CN113753917A - High-purity sodium fluoride separation and purification device in silicate production - Google Patents
High-purity sodium fluoride separation and purification device in silicate production Download PDFInfo
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- CN113753917A CN113753917A CN202111113694.6A CN202111113694A CN113753917A CN 113753917 A CN113753917 A CN 113753917A CN 202111113694 A CN202111113694 A CN 202111113694A CN 113753917 A CN113753917 A CN 113753917A
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- pipe
- liquid level
- sodium fluoride
- heat
- purity sodium
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- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 title claims abstract description 60
- 235000013024 sodium fluoride Nutrition 0.000 title claims abstract description 27
- 239000011775 sodium fluoride Substances 0.000 title claims abstract description 27
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 238000000926 separation method Methods 0.000 title claims abstract description 13
- 238000000746 purification Methods 0.000 title claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 80
- 238000004321 preservation Methods 0.000 claims abstract description 22
- 239000011261 inert gas Substances 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims description 22
- 238000007789 sealing Methods 0.000 claims description 19
- 229920001971 elastomer Polymers 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 239000007921 spray Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000004090 dissolution Methods 0.000 abstract description 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 2
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/02—Fluorides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to the technical field of sodium fluoride production by silicate, in particular to a high-purity sodium fluoride separation and purification device in silicate production, which comprises a heat-preservation tank, wherein the lower end of the heat-preservation tank is provided with a base; the beneficial effects are that: through the liquid level height that sets up the level gauge on the U-shaped pipe and reflect in the holding vessel, through the cooperation of flowmeter and liquid pump for the liquid level height of holding vessel and spherical pipe is the same, and at the dissolution in-process, the liquid level of holding vessel is higher than spherical pipe, and when the saturation back, along with inert gas's rush-in, leads to the increase of holding vessel pressure, and the liquid level descends, and then reflects the saturation of dissolving through the liquid level height.
Description
Technical Field
The invention relates to the technical field of sodium fluoride production by silicate, in particular to a device for separating and purifying high-purity sodium fluoride in silicate production.
Background
In the process of preparing sodium fluoride by using silicate, impurities such as magnesium fluoride and ammonium fluoride can be generated, the traditional mode adopts a sectional washing mode to separate and purify through the difference of solubility, one-section washing is used for obtaining sodium fluoride, two-section washing is used for obtaining ammonium fluoride, and three-section washing is used for obtaining magnesium fluoride.
However, in the actual purification process, since the critical point of solubility is difficult to control, in the solution intelligence, a problem of intermixing occurs to result in insufficient purity of separation.
Therefore, the device for separating and purifying the high-purity sodium fluoride in silicate production is provided, and the problem of water washing separation purity is solved.
Disclosure of Invention
The invention aims to provide a device for separating and purifying high-purity sodium fluoride in silicate production, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a high-purity sodium fluoride separation and purification device in silicate production comprises a heat preservation tank, wherein a base is arranged at the lower end of the heat preservation tank, two groups of supporting stand columns are arranged between the heat preservation tank and the base, a cover plate is arranged at the upper end of the heat preservation tank in a sealing mode, the lower end of the heat preservation tank is communicated with one side of a U-shaped pipe, a spherical spray head which is controlled by a liquid pump and extends to the inner cavity of the heat preservation tank is arranged on the cover plate, the lower end of the U-shaped pipe is placed on the upper end face of the base, a first connecting block is arranged at the port of one side of the U-shaped pipe, a second connecting block is arranged at the port of the other side of the U-shaped pipe, the first connecting block and the second connecting block are arranged at equal height, the first connecting block is communicated with the heat preservation tank and a liquid level pipe is vertically arranged, the upper end of the spherical pipe is communicated with the liquid pump through a return pipe, a liquid outlet pipe is arranged on the right side of the spherical pipe, and the upper end of the liquid level pipe is communicated with the inner cavity of the heat preservation tank, the lower end of the liquid level pipe is provided with a detection extension pipe.
Preferably, a sealing ring groove is formed between the upper end of the heat-preserving tank and the lower end of the cover plate, a sealing ring is arranged in the sealing ring groove, and the sealing ring is tightly pressed at the lower end of the cover plate.
Preferably, the side wall of the heat-insulating tank and the outer edge of the lower end of the cover plate are provided with lug seats which are pressed together, and a pair of the lug seats which are symmetrical up and down are fixedly connected through fastening bolts distributed in a circumferential array mode.
Preferably, the upper end of the cover plate is provided with an air inlet pipe, and inert gas is introduced into the air inlet pipe and is nitrogen or argon.
Preferably, the inner cavity of the heat preservation tank is set as a washing inner cavity, a liquid outlet is formed in the right side of the lower end of the washing inner cavity, two groups of first connectors are arranged at the upper end of the first connecting block, and the two groups of first connectors are respectively communicated with the liquid outlet and the lower end of the liquid level pipe.
Preferably, the outer walls of the liquid level pipe and the spherical pipe are vertically provided with a dial gauge, the upper end of the liquid level pipe is provided with a communicating pipe communicated with the inner cavity, the side wall of the washing inner cavity is provided with an air hole, and the upper end of the communicating pipe is inserted into the air hole.
Preferably, the lower extreme of liquid level pipe transversely extends and is provided with the detection extension pipe, the tip upper end of detecting the extension pipe passes through the rubber buffer sealed, the upper end of rubber buffer is passed through the end cover fastening and is covered, be provided with the through-hole of intercommunication rubber stopper up end on the end cover.
Preferably, the upper end of the second connecting block is provided with a second interface, the lower end of the spherical pipe is provided with a lower opening, and the spherical pipe is communicated with the inner cavity of the U-shaped pipe through the lower opening and the sealing connection of the second interface.
Preferably, an upper opening is formed in the upper end of the spherical pipe, the return pipe is inserted into the upper opening, the other end of the return pipe is communicated with the input end of the liquid pump, a flow meter is arranged on the U-shaped pipe, and the flow rate of the liquid pump is the same as the flow meter in value.
Preferably, an overflow groove is formed in the right side of the spherical pipe, the liquid outlet pipe is inserted into the overflow groove, and a lower end port of the return pipe is located below the overflow groove.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the U-shaped pipe and the return pipe are matched to realize circulating water washing, so that a saturated sodium fluoride solution is obtained, after saturation, because the solubility of sodium fluoride is far higher than that of ammonium fluoride, redundant dissolved ammonium fluoride is separated out, and a pure saturated sodium fluoride solution is separated and purified, so that the purpose of improving the separation purity is achieved;
2. according to the invention, the liquid level meter is arranged on the U-shaped pipe to reflect the liquid level height in the heat-insulating tank, the liquid level heights of the heat-insulating tank and the spherical pipe are the same through the matching of the flow meter and the liquid pump, the liquid level of the heat-insulating tank is higher than that of the spherical pipe in the dissolving process, and after the heat-insulating tank is saturated, the pressure of the heat-insulating tank is increased and the liquid level is reduced along with the flushing of inert gas, so that the saturation of the dissolving is reflected through the liquid level height.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a front view of the present invention;
FIG. 3 is a schematic perspective view of a U-shaped tube according to the present invention;
FIG. 4 is a perspective view of the fluid level tube of the present invention;
FIG. 5 is a schematic perspective view of a bulb of the present invention;
fig. 6 is a schematic perspective view of the circulation pipe connection according to the present invention.
In the figure: 1. a heat preservation tank; 2. a cover plate; 3. a base; 4. supporting the upright post; 5. a liquid pump; 6. a spherical nozzle; 7. an ear mount; 8. fastening a bolt; 9. sealing the circular groove; 10. a seal ring; 11. washing the inner cavity with water; 12. a liquid discharge port; 13. a U-shaped tube; 14. a first connection block; 15. a second connecting block; 16. a liquid level tube; 17. a bulb tube; 18. a return pipe; 19. air holes; 20. a communicating pipe; 21. an overflow trough; 22. a liquid outlet pipe; 23. detecting the extension pipe; 24. an air inlet pipe; 25. a flow meter; 26. a first interface; 27. an end cap; 28. an upper opening; 29. a lower opening; 30. a second interface; 31. a rubber plug; 32. and a through hole.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1 to 6, the present invention provides a technical solution:
the utility model provides a high-purity sodium fluoride separation and purification device in silicate production, including heat preservation jar 1, the lower extreme of heat preservation jar 1 is provided with base 3, be provided with two sets of support post 4 between heat preservation jar 1 and the base 3, the sealed apron 2 that is provided with in upper end of heat preservation jar 1, be provided with sealed ring groove 9 between the lower extreme of heat preservation jar 1's upper end and apron 2, be provided with sealing ring 10 in the sealed ring groove 9, the inseparable pressfitting of sealing ring 10 is at the lower extreme of apron 2, through the cooperation of sealing ring 10 with sealed ring groove 9, realize apron 2 and heat preservation jar 1's sealing connection.
The side wall of the heat preservation tank 1 and the lower end outer edge of the cover plate 2 are provided with lug seats 7 which are pressed together, a pair of lug seats 7 which are symmetrical up and down are fixedly connected through fastening bolts 8 which are distributed in a circumferential array mode, and the cover plate 2 is fixedly installed through the matching of the lug seats 7 and the fastening bolts 8.
The lower extreme of holding vessel 1 communicates one side of U-shaped pipe 13, the up end at base 3 is placed to the lower extreme of U-shaped pipe 13, one side port of U-shaped pipe 13 is provided with first connecting block 14, first connecting block 14 intercommunication holding vessel 1 and the vertical liquid level pipe 16 that is provided with, the inner chamber of holding vessel 1 sets up to washing inner chamber 11, the lower extreme right side of washing inner chamber 11 is provided with leakage fluid dram 12, the upper end of first connecting block 14 sets up two sets of first interfaces 26, two sets of first interfaces 26 communicate the lower extreme of leakage fluid dram 12 and liquid level pipe 16 respectively, realize holding vessel 1 through first interface 26, the intercommunication of liquid level pipe 16 and U-shaped pipe 13.
Equal vertical graduation apparatus that is provided with on the outer wall of liquid level pipe 16 and bulb 17, the upper end of liquid level pipe 16 is provided with communicating pipe 20 of intercommunication inner chamber, is provided with gas pocket 19 on the lateral wall of washing inner chamber 11, pegs graft at gas pocket 19 in the upper end of communicating pipe 20, through the cooperation of communicating pipe 20 and gas pocket 19, realizes liquid level pipe 16 and washing inner chamber 11 intercommunication to reflect the height of liquid level in the holding tank 1 through liquid level pipe 16.
The other side port of the U-shaped pipe 13 is provided with a second connecting block 15, the upper end of the second connecting block 15 is vertically connected with a spherical pipe 17, the upper end of the second connecting block 15 is provided with a second interface 30, the lower end of the spherical pipe 17 is provided with a lower opening 29, the spherical pipe 17 is communicated with the inner cavity of the U-shaped pipe 13 through the sealing connection of the lower opening 29 and the second interface 30, and the communication between the spherical pipe 17 and the U-shaped pipe 13 is realized through the second interface 30.
Be provided with the spherical shower nozzle 6 that extends to 1 inner chamber of holding tank of 5 controls of liquid pump on the apron 2, 18 intercommunication liquid pumps 5 are passed through to the upper end of spherical pipe 17 back flow, realize the purpose of circulation washing through back flow 18 and liquid pump 5, the circulation washing, thereby obtain saturated sodium fluoride solution, after the saturation, because the solubility of sodium fluoride is far greater than ammonium fluoride, thereby precipitate unnecessary dissolved ammonium fluoride, the pure saturated sodium fluoride solution of separation and purification play, reach the purpose that improves separation purity.
The first connecting block 14 and the second connecting block 15 are arranged at the same height, the upper end of the spherical pipe 17 is provided with an upper opening 28, the return pipe 18 is inserted in the upper opening 28, the other end of the return pipe 18 is communicated with the input end of the liquid pump 5, the U-shaped pipe 13 is provided with the flow meter 25, the flow rate of the liquid pump 5 is the same as the value of the flow meter 25, and the flow rate of the liquid pump 5 is controlled to be the same as the liquid discharge flow rate of the liquid discharge port 12, so that the liquid level heights of two sides of the U-shaped pipe 13 are the same.
The upper end of apron 2 is provided with intake pipe 24, let in inert gas in the intake pipe 24, inert gas is nitrogen gas or argon gas, the right side of spherical pipe 17 is provided with overflow launder 21, drain pipe 22 pegs graft in overflow launder 21, the lower extreme port of back flow pipe 18 is located the below of overflow launder 21, in the dissolution process, the liquid level of holding vessel 1 is higher than spherical pipe 17, and after the saturation, along with inert gas's rush-in, lead to holding vessel 1 pressure increase, the liquid level of liquid level pipe 16 descends, and then reflect the saturation of dissolving through the liquid level height.
The working principle is as follows: at first, through the cooperation of sealing ring 10 and sealed ring groove 9, realize apron 2 and holding tank 1's sealing connection, through the cooperation of ear seat 7 with fastening bolt 8, realize apron 2's fixed mounting, realize holding tank 1 through first interface 26, the intercommunication of liquid level pipe 16 and U-shaped pipe 13, through the cooperation of communicating pipe 20 and gas pocket 19, realize liquid level pipe 16 and washing inner chamber 11 intercommunication, thereby reflect the height of the interior liquid level of holding tank 1 through liquid level pipe 16
Realize the intercommunication of bulb 17 and U-shaped pipe 13 through second interface 30, realize the purpose of circulation washing through back flow 18 and liquid pump 5, the circulation washing to obtain saturated sodium fluoride solution, after the saturation, because the solubility of sodium fluoride is far more than ammonium fluoride, thereby separate out unnecessary dissolved ammonium fluoride, the pure saturated sodium fluoride solution of separation and purification, reach the purpose that improves separation purity.
The velocity of flow through control liquid pump 5 is the same with the flowing back velocity of flow of leakage fluid dram 12, thereby make the liquid level height of U-shaped pipe 13 both sides the same, because sodium fluoride is weak alkaline, ammonium fluoride aqueous solution is strong acid, thereby through the PH testing arrangement of pegging graft on rubber buffer 31, detect the pH nature in the aqueous solution, thereby whether the reflection contains impurity, at the dissolving process, the liquid level of holding vessel 1 is higher than spherical pipe 17, and after the saturation, along with inert gas's rush-in, lead to 1 pressure increase of holding vessel, the liquid level of liquid level pipe 16 descends, and then reflect the saturation of dissolving through the liquid level height.
The liquid pump 5 and the flow meter 25 are devices commonly used in the art and will not be described in detail.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The utility model provides a high-purity sodium fluoride separation and purification device in silicate production, includes heat preservation jar (1), its characterized in that: the lower end of the heat-insulating tank (1) is provided with a base (3), two groups of supporting upright posts (4) are arranged between the heat-insulating tank (1) and the base (3), the upper end of the heat-insulating tank (1) is hermetically provided with a cover plate (2), the lower end of the heat-insulating tank (1) is communicated with one side of a U-shaped pipe (13), the cover plate (2) is provided with a spherical spray head (6) which is controlled by a liquid pump (5) and extends to the inner cavity of the heat-insulating tank (1), the lower end of the U-shaped pipe (13) is placed on the upper end surface of the base (3), a port on one side of the U-shaped pipe (13) is provided with a first connecting block (14), a port on the other side of the U-shaped pipe (13) is provided with a second connecting block (15), the first connecting block (14) and the second connecting block (15) are arranged at equal height, the first connecting block (14) is communicated with the heat-insulating tank (1) and is vertically provided with a liquid level pipe (16), the upper end of the second connecting block (15) is vertically connected with a spherical pipe (17), the upper end of bulb (17) is passed through back flow pipe (18) and is communicated liquid pump (5), and the right side of bulb (17) is provided with drain pipe (22), the upper end intercommunication heat preservation jar inner chamber of (1) of liquid level pipe (16), the lower extreme of liquid level pipe (16) is provided with detects extension pipe (23).
2. The device for separating and purifying high-purity sodium fluoride in silicate production according to claim 1, characterized in that: a sealing ring groove (9) is formed between the upper end of the heat-insulating tank (1) and the lower end of the cover plate (2), a sealing ring (10) is arranged in the sealing ring groove (9), and the sealing ring (10) is tightly pressed at the lower end of the cover plate (2).
3. The device for separating and purifying high-purity sodium fluoride in silicate production according to claim 2, characterized in that: the heat-insulating cover plate is characterized in that lug seats (7) which are mutually pressed are arranged between the side wall of the heat-insulating tank (1) and the outer edge of the lower end of the cover plate (2), and the lug seats (7) are vertically symmetrical and are fixedly connected through fastening bolts (8) distributed in a circumferential array mode.
4. The device for separating and purifying high-purity sodium fluoride in silicate production according to claim 1, characterized in that: the upper end of apron (2) is provided with intake pipe (24), let in inert gas in intake pipe (24), inert gas is nitrogen gas or argon gas.
5. The device for separating and purifying high-purity sodium fluoride in silicate production according to claim 1, characterized in that: the inner chamber of heat preservation jar (1) sets up to washing inner chamber (11), the lower extreme right side of washing inner chamber (11) is provided with leakage fluid dram (12), the upper end of first connecting block (14) sets up two sets of first interface (26), and is two sets of first interface (26) communicate the lower extreme of leakage fluid dram (12) and liquid level pipe (16) respectively.
6. The device for separating and purifying high-purity sodium fluoride in silicate production according to claim 5, characterized in that: the outer walls of the liquid level pipe (16) and the spherical pipe (17) are vertically provided with scales, the upper end of the liquid level pipe (16) is provided with a communicating pipe (20) communicated with the inner cavity, the side wall of the washing inner cavity (11) is provided with an air hole (19), and the upper end of the communicating pipe (20) is inserted into the air hole (19).
7. The device for separating and purifying high-purity sodium fluoride in silicate production according to claim 6, characterized in that: the lower extreme of liquid level pipe (16) transversely extends and is provided with and detects extension pipe (23), the tip upper end of detecting extension pipe (23) is sealed through rubber buffer (31), end cover (27) fastening cover is passed through to the upper end of rubber buffer (31), be provided with through-hole (32) of intercommunication rubber buffer (31) up end on end cover (27).
8. The device for separating and purifying high-purity sodium fluoride in silicate production according to claim 1, characterized in that: the upper end of the second connecting block (15) is provided with a second interface (30), the lower end of the spherical pipe (17) is provided with a lower opening (29), and the spherical pipe (17) is communicated with the inner cavity of the U-shaped pipe (13) through the sealing connection of the lower opening (29) and the second interface (30).
9. The device for separating and purifying high-purity sodium fluoride in silicate production according to claim 1, characterized in that: an upper opening (28) is formed in the upper end of the spherical pipe (17), the return pipe (18) is connected with the upper opening (28) in an inserted mode, the other end of the return pipe (18) is communicated with the input end of the liquid pump (5), a flow meter (25) is arranged on the U-shaped pipe (13), and the flow rate of the liquid pump (5) is the same as the value of the flow meter (25).
10. The device for separating and purifying high-purity sodium fluoride in silicate production according to claim 1, characterized in that: an overflow groove (21) is formed in the right side of the spherical pipe (17), the liquid outlet pipe (22) is inserted into the overflow groove (21), and the lower end port of the return pipe (18) is located below the overflow groove (21).
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