Device for preparing high-purity magnesium fluoride by liquid crystallization method

Abstract

The utility model relates to the technical field of magnesium fluoride preparation devices, and discloses a device for preparing high-purity magnesium fluoride by a liquid crystallization method, which comprises a supporting bottom plate, a reaction bin is arranged on the top surface of the supporting bottom plate, a sintering furnace and a polycrystal grower are fixedly mounted on the top surface of the supporting bottom plate, a PLC (programmable logic controller) is arranged on the top surface of the supporting bottom plate, and the PLC is connected with the reaction bin. The device further comprises a discharging assembly used for discharging magnesium fluoride crystals, the discharging assembly is arranged on the outer circle wall face of the reaction bin, and the purpose of taking out the magnesium fluoride crystals in the reaction bin can be achieved through mutual cooperative use of the arranged supporting bottom plate, the reaction bin, the driving motor and the connecting shaft; the magnesium fluoride single crystals can be automatically discharged, meanwhile, residual crystals are discharged from the interior of the reaction bin under scraping of the scraping stirring frame, the situation that the magnesium fluoride single crystals are not discharged completely can be avoided while the magnesium fluoride single crystals can be discharged, use of a user and preparation work are facilitated, and practicability is achieved.

Description

TECHNICAL FIELD

[0001] The utility model relates to magnesium fluoride preparation device technical field especially relates to a kind of device of liquid crystallization method preparation high-purity magnesium fluoride. BACKGROUND

[0002] Magnesium fluoride is a colorless or white crystalline solid, soluble in water, has important industrial and scientific research applications, the following is some detailed method introduction about the preparation of high-purity magnesium fluoride using liquid crystallization method in prior art: first step: first, the concentration of 40% hydrofluoric acid is added into reaction kettle, then magnesium carbonate (wherein magnesium oxide content ≥41%) is added, the mass ratio of hydrofluoric acid and magnesium carbonate is 1:1, uniform stirring makes the reaction sufficient (reaction equation: Mg2CO3+H2F MgF2·xH2O+CO2+H2O), after reaction termination, magnesium fluoride hydrate microcrystal is generated, and the mother liquor after reaction is hydrofluoric acid solution with PH=3~4. Second step: the generated magnesium fluoride hydrate microcrystal is incubated at 100°C~105°C for 24 hours to carry out liquid single crystal growth, and magnesium fluoride single crystal with central particle size D50≥22μm is generated. Third step, the clarified mother liquor (mother liquor can be reused) is sucked out, and the magnesium fluoride single crystal is moved into polycrystal grower, and polycrystal growth is carried out at the temperature of 140°C~150°C for 20 hours to generate magnesium fluoride polycrystal with particle size of 5~20mm. Fourth step, the magnesium fluoride polycrystal is sintered at the temperature of 500°C~550°C for 24 hours in straight cylinder type three temperature zone quartz sintering furnace. Fifth step, after cooling for 24 hours, polycrystal high-purity magnesium fluoride with particle size of 5~20mm is obtained, and the purity is ≥99.99%, the content of crystal water is ≤0.005%, and the content of magnesium oxide is ≤0.001%.

[0003] Polycrystal grower, this instrument is used for growing crystal, and crystal is solid substance with specific structure and arrangement, has unique physical and chemical properties. Polycrystal grower controls the growth process of crystal by specific technical means, such as crystal growth technology, so as to obtain crystal material with required properties. These materials have wide application in many fields, including electronics, optics, magnetism, etc.

[0004] In prior art, after the generation of magnesium fluoride single crystal with central particle size D50≥22μm during the preparation of magnesium fluoride crystal, the clarified mother liquor needs to be sucked out, and then the magnesium fluoride single crystal is moved into polycrystal grower, but when the magnesium fluoride single crystal is taken out, the magnesium fluoride crystal will adhere to the inside of reaction kettle, and the flowability is poor, so that it is difficult to discharge from the inside of reaction kettle, and the magnesium fluoride single crystal is difficult to take out, and thus a device for preparing high-purity magnesium fluoride by liquid crystallization method is urgently needed to solve the above problems. UTILITY MODEL CONTENT

[0005] The utility model discloses a device for preparing high-purity magnesium fluoride by liquid crystallization method.

[0006] In order to realize the above-mentioned purpose, the utility model adopts the following technical scheme:

[0007] A device for preparing high-purity magnesium fluoride by liquid crystallization method, including support bottom plate, the top surface of support bottom plate is provided with reaction bin, the top surface of support bottom plate is fixedly installed with sintering furnace and polycrystal grower, the top surface of support bottom plate is provided with PLC controller, still include for the discharge of magnesium fluoride crystalline body exports the discharge component, the discharge component sets up in the outer circular wall surface of reaction bin, the discharge component includes: bin cover, the bin cover is fixedly installed on the top surface of reaction bin.

[0008] As a further scheme of the utility model, the discharge component further includes: a top surface of the bin cover is fixedly installed with a drive motor, the drive motor is electrically connected with the PLC controller, a bottom surface of a drive shaft of the drive motor is fixedly installed with a connecting shaft, a bottom surface of the connecting shaft is fixedly installed with a scraping stirring frame, the scraping stirring frame is movably sleeved with an inner circular wall surface of the reaction bin, a top surface of the support bottom plate is fixedly installed with a support frame, one side of the support frame is fixedly installed with a first drive mechanism, both sides of the support frame are respectively provided with a first circular through hole, an inner circular wall surface of the first circular through hole is movably sleeved with a fixed column, the fixed column is fixedly installed with the reaction bin, a drive motor of the first drive mechanism is electrically connected with the PLC controller, one end of a drive shaft of the drive motor of the first drive mechanism is fixedly installed with the fixed column, an outer circular wall surface of the support bottom plate is provided with a discharge hole, an inside of the discharge hole is fixedly sleeved with a fixed bin, both sides of the fixed bin are respectively provided with a supporting hole, an inside of the fixed bin is movably sleeved with two rotating rollers, the rotating rollers are movably sleeved with the supporting holes, an inside of the fixed bin is provided with a filter screen belt, the filter screen belt is movably sleeved with the rotating rollers, one side of the fixed bin is fixedly installed with a second drive mechanism, a drive motor of the second drive mechanism is electrically connected with the PLC controller, one end of a drive shaft of the drive motor of the second drive mechanism is fixedly installed with the rotating rollers, one side of the fixed bin is fixedly installed with a support bin, one side of the support bin is provided with a second circular through hole, an inner circular wall surface of the second circular through hole is fixedly sleeved with a liquid discharge pipe, one side of the support bin is provided with a rectangular through hole, an inside of the rectangular through hole is fixedly sleeved with a discharge pipe, an inside bottom surface of the reaction bin is fixedly installed with a filter plate, a top surface of the fixed bin is provided with a vent hole.

[0009] As a further scheme of the utility model, the inside of the discharge hole is respectively provided with a limiting groove on both sides, the inside of the limiting groove is movably sleeved with a moving sealing plate.

[0010] As a further scheme of the utility model, the outer circular wall surface of the reaction bin is provided with a limiting hole, the limiting hole is movably sleeved with the movable sealing plate, the outer circular wall surface of the reaction bin is fixedly installed with a fixed plate, the top surface of the fixed plate is provided with a pen type double ear electric push rod, the inner circular wall surface of the ear ring of the pen type double ear electric push rod is movably sleeved with a connecting column, the connecting column on the left side is fixedly installed with the movable sealing plate, and the connecting column on the right side is fixedly installed with the fixed plate.

[0011] As a further scheme of the utility model, the inner circular wall surface of the water outlet of the bottom surface of the reaction bin is fixedly sleeved with a solenoid valve mechanism.

[0012] As a further scheme of the utility model, the top surface of the supporting bottom plate is fixedly installed with a supporting pipe, and the supporting pipe is fixedly installed with the PLC controller.

[0013] As a further scheme of the utility model, one side of the inside of the supporting bin is fixedly installed with a scraper, and the scraper is attached to the filter screen belt.

[0014] Compared with the prior art, the utility model has the beneficial effects that:

[0015] The mutual cooperation of the supporting bottom plate, the reaction bin, the polycrystal grower, the sintering furnace, the bin cover, the driving motor and the connecting shaft can achieve the purpose of taking out the magnesium fluoride single crystal in the reaction bin, so that the magnesium fluoride single crystal can be discharged by itself and the residual crystal can be discharged from the inside of the reaction bin under the scraping of the scraping stirring frame, the magnesium fluoride single crystal can be discharged while avoiding the incomplete discharge of the magnesium fluoride single crystal, the use and preparation work of the user are facilitated, and the utility model is practical. BRIEF DESCRIPTION OF DRAWINGS

[0016] Figure 1 The utility model proposes a kind of overall structure schematic diagram of the device for preparing high-purity magnesium fluoride of liquid crystallization method;

[0017] Figure 2 The utility model proposes the supporting bottom plate structure schematic diagram of the device for preparing high-purity magnesium fluoride of liquid crystallization method;

[0018] Figure 3 For Figure 2 Local structure schematic diagram of A in the utility model;

[0019] Figure 4 The utility model proposes the limiting hole structure schematic diagram of the device for preparing high-purity magnesium fluoride of liquid crystallization method.

[0020] In the figure: 1, support bottom plate; 2, reaction bin; 3, polycrystal grower; 4, sintering furnace; 5, bin cover; 6, driving motor; 7, connecting shaft; 8, scraping stirring frame; 9, support frame; 10, first driving mechanism; 11, discharge hole; 12, limiting groove; 13, fixed bin; 14, filter plate; 15, rotating roller; 16, filter screen belt; 17, support bin; 18, support hole; 19, second driving mechanism; 20, liquid discharge pipe; 21, discharge pipe; 22, pen type double-ear electric push rod; 23, moving sealing plate; 24, air hole; 25, fixed plate; 26, connecting column; 27, limiting hole; 28, electromagnetic valve mechanism; 29, support pipe; 30, scraper; 31, connecting column. DETAILED DESCRIPTION

[0021] In order to make the technical means, creative features, purposes and effects realized by the utility model easy to understand, the utility model is further described below in combination with specific embodiments.

[0022] In the description of the utility model, it should be pointed out that the positions or location relationships indicated by the terms "upper", "lower", "inner", "outer", "front end", "rear end", "two ends", "one end", "the other end" and the like are the positions or location relationships shown in the drawings, and are only for the convenience of describing the utility model and simplifying the description, and do not indicate or imply that the devices or elements indicated must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the utility model. In addition, the terms "first" and "second" are only for the purpose of description, and cannot be understood as indicating or implying relative importance.

[0023] In the description of the utility model, it should be pointed out that unless otherwise explicitly specified and limited, the terms "mounting", "provided with", "connection" and the like should be broadly understood, for example, "connection" can be fixed connection, can also be detachable connection, or integral connection, can be mechanical connection, can also be electrical connection, can be directly connected, can also be indirectly connected through an intermediate medium, and can be the communication between two elements. For ordinary skilled persons in the art, the specific meanings of the above terms in the utility model can be understood according to specific circumstances.

[0024] REFERENCE Figures 1-4The utility model provides a kind of device for preparing high-purity magnesium fluoride by liquid crystallization method, including support base plate 1, the top surface of support base plate 1 is provided with reaction bin 2, sintering furnace 4 and polycrystal grower 3 are fixedly installed on the top surface of support base plate 1, the top surface of support base plate 1 is provided with PLC controller, it further includes for discharging discharge assembly to crystal, discharge assembly is arranged on the outer circular wall surface of reaction bin 2, discharge assembly includes: bin cover 5, bin cover 5 is fixedly installed on the top surface of reaction bin 2, the top surface of bin cover 5 is fixedly installed with driving motor 6, driving motor 6 is electrically connected with PLC controller, the bottom surface of the driving shaft of driving motor 6 is fixedly installed with connecting shaft 7, the bottom surface of connecting shaft 7 is fixedly installed with scraping stirring frame 8, scraping stirring frame 8 is movably sleeved with the inner circular wall surface of reaction bin 2, the top surface of support base plate 1 is fixedly installed with support frame 9, one side of support frame 9 is fixedly installed with first drive mechanism 10, first drive mechanism 10 includes driving motor and the first fixed plate for installing it, the both sides of support frame 9 are respectively provided with first circular through hole, the inner circular wall surface of first circular through hole is movably sleeved with fixed column 31, fixed column 31 is fixedly installed with reaction bin 2, the driving motor of first drive mechanism 10 is electrically connected with PLC controller, one end of the driving shaft of the driving motor of first drive mechanism 10 is fixedly installed with fixed column 31, the outer circular wall surface of support base plate 1 is provided with discharge hole 11, discharge hole 11 is fixedly sleeved with fixed bin 13 in the inside, the both sides of fixed bin 13 are respectively provided with support hole 18, the inside of fixed bin 13 is movably sleeved with two rotating rollers 15, rotating roller 15 is movably sleeved with support hole 18, the inside of fixed bin 13 is provided with filter screen belt 16, there are a large number of apertures in filter screen belt 16, filter screen belt 16 is movably sleeved with rotating roller 15, one side of fixed bin 13 is fixedly installed with second drive mechanism 19, second drive mechanism 19 includes driving motor and the second mounting plate for fixing it, the driving motor of second drive mechanism 19 is electrically connected with PLC controller, one end of the driving shaft of the driving motor of second drive mechanism 19 is fixedly installed with rotating roller 15, one side of fixed bin 13 is fixedly installed with support bin 17, one side of support bin 17 is provided with second circular through hole, the inner circular wall surface of second circular through hole is fixedly sleeved with liquid discharge pipe 20, one side of support bin 17 is provided with rectangular through hole, the inside of rectangular through hole is fixedly sleeved with discharge pipe 21, the inside bottom surface of reaction bin 2 is fixedly installed with filter plate 14, the top surface of fixed bin 13 is provided with vent hole 24.

[0025] In the embodiment, the inside of the discharge hole 11 is provided with a limiting groove 12 on both sides, a movable sealing plate 23 is movably sleeved in the limiting groove 12, the limiting groove 12 and the movable sealing plate 23 are sealed by a sealing ring, the sealing ring is installed on one side of the inside of the limiting groove 12, a limiting hole 27 is formed on the outer circular wall surface of the reaction bin 2, the limiting hole 27 movably sleeves the movable sealing plate 23, a fixed plate 25 is fixedly installed on the outer circular wall surface of the reaction bin 2, a pen type double ear electric push rod 22 is arranged on the top surface of the fixed plate 25, the inner circular wall surface of the ear ring of the pen type double ear electric push rod 22 movably sleeves a connecting column 26, the connecting column 26 on the left side is fixedly installed with the movable sealing plate 23, the connecting column 26 on the right side is fixedly installed with the fixed plate 25, an electromagnetic valve mechanism 28 is fixedly sleeved on the inner circular wall surface of the water outlet on the bottom surface of the reaction bin 2, the electromagnetic valve mechanism 28 comprises an electromagnetic valve and an inlet and outlet water pipe connected with the electromagnetic valve, that is, the inlet water pipe is connected with the water outlet on the bottom surface of the reaction bin 2, a support pipe 29 is fixedly installed on the top surface of the support bottom plate 1, the support pipe 29 is fixedly installed with a PLC controller, a scraper 30 is fixedly installed on one side of the inside of the support bin 17, and the scraper 30 is attached to the filter screen belt 16.

[0026] From the above description, it can be seen that the above-mentioned embodiments of the utility model realize the following technical effects: through the setting of the reaction bin 2, when the magnesium fluoride single crystal inside the reaction bin 2 needs to be taken out, then the mother liquor inside the reaction bin 2 is filtered through the filter plate 14 and discharged through the water outlet pipe of the electromagnetic valve mechanism 28, then the container containing the magnesium fluoride polycrystal is placed on the top surface of the support bottom plate 1, the liquid discharge pipe 20 is connected with the mother liquor container through the pipeline, then the first driving mechanism 10 is started to drive the reaction bin 2 to rotate slowly about 80 degrees to the right side, at the same time, the driving motor 6 is started to drive the connecting shaft 7 to drive the scraping stirring frame 8 to rotate in the inside of the reaction bin 2 to scrape the inner wall, so that the magnesium fluoride single crystal is scraped off and gradually accumulates in the lowest part of the inside of the reaction bin 2 along with the inclination of the reaction bin 2, so that the second driving mechanism 19 is started to drive the rotating roller 15 to drive the filter screen belt 16 to rotate, and the pen type double ear electric push rod 22 is started to pull the moving sealing plate 23 to move in the inside of the limiting groove 12, so that the moving sealing plate 23 no longer seals the discharge hole 11, so that the magnesium fluoride single crystal falls to the top surface of the filter screen belt 16 through the discharge hole 11 under the action of the gravity and the scraping stirring frame 8, the filter screen belt 16 conveys the magnesium fluoride single crystal, the scraping plate 30 is set to scrape the magnesium fluoride single crystal adhered to the outside of the filter screen belt 16, the magnesium fluoride single crystal is discharged through the setting of the discharge pipe 21 and falls into the placed container, the residual mother liquor is filtered out by the filter screen belt 16 and flows into the container through the setting of the liquid discharge pipe 20, then the magnesium fluoride single crystal is replaced and placed in the polycrystal grower 3, polycrystal growth is carried out at a temperature of 140 DEG C to 150 DEG C for 20 hours, magnesium fluoride polycrystal with a particle size of 5 to 20 mm is generated, the magnesium fluoride polycrystal is air sintered in the sintering furnace 4 at a temperature of 500 DEG C to 550 DEG C for 24 hours, and is cooled for 24 hours, so that the polycrystal high-purity magnesium fluoride with a particle size of 5 to 20 mm is obtained, so that the purpose of taking out the magnesium fluoride single crystal inside the reaction bin 2 is achieved, the magnesium fluoride single crystal can be discharged by itself, and the residual crystal is discharged from the inside of the reaction bin 2 under the scraping of the scraping stirring frame 8, so that the magnesium fluoride single crystal can be discharged while avoiding that the magnesium fluoride single crystal is not discharged completely, which facilitates the use and preparation work of the user, and is more practical.

[0027] The basic principle and main features of the utility model and the advantages of the utility model are shown and described above. Those skilled in the art should understand that the utility model is not limited to the above-mentioned embodiments, the above-mentioned embodiments and the description in the specification only illustrate the principle of the utility model, various changes and improvements of the utility model fall within the scope of the utility model without departing from the spirit and range of the utility model.

Claims

1. A device for preparing high-purity magnesium fluoride by liquid crystallization method, comprising a supporting bottom plate (1), the top surface of the supporting bottom plate (1) is provided with a reaction bin (2), the top surface of the supporting bottom plate (1) is fixedly installed with a sintering furnace (4) and a polycrystal grower (3), and the top surface of the supporting bottom plate (1) is provided with a PLC controller, characterized in that, Also include the discharge assembly for the magnesium fluoride crystal is discharged, the discharge assembly is arranged on the outer wall surface of the reaction bin (2), the discharge assembly includes: bin cover (5), the bin cover (5) is fixedly installed on the top surface of the reaction bin (2).

2. The apparatus for preparing high-purity magnesium fluoride by liquid crystallization method according to claim 1, wherein The discharge assembly further includes: the top surface of the bin cover (5) is fixedly installed with drive motor (6), the drive motor (6) is electrically connected with the PLC controller, the bottom surface of the drive shaft of the drive motor (6) is fixedly installed with connecting shaft (7), the bottom surface of the connecting shaft (7) is fixedly installed with scraping stirring frame (8), the scraping stirring frame (8) is movably sleeved with the inner wall surface of the reaction bin (2), the top surface of the support base plate (1) is fixedly installed with support frame (9), one side of the support frame (9) is fixedly installed with first drive mechanism (10), both sides of the support frame (9) are respectively provided with first circular through hole, the inner wall surface of the first circular through hole is movably sleeved with fixed column (31), the fixed column (31) is fixedly installed with the reaction bin (2), the drive motor of the first drive mechanism (10) is electrically connected with the PLC controller, one end of the drive shaft of the drive motor of the first drive mechanism (10) is fixedly installed with the fixed column (31), the outer wall surface of the support base plate (1) is provided with discharge hole (11), the inside of the discharge hole (11) is fixedly sleeved with fixed bin (13), both sides of the fixed bin (13) are respectively provided with support hole (18), the inside of the fixed bin (13) is movably sleeved with two rotating rollers (15), the rotating rollers (15) are movably sleeved with the support hole (18), the inside of the fixed bin (13) is provided with filter screen belt (16), the filter screen belt (16) is movably sleeved with the rotating rollers (15), one side of the fixed bin (13) is fixedly installed with second drive mechanism (19), the drive motor of the second drive mechanism (19) is electrically connected with the PLC controller, one end of the drive shaft of the drive motor of the second drive mechanism (19) is fixedly installed with the rotating rollers (15), one side of the fixed bin (13) is fixedly installed with support bin (17), one side of the support bin (17) is provided with second circular through hole, the inner wall surface of the second circular through hole is fixedly sleeved with liquid discharge pipe (20), one side of the support bin (17) is provided with rectangular through hole, the inside of the rectangular through hole is fixedly sleeved with discharge pipe (21), the inside bottom surface of the reaction bin (2) is fixedly installed with filter plate (14), the top surface of the fixed bin (13) is provided with vent hole (24).

3. The apparatus for preparing high-purity magnesium fluoride by liquid crystallization method according to claim 2, wherein The inside of the discharge hole (11) is respectively provided with limiting groove (12) on both sides, the inside of the limiting groove (12) is movably sleeved with moving sealing plate (23).

4. The apparatus for preparing high-purity magnesium fluoride by liquid crystallization method according to claim 3, wherein The outer circular wall surface of the reaction bin (2) is provided with a limiting hole (27), the limiting hole (27) is movably sleeved with the movable sealing plate (23), the outer circular wall surface of the reaction bin (2) is fixedly installed with a fixed plate (25), the top surface of the fixed plate (25) is provided with a pen type double ear electric push rod (22), the inner circular wall surface of the ear ring of the pen type double ear electric push rod (22) is movably sleeved with a connecting column (26), the connecting column (26) located on the left side is fixedly installed with the movable sealing plate (23), and the connecting column (26) located on the right side is fixedly installed with the fixed plate (25).

5. The apparatus for preparing high-purity magnesium fluoride by liquid crystallization method according to claim 1, wherein The inner circular wall surface of the water outlet of the bottom surface of the reaction bin (2) is fixedly sleeved with an electromagnetic valve mechanism (28).

6. The apparatus for preparing high purity magnesium fluoride by liquid crystallization method according to claim 1, wherein The top surface of the supporting bottom plate (1) is fixedly installed with a supporting pipe (29), and the supporting pipe (29) is fixedly installed with the PLC controller.

7. The apparatus for preparing high-purity magnesium fluoride by liquid crystallization method according to claim 2, wherein One side of the inside of the supporting bin (17) is fixedly installed with a scraper (30), and the scraper (30) is attached to the filter screen belt (16).

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