction of fluorophosphate ore and concentrated sulfuric acid, ultrasound can remove impurities attached to the surface of fluorophosphate ore, increase the contact area between fluorophosphate ore and concentrated sulfuric acid, make the reaction more thorough, and increase the amount of fluoride entering dilute phosphoric acid;

[0010] 3. In the process of extracting fluoride phosphate ore with concentrated sulfuric acid, the application of ultrasound can accelerate the precipitation or crystallization of fluoride in the fluoride phosphate ore, thereby shortening its reaction time;

[0011] 4. The frequency and power of the ultrasound can be adjusted according to the amount of fluorophosphate ore extracted by concentrated sulfuric acid to meet the needs of the industry.

[0012] In summary, the utility model has the characteristics of increasing the reaction rate between fluoride and concentrated sulfuric acid, reducing the precipitation time of fluorine element, increasing the precipitation amount of fluorine element, and being convenient to use. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 It is a schematic diagram of the overall structure of the utility model;

[0014] Figure 2 It is a partial perspective view of the utility model;

[0015] In the figure: 1-crusher, 2-conveyor belt, 3-reaction extraction tank, 301-ultrasonic probe, 302-motor, 303-rotating shaft, 304-stirring rod, 305-injection port, 4-drain pipe, 401-drain valve, 5-waste liquid tank, 6-first conveying pipe, 601-valve I, 7-vacuum evaporator, 8-second conveying pipe, 801-valve II, 9-third conveying pipe, 901-valve III, 10-fourth conveying pipe, 1001-valve IV, 11-first condenser, 12-second condenser, 13-first liquid storage tank, 14-second liquid storage tank, 15-third liquid storage tank, 16-exhaust pipe, 1601-exhaust valve, 17-vacuum pump, 18-vacuum gauge. DETAILED DESCRIPTION

[0016] The technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. It is obvious that the described embodiments are only part of the embodiments of the present application, rather than all the embodiments.

[0017] In the description of the embodiments, it should be noted that the terms "upper", "lower", "up", "down", etc. indicate positions or positional relationships based on the positions or positional relationships shown in the accompanying drawings, which are only for the convenience of describing the present application and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific position, be constructed and operated in a specific position, and therefore cannot be understood as a limitation on the present application. In the description of the present application, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "provided with", "connected", etc. should be understood in a broad sense. For example, "connected" can be a fixed connection, a detachable connection, or an integral connection: it can be a mechanical connection or an electrical connection: it can be a direct connection, it can be an indirect connection through an intermediate medium, and it can be a connection between the two elements. In addition, the terms "first", "second", and "third" are used for descriptive purposes only and cannot be understood as indicating or implying relative importance. For ordinary technicians in this field, the specific meanings of the above terms in the present application can be understood according to specific circumstances.

[0018] like Figure 1 to Figure 2 As shown, an ultrasonic-assisted fluoride recovery extraction device comprises a stone crusher 1, a reaction extraction tank 3, a vacuum evaporator 7, and a waste liquid tank 5. The outlet end of the stone crusher 1 is connected to the inlet end of the closed reaction extraction tank 3 through a conveyor belt 2. The top of the reaction extraction tank 3 is provided with an injection port 305. The inner wall of the reaction extraction tank 3 is provided with a plurality of rows of ultrasonic probes 301 arranged along the inner wall generatrix direction at intervals in the circumferential direction. At least two ultrasonic probes 301 are also provided at intervals at the bottom of the reaction extraction tank 3. The outlet end of the reaction extraction tank 3 is connected to the inlet end of the closed reaction extraction tank 3 through a conveyor belt 2. The top of the reaction extraction tank 3 is provided with an injection port 305. The inner wall of the reaction extraction tank 3 is provided with a plurality of rows of ultrasonic probes 301 arranged along the inner wall generatrix direction at intervals in the circumferential direction. At least two ultrasonic probes 301 are also provided at intervals at the bottom of the reaction extraction tank 3. The sewage pipe 4 is connected to the inlet end of the waste liquid pool 5, and the other outlet end of the reaction extraction pool 3 is connected to the inlet end of the vacuum evaporator 7 through the first delivery pipe 6. The vacuum evaporator 7 is provided with a plurality of outlet ends and is respectively connected to the inlet ends of the first condenser 11, the second condenser 12, and the third liquid storage tank 15 through the second delivery pipe 8, the third delivery pipe 9, and the fourth delivery pipe 10. The outlet ends of the first condenser 11 and the second condenser 12 are respectively connected to the inlet ends of the first liquid storage tank 13 and the second liquid storage tank 14 through corresponding pipes.

[0019] A motor 302 is fixedly installed on the upper end of the reaction extraction pool 3 , and a rotating shaft 303 extending into the reaction extraction pool 3 is fixedly connected to the output end of the motor 302 . A plurality of stirring rods 304 are evenly distributed along the axial direction on the rotating shaft 303 in the reaction extraction pool 3 .

[0020] The minimum distance between the ultrasonic probe 301 on the inner wall of the reaction extraction pool 3 and the stirring rod 304 projected at the bottom of the reaction extraction pool 3 is 80-150 mm, and the minimum distance between the ultrasonic probe 301 at the bottom of the reaction extraction pool 3 and the bottom end of the rotating shaft 303 is 100-150 mm.

[0021] The frequency of the ultrasonic probe 301 is 20-40 KHz.

[0022] A vacuum gauge 18 is fixedly installed on the upper portion of the vacuum evaporator 7 , and the top of the vacuum evaporator 7 is also connected to the inlet end of the vacuum pump 17 through an exhaust pipe 16 .

[0023] The outlet end of the vacuum evaporator 7 connected to the second conveying pipeline 8 is located in the middle and / or upper middle part of the side wall, the outlet end of the vacuum evaporator 7 connected to the third conveying pipeline 9 is located at the top, and the outlet end of the vacuum evaporator 7 connected to the fourth conveying pipeline 10 is located at the bottom.

[0024] The sewage pipe 4, the first delivery pipe 6, the second delivery pipe 8, the third delivery pipe 9, the fourth delivery pipe 10, and the air extraction pipe 16 are respectively fixedly installed with a sewage valve 401, a valve I 601, a valve II 801, a valve III 901, a valve IV 1001, and an air extraction valve 1601.

[0025] The sewage valve 401, valve I 601, valve II 801, valve III 901, valve IV 1001 and air extraction valve 1601 are solenoid valves or manual valves.

[0026] A control console is also provided, and the lithotripter 1, ultrasonic probe 301, motor 302, drain valve 401, valve I601, valve II801, valve III901, valve IV1001, air extraction valve 1601, vacuum pump 17, and vacuum gauge 18 are electrically connected to the control console respectively.

[0027] The reaction extraction tank 3, ultrasonic probe 301, rotating shaft 303, stirring rod 304, waste liquid tank 5, vacuum evaporator 7, first condenser 11, second condenser 12, first liquid storage tank 13, second liquid storage tank 14, third liquid storage tank 15, and vacuum gauge 18 are all made of corrosion-resistant materials.

[0028] The working principle and working process of this utility model:

[0029] like Figure 1 to Figure 2As shown, the fluorophosphate ore is first put into the crusher 1 for crushing, and then the crushed fluorophosphate ore is conveyed to the reaction extraction tank 3 through the conveyor belt 2, and then the reaction solvent is injected into the reaction extraction tank 3 through the injection port 305, and then the motor 302 is started to drive the rotating shaft 303 to rotate so that the stirring rod 304 rotates and stirs the solvent. During this period, the ultrasonic probe 301 is started according to specific parameters. After the extraction is completed, the sewage valve 401 is opened to filter out the residue and waste liquid and discharge it into the waste liquid tank 5 through the sewage pipe 4, and then the exhaust valve 1601 is opened to start the vacuum pump 17 to extract the air of the vacuum evaporator 7 according to the value detected by the vacuum meter 18 so that the vacuum degree reaches a suitable range, and then the valve is slowly opened. Ⅰ601 slowly delivers the fluorine-containing solvent to the vacuum evaporator 7 through the first delivery pipeline 6, then closes all valves connected to the vacuum evaporator 7 and heats the vacuum evaporator 7. The fluorine-containing substance has the lowest boiling point under a vacuum environment. After the temperature reaches the boiling point of the fluorine-containing substance, slowly open valve Ⅱ801 to discharge the fluorine-containing substance into the first condenser 11 for condensation and then flow into the first liquid storage tank 13. Then close valve Ⅱ801 and heat the vacuum evaporator 7 again to heat the water to the boiling point, then slowly open valve Ⅲ901 to discharge the fluorine-containing water vapor into the second condenser 12 for condensation and then flow into the second liquid storage tank 14. Finally, open valve Ⅳ1001 to discharge the remaining substance into the third liquid storage tank 15 to complete the recovery of fluoride.

[0030] It should be noted that the above description is only a preferred embodiment of the utility model and is not intended to limit the utility model. Although the utility model is described in detail with reference to the above embodiments, those skilled in the art can still modify the technical solutions recorded in the above embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the utility model shall be included in the protection scope of the utility model.

Claims

1. An ultrasonic-assisted fluoride recovery extraction device, comprising a stone crusher (1), a reaction extraction tank (3), a vacuum evaporator (7), and a waste liquid tank (5), characterized in that The outlet end of the stone crusher (1) is connected to the inlet end of the closed reaction extraction pool (3) through a conveyor belt (2); an injection port (305) is provided at the top of the reaction extraction pool (3); a plurality of rows of ultrasonic probes (301) arranged along the inner wall generatrix direction are arranged at intervals on the inner wall of the reaction extraction pool (3); at least two ultrasonic probes (301) are also arranged at intervals on the bottom of the reaction extraction pool (3); the outlet end of the reaction extraction pool (3) is connected to the inlet end of the waste liquid pool (5) through a sewage pipe (4); and the reaction extraction pool (3) ) is connected to the inlet end of the vacuum evaporator (7) through the first delivery pipeline (6); the vacuum evaporator (7) is provided with a plurality of outlet ends which are respectively connected to the inlet ends of the first condenser (11), the second condenser (12) and the third liquid storage tank (15) through the second delivery pipeline (8), the third delivery pipeline (9) and the fourth delivery pipeline (10); the outlet ends of the first condenser (11) and the second condenser (12) are respectively connected to the inlet ends of the first liquid storage tank (13) and the second liquid storage tank (14) through the corresponding pipelines.

2. The ultrasonic-assisted fluoride recovery extraction device according to claim 1, characterized in that: A motor (302) is fixedly mounted on the upper end of the reaction extraction cell (3); an output end of the motor (302) is fixedly connected to a rotating shaft (303) extending into the reaction extraction cell (3); and a plurality of stirring rods (304) are evenly distributed along the axial direction on the rotating shaft (303) in the reaction extraction cell (3).

3. The ultrasonic-assisted fluoride recovery extraction device according to claim 2, characterized in that: The minimum distance between the ultrasonic probe (301) on the inner wall of the reaction extraction tank (3) and the stirring rod (304) projected at the bottom of the reaction extraction tank (3) is 80-150 mm, and the minimum distance between the ultrasonic probe (301) at the bottom of the reaction extraction tank (3) and the bottom end of the rotating shaft (303) is 100-150 mm.

4. The ultrasonic-assisted fluoride recovery extraction device according to claim 1, characterized in that: The frequency of the ultrasonic probe (301) is 20-40 KHz.

5. The ultrasonic-assisted fluoride recovery extraction device according to claim 1, characterized in that: A vacuum gauge (18) is fixedly mounted on the upper portion of the vacuum evaporator (7), and the top of the vacuum evaporator (7) is also connected to the inlet end of a vacuum pump (17) via an exhaust pipe (16).

6. The ultrasonic-assisted fluoride recovery extraction device according to claim 5, characterized in that: The outlet end of the vacuum evaporator (7) connected to the second delivery pipeline (8) is located in the middle and / or upper middle part of the side wall, the outlet end of the vacuum evaporator (7) connected to the third delivery pipeline (9) is located at the top, and the outlet end of the vacuum evaporator (7) connected to the fourth delivery pipeline (10) is located at the bottom.

7. The ultrasonic-assisted fluoride recovery extraction device according to any one of claims 1 to 6, characterized in that: The sewage pipe (4), the first delivery pipe (6), the second delivery pipe (8), the third delivery pipe (9), the fourth delivery pipe (10), and the air extraction pipe (16) are respectively fixedly installed with a sewage valve (401), a valve I (601), a valve II (801), a valve III (901), a valve IV (1001), and an air extraction valve (1601).

8. The ultrasonic-assisted fluoride recovery extraction device according to claim 7, characterized in that: The sewage valve (401), valve I (601), valve II (801), valve III (901), valve IV (1001), and air extraction valve (1601) are solenoid valves or manual valves.

9. The ultrasonic-assisted fluoride recovery extraction device according to claim 8, characterized in that: A control console is also provided, and the lithotripter (1), ultrasonic probe (301), motor (302), drain valve (401), valve I (601), valve II (801), valve III (901), valve IV (1001), air extraction valve (1601), vacuum pump (17), and vacuum gauge (18) are electrically connected to the control console respectively.

10. The ultrasonic-assisted fluoride recovery extraction device according to claim 7, characterized in that: The reaction extraction tank (3), ultrasonic probe (301), rotating shaft (303), stirring rod (304), waste liquid tank (5), vacuum evaporator (7), first condenser (11), second condenser (12), first liquid storage tank (13), second liquid storage tank (14), third liquid storage tank (15), and vacuum gauge (18) are all made of corrosion-resistant materials.

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