CN113083160A - Multifunctional molten salt system - Google Patents
Multifunctional molten salt system Download PDFInfo
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- CN113083160A CN113083160A CN202110383065.9A CN202110383065A CN113083160A CN 113083160 A CN113083160 A CN 113083160A CN 202110383065 A CN202110383065 A CN 202110383065A CN 113083160 A CN113083160 A CN 113083160A
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- 150000003839 salts Chemical class 0.000 title claims abstract description 220
- 239000000463 material Substances 0.000 claims abstract description 138
- 238000010438 heat treatment Methods 0.000 claims abstract description 76
- 239000007788 liquid Substances 0.000 claims abstract description 71
- 239000012535 impurity Substances 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 230000001681 protective effect Effects 0.000 claims abstract description 16
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 30
- 235000019270 ammonium chloride Nutrition 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 10
- 239000011343 solid material Substances 0.000 claims description 9
- 239000002893 slag Substances 0.000 claims description 6
- 230000001502 supplementing effect Effects 0.000 claims description 5
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 239000010431 corundum Substances 0.000 claims description 3
- 238000003795 desorption Methods 0.000 claims description 3
- 229910001119 inconels 625 Inorganic materials 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 206010039509 Scab Diseases 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 abstract description 46
- 239000000956 alloy Substances 0.000 abstract description 46
- 229910052751 metal Inorganic materials 0.000 abstract description 34
- 239000002184 metal Substances 0.000 abstract description 34
- 238000000034 method Methods 0.000 abstract description 34
- 230000008569 process Effects 0.000 abstract description 29
- 238000005275 alloying Methods 0.000 abstract description 23
- 230000003647 oxidation Effects 0.000 abstract description 19
- 238000007254 oxidation reaction Methods 0.000 abstract description 19
- 238000002844 melting Methods 0.000 abstract description 16
- 230000008018 melting Effects 0.000 abstract description 16
- 230000001276 controlling effect Effects 0.000 description 16
- 230000007062 hydrolysis Effects 0.000 description 16
- 238000006460 hydrolysis reaction Methods 0.000 description 16
- 239000007789 gas Substances 0.000 description 14
- 238000002360 preparation method Methods 0.000 description 12
- 239000000047 product Substances 0.000 description 8
- 238000011065 in-situ storage Methods 0.000 description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 6
- 230000004907 flux Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000010309 melting process Methods 0.000 description 6
- 239000013049 sediment Substances 0.000 description 6
- 239000011261 inert gas Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 229910000861 Mg alloy Inorganic materials 0.000 description 3
- 238000007667 floating Methods 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000003570 air Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910004835 Na2B4O7 Inorganic materials 0.000 description 1
- 229910000978 Pb alloy Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- IZJSTXINDUKPRP-UHFFFAOYSA-N aluminum lead Chemical compound [Al].[Pb] IZJSTXINDUKPRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 150000001805 chlorine compounds Chemical group 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 229910001610 cryolite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000006052 feed supplement Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000009853 pyrometallurgy Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011833 salt mixture Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
- B01J6/005—Fusing
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/04—Electrolytic production, recovery or refining of metals by electrolysis of melts of magnesium
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The invention provides a multifunctional molten salt system which comprises a preheating impurity removal unit, a feeding protection unit and a molten salt heating/reaction unit, wherein the preheating impurity removal unit is used for removing impurities from molten salt; the molten salt heating/reaction unit comprises a molten salt furnace and a lower heating assembly; the inner cavity of the molten salt furnace is divided into a liquid molten salt area at the lower part and a protective atmosphere area at the upper part, and the heating assembly at the lower part is positioned at the bottom of the liquid molten salt area; the preheating and impurity removing unit comprises a material conveying pipe inserted in the molten salt furnace, a stirring rod arranged in the conveying pipe and an upper heating assembly arranged outside the outer end of the conveying pipe, and the bottom end of the material conveying pipe is positioned in the liquid molten salt area; the feeding protection unit comprises a molten salt support piece arranged in the liquid molten salt area and a spiral feeder arranged at the lower end of the stirring rod; the lower pipe orifice of the material conveying pipe is connected with the feeding port of the molten salt support piece, and the bottom of the spiral feeder is spaced from the surface of the liquid molten salt. The invention greatly reduces the oxidation burning loss of the metal (or alloy) in the high-temperature melting (or alloying) process and increases the process safety.
Description
Technical Field
The invention relates to the technical field of high-purity molten salt preparation, in particular to a multifunctional molten salt system.
Background
Many metals or alloys (such as alkali metals, alkaline earth metals, rare earth metals and alloys thereof) are easily damaged by high-temperature oxidation and even violently exploded during melting or further alloying. For example, in the preparation of rare earth-containing alloys, rare earth elements are highly reactive at high temperatures and can easily react with the ambient atmosphere during pyrometallurgical processes, resulting in the loss of expensive rare earth metals. For another example, magnesium alloys are easily oxidized at high temperatures for a short period of time to release a large amount of heat during melting or preparation at high temperatures, thereby causing severe combustion or even explosion. In addition, many molten salts contain easily hydrolyzable substances, which cause severe hydrolysis when contacting with ambient gas at high temperature, and greatly affect the physicochemical properties. For example, KCl-NaCl-MgCl is commonly used in the process of preparing magnesium metal by electrolysis2-CaCl2A quaternary chloride electrolyte melt. The anhydrous magnesium chloride is easy to hydrolyze in the melt preparation or high-temperature standing process, so that a large amount of hydrolysis products are generated, and the subsequent electrolysis process is seriously influenced. Therefore, reducing the high-temperature oxidation of the metal or alloy and reducing the high-temperature hydrolysis of the molten salt are the key points for safe production and cost reduction in many metal or alloy preparation industries. Currently, the following technologies exist:
(1) and (5) vacuum protection. The container filled with the easily oxidized metal (or alloy) or the easily hydrolyzed molten salt is vacuumized to reduce the content of oxygen-containing gas to a certain level, and then heating operation is carried out, so that the probability of oxidation or hydrolysis is reduced by reducing the contact chance of the materials and air. For example, Sun Tian et al propose a vacuum ladle system for protecting anhydrous magnesium chloride melt (see the literature: application of magnesium chloride discharged by vacuum method in the production of titanium sponge, light metal, 2017 (3)). The system comprises a heat-preservation vacuum ladle, a hook scale, a vacuum pipeline, a three-way valve, a metal hose and a vacuum pump, wherein the chloride molten salt is discharged out of the ladle by a vacuum pumping method, so that the hydrolysis of the high-temperature chloride molten salt is greatly reduced. However, the method is complicated in operation process and high in requirement on sealing performance, and the production cost is greatly increased.
(2) And (5) protecting by inert gas. Inert gas is introduced into a container for containing high-temperature easily-oxidized metal (or alloy) or easily-hydrolyzed molten salt, so that the inert gas is filled on the surface of the material, and the probability of the contact of the ambient atmosphere and the material is reduced. For example, in magnesium metal smelting process, a large amount of SF is introduced into a container6The gas or other inert gases react with the high-temperature magnesium liquid to form a layer of compact and continuous protective film with metallic luster on the surface of the magnesium liquid, thereby protecting the magnesium liquid. However, since the protective film can be maintained at a high temperature for only several minutes, the protective gas is continuously supplied, thereby increasing the production cost.
(3) And covering and protecting the flux. The flux covering protection is to cover the surface of the metal (or alloy) or chloride melt to be protected with solid salt mixture, so as to reduce the contact area between the metal (or alloy) or chloride melt and achieve the purpose of high temperature protection. For example, the invention described in patent CN1162562C will contain NaCl, KCl, (La, Ce) F3、CaCO3、Na3AlF6And Na2B4O7The flux is covered on the surface of the aluminum-lead alloy melt, and the melt is protected at high temperature by utilizing the characteristics of small density and good covering property of the flux, so that the volatilization and burning loss of lead are reduced to the level of 1 percent. However, the flux is difficult to separate completely from the protected melt, thereby forming flux inclusions in the alloy melt, which greatly affect the overall properties of the alloy.
The multifunctional molten salt furnace is developed to solve the problems of oxidation and hydrolysis in the high-temperature smelting process, and has profound significance for magnesium metal and alloy production and accelerating further application of high-purity molten salt. Currently, the following problems exist in this aspect of research:
(1) the function is single, and the application in many occasions can not be realized. Because the high-temperature hydrolysis of the molten salt and the high-temperature oxidation mechanism of the metal (or alloy) are different, the device is highly specialized and cannot be used universally. For example, a magnesium alloy smelting furnace independently developed by Chongqing university can realize instant protection in the magnesium alloy smelting process, but for a high-temperature molten salt system, from the furnace structure, high-temperature hydrolysis of molten salt cannot be effectively avoided.
(2) The safety of the process is poor, and major accidents are easily caused. The oxidizable metal or alloy is easily subjected to violent oxidation in a high-temperature heating process, and generates a large amount of heat in a short time, so that combustion or explosion is initiated. Protective gas, inert gas or vacuum technology can only slow down the high-temperature oxidation rate, cannot effectively isolate the contact between metal or alloy and air, and still has great potential safety hazard.
Disclosure of Invention
The invention aims to solve the technical problem of providing a multifunctional molten salt system aiming at the defects of the prior art, realizing the melting and alloying (alloying for alloy blending or in-situ alloying of molten salt) of easily-oxidized metal or alloy in a molten salt medium, and greatly reducing the oxidation burning loss. In addition, the invention greatly reduces the hydrolysis in the molten salt preparation process and realizes the preparation of high-purity molten salt.
In order to solve the above technical problems, the present invention comprises:
a multifunctional molten salt system comprises a preheating impurity removal unit, a feeding protection unit and a molten salt heating/reaction unit; the molten salt heating/reaction unit comprises a molten salt furnace and a lower heating assembly arranged in the molten salt furnace; the inner cavity of the molten salt furnace is divided into a liquid molten salt area at the lower part and a protective atmosphere area at the upper part, and the lower part heating assembly is positioned at the bottom of the liquid molten salt area; the lower heating assembly is used for heating the solid molten salt into liquid molten salt and heating materials added into the liquid molten salt; the preheating impurity removal unit comprises a material conveying pipe vertically inserted into the molten salt furnace, a stirring rod arranged in the material conveying pipe, an upper heating assembly arranged outside the outer end of the material conveying pipe and a charging opening arranged at the top of the material conveying pipe, and the bottom end of the material conveying pipe is positioned in the liquid molten salt area; the feeding protection unit comprises a molten salt support piece arranged in the liquid molten salt area and positioned below the material conveying pipe and a spiral feeder arranged at the lower end of the stirring rod; the lower pipe orifice of the material conveying pipe is connected with the feeding hole of the molten salt support piece, and the bottom of the spiral feeder is spaced from the surface of the liquid molten salt; the spiral feeder is used for preventing most materials from directly falling into the liquid molten salt and controlling the downward speed of the materials by controlling the propelling speed of the spiral feeder; the material in the material conveying pipe is heated jointly through the high-temperature molten salt in upper portion heating element and the liquid molten salt district, and when the lower material of temperature contacted with the high-temperature molten salt, through the addition of control fused salt temperature and low temperature material for the fused salt surface crusts owing to exothermic solidification, thereby supports the solid material on upper portion, makes the material pile up in the material conveying pipe, realizes preheating and the desorption of partial impurity of material.
Further, the ratio of the height to the diameter of the material conveying pipe is 0.5-35.0.
Furthermore, the upper end of the material conveying pipe is provided with a transverse exhaust pipeline through an exhaust connecting piece.
Furthermore, the difference between the inner diameter of the material conveying pipe and the diameter of the blade of the spiral feeder is 0.5-5.0 mm.
Furthermore, a thermocouple and a liquid level measurer for respectively measuring the internal temperature and the molten salt liquid level of the molten salt furnace are arranged at the top of the molten salt furnace.
Furthermore, the top of the molten salt furnace is provided with a feeding port which is used for adding and supplementing solid molten salt into the molten salt furnace and adding ammonium chloride at regular time to ensure protective atmosphere above the molten salt furnace.
Furthermore, a discharge hole is formed in the side wall of the molten salt furnace and is located below the liquid level of the liquid molten salt, and a slag hole is formed in the bottom of the molten salt furnace.
Furthermore, an overflow hole is formed in the middle of the side face of the molten salt support piece.
Furthermore, the material of the stirring rod and the screw feeder is any one or any two of corundum, silicon carbide, Inconel 625 and ceramic.
The invention has the beneficial effects that:
according to the invention, by controlling the material heating temperature and the descending speed, the solid material can be preheated and part of impurities can be removed in the preheating and impurity removing unit; by controlling the propelling speed of the spiral feeder, the solid materials can be melted in an immersion manner in the feeding protection unit, so that the oxidation or hydrolysis in the melting process is greatly reduced; the melting or alloying of the materials is realized through the protection of the liquid molten salt of the molten salt heating/reaction unit. The multifunctional molten salt furnace can realize the protective melting, alloying (alloying for alloy blending or in-situ alloying of molten salt) and the preparation of high-purity easily-hydrolyzed molten salt of easily-oxidized burning loss metal or alloy. The invention has profound significance for the production of easily oxidized metal or alloy and the further application of high-purity molten salt.
Compared with the prior device, the invention has the advantages that: (1) the multifunctional mobile phone can realize multiple applications: the melting and alloying (alloying for alloy blending or in-situ alloying of molten salt) of the easily oxidized metal or alloy and the preparation of high-purity easily hydrolyzed molten salt can be realized, and the oxidation burning loss and hydrolysis in the heating process are greatly reduced; (2) whole protection, process safety: the furnace body has a special structure, so that the added materials can be accumulated in a certain mode, and the whole-course protection of the heating process can be realized by regulating and controlling the heating temperature, the melting speed of the materials and the escape speed of the protective gas (steam volatilized by molten salt and gas released by ammonium chloride decomposition); in addition, the fused salt is a good flame retardant, and can ensure the safety in the heating process.
Drawings
FIG. 1 is a schematic view showing the composition of the multifunctional molten salt furnace of the present invention.
In the figure: 1-upper heating component, 2-material conveying pipe, 3-exhaust connecting piece, 4-exhaust pipeline, 5-charging opening, 6-stirring rod, 7-spiral feeder, 8-molten salt supporting piece, 9-overflow hole, 10-molten salt furnace, 11-lower heating component, 12-thermocouple, 13-liquid level measurer, 14-feeding opening, 15-discharging opening and 16-slag outlet.
Detailed Description
For the purpose of promoting an understanding of the invention, reference will now be made in detail to the present embodiments of the invention, examples of which are illustrated in the accompanying drawings. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
As shown in FIG. 1, the invention provides a multifunctional molten salt system, which comprises a preheating impurity removal unit, a feeding protection unit and a molten salt heating/reaction unit; the molten salt heating/reaction unit comprises a molten salt furnace 10 and a lower heating assembly 11 arranged in the molten salt furnace 10; the inner cavity of the molten salt furnace 10 is divided into a liquid molten salt area at the lower part and a protective atmosphere area at the upper part, and the lower heating component 11 is positioned at the bottom of the liquid molten salt area; the lower heating assembly 11 is used for heating the solid molten salt into liquid molten salt and heating the materials added into the liquid molten salt; the preheating and impurity removing unit comprises a material conveying pipe 2 vertically inserted into the molten salt furnace 10, a stirring rod 6 arranged in the material conveying pipe 2, an upper heating assembly 1 arranged outside the outer end of the material conveying pipe 2 and a charging opening 5 arranged at the top of the material conveying pipe 2, wherein the bottom end of the material conveying pipe 2 is positioned in a liquid molten salt region; the feeding protection unit comprises a molten salt support member 8 arranged in the liquid molten salt area and positioned below the material conveying pipe 2 and a spiral feeder 7 arranged at the lower end of the stirring rod 6; and an overflow hole 9 is arranged in the middle of the side surface of the molten salt support 8. The lower pipe opening of the material conveying pipe 2 is connected with the feeding hole of the molten salt supporting piece 8, and the bottom of the spiral feeder 7 is spaced from the surface of the liquid molten salt; the spiral feeder 7 is used for preventing most materials from directly falling into the liquid molten salt and controlling the descending speed of the materials by controlling the propelling speed of the materials; the material of high temperature fused salt in through upper portion heating element 1 and the liquid fused salt district in to material conveying pipe 2 heats jointly, when the lower material of temperature and high temperature fused salt contact, through the addition of control fused salt temperature and low temperature material for the fused salt surface is because exothermic solidification encrusts, thereby supports the solid material on upper portion, makes the material pile up in material conveying pipe 2, realizes preheating and the desorption of partial impurity of material.
The ratio of the height to the diameter of the material-conveying pipe 2 is 0.5 to 35.0, preferably 1.5 to 30.0, and more preferably 2.5 to 25.0.
The upper end of the material conveying pipe 2 is provided with a transverse exhaust pipeline 4 through an exhaust connecting piece 3.
The top of the material conveying pipe 2 is provided with a stirring motor, and the top of the stirring rod 6 is connected with an output shaft of the stirring motor; the screw feeder 7 is arranged at the position where the material conveying pipe 2 is connected with the top of the molten salt furnace 10. The spiral feeder 7 plays the roles of quantitatively propelling materials, reducing the contact area of metal or alloy and air, uniformly stirring and regulating the escape speed of protective gas. The material of the stirring rod 6 and the screw feeder 7 is any one or any two of corundum, silicon carbide, Inconel 625 and ceramic.
The difference between the inner diameter of the material conveying pipe 2 and the diameter of the blade of the spiral feeder 7 is 0.5-5.0mm, so that most materials can be prevented from directly falling into the liquid molten salt and being accumulated in the pipe; the material heating temperature is controlled by the temperature of the upper heating component 1 outside the outer end of the material conveying pipe 2 and the temperature of the molten salt at the bottom; when the added low-temperature material is in contact with the high-temperature molten salt, the surface of the molten salt can be crusted due to exothermic solidification by controlling the temperature of the molten salt and the adding amount of the low-temperature material, so that the solid material on the upper part is supported, and the material is accumulated in the pipe. Therefore, the melting speed of the material is controlled by the temperature of the molten salt at the bottom, and the descending speed of the material is controlled by the propelling speed of the screw feeder 7.
The molten salt furnace 10 adopts any one or combination of any two of internal electrode heating, heating assembly external heating and gas external heating. The heating temperature of the preheating and impurity removing unit is 650 ℃, preferably 350-600 ℃, and further preferably 380-580 ℃; the ratio of the height of the molten salt liquid level in the molten salt heating/reaction unit to the height of the molten salt furnace 10 is 0.10 to 0.95, preferably 0.20 to 0.90, and more preferably 0.30 to 0.80.
The top of the molten salt furnace 10 is provided with a thermocouple 12 and a liquid level measurer 13 for measuring the internal temperature and the molten salt liquid level of the molten salt furnace, respectively. The top of the molten salt furnace 10 is provided with a feeding port 14 for feeding and supplementing solid molten salt into the molten salt furnace 10 and adding ammonium chloride at regular time to ensure a protective atmosphere above the molten salt furnace 10. In the descending process of the materials, the partial pressure of gas in the whole system is kept at 1.00-1.50 atmospheric pressure by adding ammonium chloride into the feed supplement port 14 at regular time. A discharge hole 15 is arranged on the side wall of the molten salt furnace 10 and below the liquid level of the liquid molten salt, and a slag hole 16 is arranged at the bottom of the molten salt furnace 10.
The molten salt heating/reaction unit is used for providing liquid molten salt for protecting materials from melting or alloying, realizing protective melting of easily oxidized burning loss metal or alloy in the liquid molten salt, alloying (alloying for alloy blending or molten salt in situ alloying) and preparation of high-purity easily hydrolyzed molten salt, and simultaneously providing protection for the atmosphere around the materials in the process of heating the materials; the preheating and impurity removing unit is used for preheating and removing impurities of the materials entering the molten salt heating/reaction unit by controlling the heating temperature and the descending speed of the materials; the feeding protection unit is used for quantitatively pushing the materials in the preheating impurity removal unit into the liquid molten salt in the molten salt heating/reaction unit.
The functions and the implementation process of each part of the multifunctional molten salt furnace are as follows:
(a1) preheating and impurity removing units: after materials (molten salt, metal or alloy) are added into the material conveying pipe 2 through the feeding port 5, the materials are stacked in a certain shape in the material conveying pipe 2; the preheating temperature of the materials is controlled by the upper heating assembly 1, and the effective control of the internal atmosphere (including ammonium chloride gas, ammonia gas and hydrogen chloride released by decomposition of ammonium chloride and fused salt steam) of the materials is realized by the accumulation mode of the materials in the material conveying pipe 2 and the opening and closing degrees of the exhaust connecting piece 3 and the exhaust pipeline 3; part of impurities in the material can selectively react with ambient gas under certain conditions to generate volatile substances to escape, so that preheating and impurity removal of the material are realized.
(a2) A feeding protection unit: the preheated and impurity-removed materials are gradually melted in the liquid molten salt by the propulsion of a stirring rod 6 and a spiral feeder 7. Wherein, fused salt support piece 8, overflow hole 9 are arranged in liquid fused salt below, can guarantee to insulate against air effectively at the in-process that the material melts, reduce high temperature oxidation or hydrolyze.
The feeding protection unit can realize the following functions through the synergistic action of the components: firstly, preventing materials from caking: solid materials are easy to sinter at high temperature, so that smooth blanking cannot be realized. The sintered structure formed by the materials can be continuously destroyed by spiral stirring, and the materials can be ensured to move smoothly; secondly, quantitative feeding: by controlling the rotating speed of the stirrer and further controlling the propelling speed of the spiral feeder 7, the solid materials entering the liquid molten salt can be quantitatively controlled, and the problem that the feeding speed is not matched with the material melting speed can be effectively solved; protecting atmosphere: the shape and size of the spiral feeder 7 and the speed of pushing the materials are controlled, so that the control of the surrounding atmosphere before the materials are melted can be realized; protecting the material melting process: the material melting process is carried out at the lower part of the liquid molten salt, so that the contact between the material and the oxygen-containing gas in the air is effectively isolated, and the probability of oxidation and hydrolysis is greatly reduced; in addition, the spiral feeder 7 can also press metal or alloy with lower density into the lower part of the molten salt, so that serious oxidation caused by floating in the heating process is avoided; homogenizing alloy: the spiral feeder 7 can stir the alloy liquid in the alloying process to realize the uniform distribution of the components of the alloy liquid.
(a3) Molten salt heating/reaction unit: heating the molten salt into a liquid state by adopting a lower heating assembly 11, and adding a molten salt solid material from a material supplementing opening 14 along with the heating to supplement the loss of volatilization of the high-temperature molten salt or adding ammonium chloride at regular time to ensure the protective atmosphere above the molten salt furnace; the thermocouple 12 and the liquid level measurer 13 are used for continuously testing and displaying the internal temperature of the molten salt furnace and the molten salt liquid level so as to facilitate continuous production; the product is discharged through a discharge port 15, and the slag precipitated at the bottom of the molten salt is discharged through a slag outlet 16.
The molten salt heating/reaction unit may perform the following functions: uniformly heating: the fused salt can be directly contacted with the materials, the heat transfer efficiency is high, and the heating is uniform; melting the easily oxidized metal or alloy: the liquid molten salt can well isolate the contact of materials and air, and avoid serious oxidation and burning loss in the high-temperature heating process; the easily oxidized metal or alloy is placed in the molten salt for heating and melting, so that the high-temperature oxidation burning loss is greatly reduced; and thirdly, the alloying process can be realized: various metals are placed at the lower part of the molten salt and are uniformly mixed, so that the oxidation burning loss in the alloying process by a doping method can be greatly reduced; in addition, the metal can be used for reacting with part of components in the molten salt, so that in-situ alloying in the molten salt environment is realized; preparing high-purity easily-hydrolyzed molten salt: by controlling the atmosphere of the heating/reaction zone, the hydrolysis of the high-temperature easily-hydrolyzed molten salt can be effectively controlled, the hydrolysis product is ensured to have enough time to precipitate, and the purity of the molten salt is further improved.
The multifunctional molten salt furnace of the invention is operated as a whole as follows:
(b1) bottom molten salt preparation:
heating and melting the added solid molten salt by using a lower heating assembly 11, and continuously monitoring the molten salt state by using a thermocouple 12 and a liquid level measurer 13; ammonium chloride is added at regular time through the feeding port 14, and the position of the spiral feeder 7 is adjusted to adjust the atmosphere composition above the liquid molten salt and the partial pressure of each component, so as to ensure that the molten salt at the bottom is not hydrolyzed at high temperature.
(b2) Metal or alloy melting process/alloying process for blend:
the metal or alloy is added from the feeding port 5 at the upper part, when the metal or alloy is stacked in the material conveying pipe 2, the preheating and impurity removal (including the adsorption of gas and metal impurities on the surface or inside of the alloy) of the metal or alloy are realized by controlling the amount of ammonium chloride added from the feeding port 2, the advancing speed of the spiral feeder 7, the material stacking state and the heating temperature. The atmosphere (including ammonia gas, hydrogen chloride and ammonium chloride) around the materials is used for protecting the materials in the heating process, and the hydrolysis in the heating process is reduced.
In the material descending process, the solid metal or alloy is pressed into the molten salt by using the spiral feeder 7, so that the whole melting process is carried out in the molten salt, and the serious oxidation burning loss caused by the floating of the material is avoided. In the alloying process, the spiral feeder 7 can stir the alloy liquid to ensure the components of the alloy liquid to be uniform. The product and the sediment are discharged from the discharge hole 15 and the sediment discharge hole 16 respectively, thereby realizing continuous operation.
(b3) In-situ alloying process:
adding metal or alloy and reactant fused salt from a feeding port 5 at the upper part, when materials are stacked in the material conveying pipe 2, preheating and impurity removal of the materials are realized by controlling the amount of ammonium chloride added from a material supplementing port 14, the propelling speed of a spiral feeder 7, the material stacking state and the heating temperature, and the protection of the material heating process is realized by utilizing the atmosphere (comprising ammonia gas, hydrogen chloride and ammonium chloride) around the materials.
In the material descending process, the solid metal or alloy is pressed into the molten salt by using the spiral feeder 7, so that the whole melting process is carried out in the molten salt, and the serious oxidation burning loss caused by the floating of the material is avoided. The molten metal or alloy and molten reactant fused salt are subjected to in-situ reaction, and the alloy liquid is stirred by a spiral feeder 7 to prepare the required alloy liquid. The product and the sediment are discharged from the discharge hole 15 and the sediment discharge hole 16 respectively, thereby realizing continuous operation.
(b4) The preparation process of the high-purity molten salt comprises the following steps:
the fused salt is added from the feeding port 5 at the upper part, when the materials are stacked in the material conveying pipe 2, the preheating, the impurity removal and the hydrolysis product conversion of the materials are realized by controlling the amount of ammonium chloride added from the feeding port 14, the propelling speed of the spiral feeder 7, the material stacking state and the heating temperature, and the protection of the material heating process is realized by utilizing the atmosphere (comprising ammonia gas, hydrogen chloride and ammonium chloride) around the materials.
In the material descending process, the matching of the molten salt feeding speed and the melting speed is realized by regulating and controlling the propelling speed of the spiral feeder 7, so that the easily hydrolyzed molten salt is protected by liquid molten salt as soon as possible. The product and the sediment are discharged from the discharge hole 15 and the sediment discharge hole 16 respectively, thereby realizing continuous operation.
Although the present invention is illustrated by the above examples to show the detailed process parameters and process flows of the present invention, the present invention is not limited to the above detailed process parameters and process flows, i.e., it is not meant that the present invention is necessarily dependent on the above detailed process parameters and process flows to be practiced. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (9)
1. A multifunctional molten salt system, characterized in that: comprises a preheating impurity removal unit, a feeding protection unit and a molten salt heating/reaction unit;
the molten salt heating/reaction unit comprises a molten salt furnace (10) and a lower heating assembly (11) arranged in the molten salt furnace (10); the inner cavity of the molten salt furnace (10) is divided into a liquid molten salt area at the lower part and a protective atmosphere area at the upper part, and the lower part heating assembly (11) is positioned at the bottom of the liquid molten salt area; the lower heating assembly (11) is used for heating the solid molten salt into liquid molten salt and heating materials added into the liquid molten salt;
the preheating and impurity removing unit comprises a material conveying pipe (2) vertically inserted into the molten salt furnace (10), a stirring rod (6) arranged in the material conveying pipe (2), an upper heating assembly (1) arranged outside the outer end of the material conveying pipe (2) and a feeding port (5) arranged at the top of the material conveying pipe (2), and the bottom end of the material conveying pipe (2) is positioned in a liquid molten salt area;
the feeding protection unit comprises a molten salt support member (8) arranged in the liquid molten salt area and positioned below the material conveying pipe (2), and a spiral feeder (7) arranged at the lower end of the stirring rod (6); the lower pipe opening of the material conveying pipe (2) is connected with the feeding hole of the molten salt support piece (8), and the bottom of the spiral feeder (7) is spaced from the surface of the liquid molten salt;
the spiral feeder (7) is used for preventing most materials from directly falling into the liquid molten salt and controlling the downward speed of the materials by controlling the propelling speed of the spiral feeder; the material of high temperature fused salt in through upper portion heating element (1) and the liquid fused salt district heats in material conveying pipe (2) jointly, when the lower material of temperature and high temperature fused salt contact, through the addition of control fused salt temperature and low temperature material for the fused salt surface is because exothermic solidification crusts, thereby supports the solid material on upper portion, makes the material pile up in material conveying pipe (2), realizes preheating of material and the desorption of partial impurity.
2. The multifunctional molten salt system of claim 1 wherein: the ratio of the height to the diameter of the material conveying pipe (2) is 0.5-35.0.
3. The multifunctional molten salt system of claim 1 wherein: the upper end of the material conveying pipe (2) is provided with a transverse exhaust pipeline (4) through an exhaust connecting piece (3).
4. The multifunctional molten salt system of claim 1 wherein: the difference between the inner diameter of the material conveying pipe (2) and the diameter of the blade of the spiral feeder (7) is 0.5-5.0 mm.
5. The multifunctional molten salt system of claim 1 wherein: the top of the molten salt furnace (10) is provided with a thermocouple (12) and a liquid level measurer (13) which are used for respectively measuring the internal temperature and the molten salt liquid level of the molten salt furnace.
6. The multifunctional molten salt system of claim 1 wherein: and a feeding port (14) for adding and supplementing solid molten salt into the molten salt furnace (10) and adding ammonium chloride at regular time to ensure protective atmosphere above the molten salt furnace (10) is arranged at the top of the molten salt furnace (10).
7. The multifunctional molten salt system of claim 1 wherein: a discharge hole (15) is formed in the side wall of the molten salt furnace (10) and is located below the liquid level of the liquid molten salt, and a slag outlet (16) is formed in the bottom of the molten salt furnace (10).
8. The multifunctional molten salt system of claim 1 wherein: and an overflow hole (9) is formed in the middle of the side surface of the molten salt support member (8).
9. The multifunctional molten salt system of claim 1 wherein: the material of the stirring rod (6) and the spiral feeder (7) is any one or any two of corundum, silicon carbide, Inconel 625 and ceramic.
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