CN116358253A - Potassium fluorotantalate drying and preserving equipment and method - Google Patents
Potassium fluorotantalate drying and preserving equipment and method Download PDFInfo
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- CN116358253A CN116358253A CN202310113615.4A CN202310113615A CN116358253A CN 116358253 A CN116358253 A CN 116358253A CN 202310113615 A CN202310113615 A CN 202310113615A CN 116358253 A CN116358253 A CN 116358253A
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- potassium
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- valve
- drying
- fluotantalate
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- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 157
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 157
- 239000011591 potassium Substances 0.000 title claims abstract description 157
- 238000001035 drying Methods 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000007599 discharging Methods 0.000 claims abstract description 43
- 238000006243 chemical reaction Methods 0.000 claims abstract description 42
- 238000001291 vacuum drying Methods 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000007789 gas Substances 0.000 claims abstract description 38
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 22
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 22
- 239000011734 sodium Substances 0.000 claims abstract description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 26
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
- 238000006073 displacement reaction Methods 0.000 claims description 12
- 229910021529 ammonia Inorganic materials 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 11
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 27
- 239000001301 oxygen Substances 0.000 abstract description 27
- 229910052760 oxygen Inorganic materials 0.000 abstract description 27
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 10
- RHDUVDHGVHBHCL-UHFFFAOYSA-N niobium tantalum Chemical compound [Nb].[Ta] RHDUVDHGVHBHCL-UHFFFAOYSA-N 0.000 description 6
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000007781 pre-processing Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 3
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 235000002639 sodium chloride Nutrition 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 239000011698 potassium fluoride Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
Images
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B9/00—Machines or apparatus for drying solid materials or objects at rest or with only local agitation; Domestic airing cupboards
- F26B9/06—Machines or apparatus for drying solid materials or objects at rest or with only local agitation; Domestic airing cupboards in stationary drums or chambers
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/001—Drying-air generating units, e.g. movable, independent of drying enclosure
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/14—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects using gases or vapours other than air or steam, e.g. inert gases
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
- F26B25/06—Chambers, containers, or receptacles
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Drying Of Solid Materials (AREA)
Abstract
The application provides potassium fluotantalate drying and preserving equipment and a potassium fluotantalate drying and preserving method. The potassium fluotantalate drying and preserving device comprises a vacuum drying device and a collector, wherein the collector is of a cylindrical hollow structure with two conical ends. The upper end and the lower end of the collector are provided with a first discharging valve and a second discharging valve, the collector is also provided with an air inlet valve and an air outlet valve, the first discharging valve is connected with a vacuum drying device, and the second discharging valve is connected with the reaction container. And the vacuum drying equipment is connected with a water ring vacuum pump and a Lotz vacuum pump. The potassium fluotantalate drying and preserving method is characterized in that the potassium fluotantalate drying and preserving equipment is used, water vapor and oxygen on the surface of the potassium fluotantalate are removed under ultrahigh vacuum, replacement gas is used for replacement, the dried potassium fluotantalate is packaged by a closed container, a sodium reduction potassium fluotantalate reaction container is communicated with the closed container, then the potassium fluotantalate is directly added, and the influence of the oxygen and the water vapor in the potassium fluotantalate on the potassium fluotantalate is reduced.
Description
Technical Field
The application relates to the field of tantalum-niobium production, and mainly relates to potassium fluotantalate drying and preserving equipment and method.
Background
In the tantalum-niobium production process, potassium fluotantalate is an important raw material of tantalum metal, and meanwhile, the quality of the potassium fluotantalate is directly related to the quality of a product. Drying potassium fluorotantalate, adding the potassium fluorotantalate into a reaction container, adding potassium chloride, sodium chloride, potassium fluoride and the like into the container, then introducing argon for replacement, heating, and finally adding metal sodium for reaction. Tantalum is an oxygen-related element that readily combines with oxygen to form stable compounds, and in sodium reduction processes, a molten salt system is required, with no oxygen present.
The potassium fluotantalate needs to be dried in the preparation process, and the potassium fluotantalate is directly added into a reaction kettle to participate in the reaction after being dried. In the process, as the potassium fluotantalate is in the aqueous solution, the surface of the potassium fluotantalate contains some aqueous solution which cannot be removed in the crystal, and meanwhile, the surface of the potassium fluotantalate particles also contains a large amount of oxygen. Because the surface also contains a large amount of water vapor and oxygen, the potassium fluotantalate still contains partial oxygen after being added into the reaction kettle, and the oxygen in the reaction kettle can not be completely replaced by the water vapor and the oxygen in the potassium fluotantalate although the oxygen in the reaction kettle is automatically replaced by argon at the bottom. Meanwhile, in the raw material transferring and feeding process, the raw material can be contacted with air, so that the influence of oxygen and water vapor in the air on potassium fluotantalate cannot be completely avoided. At present, the baking temperature of potassium fluotantalate is mostly about 150 ℃, at the temperature, potassium fluotantalate crystals are unchanged, when the temperature is higher than 150 ℃, the potassium fluotantalate crystals are crushed, and the inner holes are further exposed, so that water and oxygen are more favorably removed.
Disclosure of Invention
The application provides potassium fluotantalate drying and preserving equipment and a potassium fluotantalate drying and preserving method, which solve the problem that oxygen and water vapor influence the quality of potassium fluotantalate in the potassium fluotantalate drying and preserving process and the process of adding the potassium fluotantalate into a sodium reduction potassium fluotantalate reaction kettle. Meanwhile, the introduced gas containing nitrogen reacts with the tantalum powder in trace amount to generate tantalum nitride, so that the performance of the tantalum powder is further improved.
The potassium fluotantalate drying and preserving device comprises a vacuum drying device and a collector, wherein the collector is of a cylindrical hollow structure with two conical ends, a first discharging valve and a second discharging valve are arranged at the upper end and the lower end of the collector, the collector is provided with an air inlet valve and an air outlet valve at one end of the first discharging valve, the first discharging valve is connected with the vacuum drying device, and the second discharging valve is connected with a reaction container in a quick connection mode.
The device connects the drying device and the preservation device of potassium fluotantalate, namely, the vacuum drying equipment is connected with the collector, so that the drying of potassium fluotantalate and the whole storage process after drying can be guaranteed to avoid contact with air, and the influence of oxygen and water vapor on the quality of potassium fluotantalate is reduced. The device is also connected with the preservation device and the reaction container, namely the collector is connected with the reaction container, so that the contact between potassium fluotantalate materials and air is reduced as much as possible, and the influence of oxygen and water vapor on the quality of potassium fluotantalate is further reduced.
Optionally, the vacuum drying equipment is connected with a water ring vacuum pump and a lorentz vacuum pump.
Optionally, a check valve is arranged on the exhaust valve.
Optionally, the collector is lined with a tetrafluoro material.
Optionally, the vacuum drying device is characterized in that the inner lining is made of pure nickel-based materials.
Optionally, hang the material buckle on the collector outer wall along the diameter direction of collector cross section, hang the quantity of material buckle and be two, and distribute in the relative both sides of collector.
The application also provides a potassium fluotantalate drying and preserving method, which applies any one of the potassium fluotantalate drying and preserving equipment and comprises the following steps:
after potassium fluotantalate is added into vacuum drying equipment, a water ring vacuum pump is started, and the temperature is kept at 150-180 ℃ for drying for 2-4 hours under-0.06 Mpa;
turning on a Lotz vacuum pump, and keeping the temperature of 180-300 ℃ for 1-2 hours under 200-300Pa to obtain dried potassium fluotantalate;
closing a water ring vacuum pump and a Loz vacuum pump, opening a vacuum valve of vacuum drying equipment, introducing replacement gas, and cooling to room temperature, wherein the replacement gas is mixed gas of nitrogen-containing gas and argon, and the volume fraction of the nitrogen-containing gas is 10% -20%;
opening an exhaust valve of the collector, vacuumizing the collector, and closing the exhaust valve and the check valve;
opening an air inlet valve and introducing displacement air;
and opening a first discharge valve, transferring the dried potassium fluotantalate into the collector, and closing the first discharge valve.
Optionally, the gas containing nitrogen element comprises one or two of nitrogen and ammonia.
Optionally, the method further comprises:
after the first discharging valve is closed, carrying a collector filled with potassium fluorotantalate to the upper part of a sodium-reduced potassium fluorotantalate reactor, connecting a quick-connection valve on the quick-connection collector and a reaction kettle, opening a second discharging valve, and transferring the dried potassium fluorotantalate to a sodium-reduced potassium fluorotantalate reaction container.
The application provides a potassium fluotantalate stoving save equipment and method, wherein potassium fluotantalate stoving save equipment includes vacuum drying equipment and collector, the collector is the cylindrical hollow structure that both ends are the toper. The upper end and the lower end of the collector are provided with a first discharging valve and a second discharging valve, one end of the collector, which is provided with the first discharging valve, is also provided with an air inlet valve and an air outlet valve, the first discharging valve is connected with a vacuum drying device, and the second discharging valve is connected with a reaction container. And the vacuum drying equipment is connected with a water ring vacuum pump and a Lotz vacuum pump.
The potassium fluotantalate drying and preserving method is characterized in that the potassium fluotantalate drying and preserving equipment is used, water vapor and oxygen on the surface of the potassium fluotantalate are removed under ultrahigh vacuum, replacement gas is used for replacement, the dried potassium fluotantalate is packaged by a closed container, a sodium-reduced potassium fluotantalate reaction container is communicated with the closed container, then the potassium fluotantalate is directly added, contact with air is further avoided, the whole process is closed, and the influence of the oxygen and the water vapor in the potassium fluotantalate on the potassium fluotantalate is further reduced.
Drawings
In order to more clearly illustrate the technical solutions of the present application, the drawings that are needed in the embodiments will be briefly described below, and it will be obvious to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
Fig. 1 is a schematic view of a collector.
Legend description:
1-a first discharge valve; 2-a second discharge valve; 3-an intake valve; 4-exhaust valve; 5-hanging buckle.
Detailed Description
Reference will now be made in detail to the embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, the same numbers in different drawings refer to the same or similar elements, unless otherwise indicated. The embodiments described in the examples below are not intended to represent all embodiments consistent with the application. Merely as examples of systems and methods consistent with some aspects of the present application as detailed in the claims.
The potassium fluotantalate can be changed into small crystal powder at the temperature of more than 180 ℃, the holes in the potassium fluotantalate are completely opened, the related water, air and the like wrapped in the crystal can be completely released, and then the water and oxygen in the potassium fluotantalate are further removed through vacuum filtration.
The potassium fluotantalate drying and preserving device comprises a vacuum drying device and a collector, wherein the collector is of a cylindrical hollow structure with two conical ends, a first discharging valve 1 and a second discharging valve 2 are arranged at the upper end and the lower end of the collector, the collector is provided with an air inlet valve 3 and an air outlet valve 4 which are also arranged at one end of the first discharging valve 1, the first discharging valve 1 is connected with the vacuum drying device, and the second discharging valve 2 is connected with a reaction container in a quick connection mode.
The device connects the drying device and the preservation device of potassium fluotantalate, namely, the vacuum drying equipment is connected with the collector, so that the drying of potassium fluotantalate and the whole storage process after drying can be guaranteed to avoid contact with air, and the influence of oxygen and water vapor on the quality of potassium fluotantalate is reduced. The device is also connected with the preservation device and the reaction container for preparing tantalum powder by reducing potassium fluorotantalate by sodium, namely the collector is connected with the reaction container, so that the contact between potassium fluorotantalate materials and air is reduced as much as possible, and the influence of oxygen and water vapor on potassium fluorotantalate and on the quality of tantalum powder is further reduced.
In some embodiments, a water ring vacuum pump and a lorentz vacuum pump are connected to the vacuum drying device.
The two vacuum pumps are connected, so that the vacuum degree of the vacuum drying equipment reaches 200-300Pa.
In some embodiments, a non-return valve is provided on the exhaust valve 4.
The check valve is arranged on the exhaust valve 4 to prevent air from entering the collector, so that potassium fluorotantalate material is prevented from contacting with air, and the influence of oxygen and water vapor on the quality of potassium fluorotantalate is reduced.
In some embodiments, the collector is lined with a tetrafluoro material.
The collector lined with the tetrafluoro material has excellent temperature resistance and corrosion resistance, can stably work under the high-temperature limit negative pressure working condition for a long time, and can meet the requirements of drying and preserving potassium fluotantalate.
In some embodiments, the vacuum drying apparatus is lined with pure nickel.
The vacuum drying equipment lined with pure nickel has hydrofluoric acid corrosion resistance, can work at 180-300 ℃, and can meet the drying requirement of potassium fluotantalate. The baked potassium fluotantalate becomes powder, which is more beneficial to removing oxygen and moisture. The oxidation of a reaction kettle and a stirring paddle in the process of preparing tantalum powder by reducing potassium fluorotantalate by sodium is prevented, and the influence on the quality of the tantalum powder is prevented;
in some embodiments, hanging material buckles 5 are arranged on the outer wall of the collector along the diameter direction of the cross section of the collector, and the number of the hanging material buckles 5 is two and distributed on two opposite sides of the collector.
The hanging buckle 5 can be clamped on the platform to fix the collector.
In some embodiments, the gas is a mixed gas of nitrogen-containing gas and argon, wherein the volume fraction of the nitrogen-containing gas is 10% -20%, and the nitrogen-containing gas comprises one or two of nitrogen and ammonia.
The argon is used for replacing air in potassium fluotantalate, so that the contact with oxygen is avoided, part of the introduced nitrogen-containing gas reacts with tantalum powder to generate tantalum nitride, and the nitrogen-containing gas with the proportion of 10% -20% is beneficial to generating fine tantalum nitride, so that the performance of the tantalum powder can be further improved.
The application also provides a potassium fluotantalate drying and preserving method, and the potassium fluotantalate drying and preserving equipment is applied to any one of the above.
Example 1:
and (3) placing 100kg of centrifuged potassium fluotantalate into a belt dryer, and drying and preprocessing at 180 ℃ to obtain preprocessed potassium fluotantalate. Adding pretreated potassium fluorotantalate into vacuum drying equipment of potassium fluorotantalate, firstly, opening a water ring vacuum pump, vacuumizing to-0.06 Mpa, and keeping the temperature at 150 for 2 hours; then, the Lotz vacuum pump was turned on, the vacuum in the vessel was maintained at 200Pa, and the vessel was baked at 180℃for 1 hour. And closing the water ring vacuum pump and the Lotz vacuum pump, opening a vacuum valve of the vacuum drying equipment, introducing replacement gas, and cooling to room temperature. Opening an exhaust valve 4 of the collector, vacuumizing the collector, and closing the exhaust valve 4 and the check valve; opening the air inlet valve 3 and introducing the displacement air; and opening the first discharge valve 1, transferring the dried potassium fluotantalate into the collector, and closing the first discharge valve 1. After the first discharging valve is closed, 1, carrying a collector filled with potassium fluorotantalate to the upper part of a reactor for sodium reduction of potassium fluorotantalate, connecting a quick-connection valve on the quick-connection collector and a reaction kettle, opening a second discharging valve 2, transferring the dried potassium fluorotantalate to a sodium reduction potassium fluorotantalate reaction container, entering a potassium sodium fluorotantalate reduction step, placing materials into the reaction container, discharging while introducing replacement gas, and realizing the whole-process airtight transportation. The displacement gas is a mixture of argon and ammonia, wherein the ammonia content is 10%.
Example 2:
and (3) placing 100kg of centrifuged potassium fluotantalate into a belt dryer, and drying and preprocessing at 180 ℃ to obtain preprocessed potassium fluotantalate. Adding pretreated potassium fluorotantalate into vacuum drying equipment of potassium fluorotantalate, firstly, opening a water ring vacuum pump, vacuumizing to-0.06 Mpa, and keeping the temperature at 170 ℃ for 3 hours; then, the Lotz vacuum pump was turned on, the vacuum in the vessel was maintained at 300Pa, and the vessel was baked at 180℃for 2 hours. And closing the water ring vacuum pump and the Lotz vacuum pump, opening a vacuum valve of the vacuum drying equipment, introducing replacement gas, and cooling to room temperature. Opening an exhaust valve 4 of the collector, vacuumizing the collector, and closing the exhaust valve 4 and the check valve; opening the air inlet valve 3 and introducing the displacement air; and opening the first discharge valve 1, transferring the dried potassium fluotantalate into the collector, and closing the first discharge valve 1. After the first discharging valve is closed, 1, carrying a collector filled with potassium fluorotantalate to the upper part of a reactor for sodium reduction of potassium fluorotantalate, connecting a quick-connection valve on the quick-connection collector and a reaction kettle, opening a second discharging valve 2, transferring the dried potassium fluorotantalate to a sodium reduction potassium fluorotantalate reaction container, entering a potassium sodium fluorotantalate reduction step, placing materials into the reaction container, discharging while introducing replacement gas, and realizing the whole-process airtight transportation. The displacement gas is a mixture of argon, nitrogen and ammonia, wherein the content of the nitrogen and the ammonia is 20%.
Example 3:
and (3) placing 100kg of centrifuged potassium fluotantalate into a belt dryer, and drying and preprocessing at 180 ℃ to obtain preprocessed potassium fluotantalate. Adding pretreated potassium fluorotantalate into vacuum drying equipment of potassium fluorotantalate, firstly, opening a water ring vacuum pump, vacuumizing to-0.06 Mpa, and drying at 160 ℃ for 4 hours; then, the Lotz vacuum pump was turned on, the vacuum in the vessel was kept at 250Pa, and the temperature was kept at 300℃for 2 hours. And closing the water ring vacuum pump and the Lotz vacuum pump, opening a vacuum valve of the vacuum drying equipment, introducing replacement gas, and cooling to room temperature. Opening an exhaust valve 4 of the collector, vacuumizing the collector, and closing the exhaust valve 4 and the check valve; opening the air inlet valve 3 and introducing the displacement air; and opening the first discharge valve 1, transferring the dried potassium fluotantalate into the collector, and closing the first discharge valve 1. After the first discharging valve is closed, 1, carrying a collector filled with potassium fluorotantalate to the upper part of a reactor for sodium reduction of potassium fluorotantalate, connecting a quick-connection valve on the quick-connection collector and a reaction kettle, opening a second discharging valve 2, transferring the dried potassium fluorotantalate to a sodium reduction potassium fluorotantalate reaction container, entering a potassium sodium fluorotantalate reduction step, placing materials into the reaction container, discharging while introducing replacement gas, and realizing the whole-process airtight transportation. The displacement gas is a mixture of argon and nitrogen, wherein the nitrogen content is 15%.
Example 4:
and (3) placing 100kg of centrifuged potassium fluotantalate into a belt dryer, and drying and preprocessing at 180 ℃ to obtain preprocessed potassium fluotantalate. Adding pretreated potassium fluorotantalate into vacuum drying equipment of potassium fluorotantalate, firstly, opening a water ring vacuum pump, vacuumizing to-0.06 Mpa, and drying for 3 hours at 180 ℃; then, the Lotz vacuum pump was turned on, the vacuum in the vessel was maintained at 270Pa, and the temperature was kept at 200℃for 2 hours. And closing the water ring vacuum pump and the Lotz vacuum pump, opening a vacuum valve of the vacuum drying equipment, introducing replacement gas, and cooling to room temperature. Opening an exhaust valve 4 of the collector, vacuumizing the collector, and closing the exhaust valve 4 and the check valve; opening the air inlet valve 3 and introducing the displacement air; and opening the first discharge valve 1, transferring the dried potassium fluotantalate into the collector, and closing the first discharge valve 1. After the first discharging valve is closed, 1, carrying a collector filled with potassium fluorotantalate to the upper part of a reactor for sodium reduction of potassium fluorotantalate, connecting a quick-connection valve on the quick-connection collector and a reaction kettle, opening a second discharging valve 2, transferring the dried potassium fluorotantalate to a sodium reduction potassium fluorotantalate reaction container, entering a potassium sodium fluorotantalate reduction step, placing materials into the reaction container, discharging while introducing replacement gas, and realizing the whole-process airtight transportation. The displacement gas is a mixture of argon, ammonia and nitrogen, wherein the ammonia and nitrogen content is 17%.
Comparative example:
and (3) placing 100kg of centrifuged potassium fluotantalate into a belt dryer, and drying and preprocessing at 150 ℃ to obtain preprocessed potassium fluotantalate. Adding pretreated potassium fluorotantalate into vacuum drying equipment of potassium fluorotantalate, firstly, opening a water ring vacuum pump, vacuumizing to-0.06 Mpa, and drying at 150 ℃ for 3 hours; then, the Lotz vacuum pump was turned on, the vacuum in the container was maintained at 2400Pa, and the temperature was kept at 180℃for 2 hours. And closing the water ring vacuum pump and the Lotz vacuum pump, opening a vacuum valve of the vacuum drying equipment, introducing replacement gas, and cooling to room temperature. Opening an exhaust valve 4 of the collector, vacuumizing the collector, and closing the exhaust valve 4 and the check valve; opening the air inlet valve 3 and introducing the displacement air; and opening the first discharge valve 1, transferring the dried potassium fluotantalate into the collector, and closing the first discharge valve 1. After the first discharging valve is closed, 1, carrying a collector filled with potassium fluorotantalate to the upper part of a reactor for sodium reduction of potassium fluorotantalate, connecting a quick-connection valve on the quick-connection collector and a reaction kettle, opening a second discharging valve 2, transferring the dried potassium fluorotantalate to a sodium reduction potassium fluorotantalate reaction container, entering a potassium sodium fluorotantalate reduction step, placing materials into the reaction container, discharging while introducing replacement gas, and carrying out whole-process airtight transportation to prepare the first tantalum niobium. The displacement gas is a mixture of argon, ammonia and nitrogen, wherein the nitrogen and ammonia content is 17%.
100kg of potassium fluotantalate is dried on a belt dryer at 180 ℃, and then is added into vacuum drying equipment of potassium fluotantalate, firstly, vacuum is pumped to-0.06 Mpa, the temperature is kept at 180 ℃ for drying for 3 hours, then, the air is broken, and the plastic barrel is placed. And (3) entering a potassium sodium fluotantalate reduction step, and placing the materials into a potassium fluotantalate reaction container to prepare the second tantalum niobium.
The purity of the first tantalum niobium is 99.5% and the purity of the second tantalum niobium is 96.5%, so that the potassium fluotantalate prepared by the potassium fluotantalate drying and preserving method avoids the influence of oxygen and water vapor, has better quality and has higher purity.
The application provides a potassium fluotantalate stoving save equipment and method, wherein potassium fluotantalate stoving save equipment includes vacuum drying equipment and collector, the collector is the cylindrical hollow structure that both ends are the toper. The upper end and the lower end of the collector are provided with a first discharging valve and a second discharging valve, one end of the collector, which is provided with the first discharging valve, is also provided with an air inlet valve and an air outlet valve, the first discharging valve is connected with a vacuum drying device, and the second discharging valve is connected with a reaction container. And the vacuum drying equipment is connected with a water ring vacuum pump and a Lotz vacuum pump.
The potassium fluotantalate drying and preserving method is characterized in that the potassium fluotantalate drying and preserving equipment is used, water vapor and oxygen on the surface of the potassium fluotantalate are removed under ultrahigh vacuum, replacement gas is used for replacement, the dried potassium fluotantalate is packaged by a closed container, a sodium-reduced potassium fluotantalate reaction container is communicated with the closed container, then the potassium fluotantalate is directly added, contact with air is further avoided, the whole process is closed, and the influence of the oxygen and the water vapor in the potassium fluotantalate on the potassium fluotantalate is further reduced.
The foregoing detailed description of the embodiments is merely illustrative of the general principles of the present application and should not be taken in any way as limiting the scope of the invention. Any other embodiments developed in accordance with the present application without inventive effort are within the scope of the present application for those skilled in the art.
Claims (10)
1. The utility model provides a potassium fluorotantalate stoving save equipment, its characterized in that, includes vacuum drying equipment and collector, the collector is the cylindrical hollow structure that both ends are the toper, both ends are provided with first blowing valve (1) and second blowing valve (2) about the collector, and the collector sets up one end of first blowing valve (1) still is provided with admission valve (3) and discharge valve (4), first blowing valve (1) are connected with vacuum drying equipment, second blowing valve (2) connect soon with reaction vessel and are connected.
2. The potassium fluorotantalate drying and preserving apparatus of claim 1 wherein the vacuum drying apparatus is connected with a water ring vacuum pump and a lorentz vacuum pump.
3. The potassium fluorotantalate drying and preserving apparatus of claim 1 wherein the vacuum drying apparatus is lined with a pure nickel-based material.
4. The potassium fluorotantalate drying and preserving apparatus of claim 1 wherein the vacuum drying apparatus is a drying temperature of 180-300 ℃.
5. The potassium fluorotantalate drying and preserving apparatus as claimed in claim 1, wherein the exhaust valve (4) is provided with a non-return valve.
6. The potassium fluorotantalate dry storage apparatus of claim 5 wherein the collector is lined with tetrafluoro material.
7. The potassium fluotantalate drying and preserving device according to claim 6, wherein hanging material buckles (5) are arranged on the outer wall of the collector along the diameter direction of the cross section of the collector, and the number of the hanging material buckles (5) is two and distributed on two opposite sides of the collector.
8. A potassium fluorotantalate baking and preserving method, using the potassium fluorotantalate baking and preserving apparatus as claimed in any one of claims 1 to 7, characterized by comprising:
after potassium fluotantalate is added into vacuum drying equipment, a water ring vacuum pump is started, and the temperature is kept at 150-180 ℃ for drying for 2-4 hours under-0.06 Mpa;
turning on a Lotz vacuum pump, and keeping the temperature of 180-300 ℃ for 1-2 hours under 200-300Pa to obtain dried potassium fluotantalate;
closing a water ring vacuum pump and a Loz vacuum pump, opening a vacuum valve of vacuum drying equipment, introducing replacement gas, and cooling to room temperature, wherein the replacement gas is mixed gas of nitrogen-containing gas and argon, and the volume fraction of the nitrogen-containing gas is 10% -20%;
opening an exhaust valve of the collector, vacuumizing the collector, and closing the exhaust valve and the check valve;
opening an air inlet valve and introducing displacement air;
and opening a first discharge valve, transferring the dried potassium fluotantalate into the collector, and closing the first discharge valve.
9. The method for dry-keeping potassium fluorotantalate according to claim 8, wherein the nitrogen-containing gas includes one or both of nitrogen and ammonia.
10. The method for dry preservation of potassium fluorotantalate according to claim 9, further comprising:
after the first discharging valve is closed, carrying a collector filled with potassium fluorotantalate to the upper part of a sodium-reduced potassium fluorotantalate reactor, connecting a quick-connection valve on the quick-connection collector and a reaction kettle, opening a second discharging valve, and transferring the dried potassium fluorotantalate to a sodium-reduced potassium fluorotantalate reaction container.
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| US20040038415A1 (en) * | 2001-09-27 | 2004-02-26 | Yoshitsugu Uchino | Method for producing potassium fluorotantalate crystal being low in oxygen content and method for producing potassium fluoroniobate crystal being low in oxygen content, potassium fluorotantalate crystal bein low in oxygen content and potassium fluoroniobate crystal bein low in oxygen produced by the methods, a |
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