Method for Preparing High-purity Metal Lithium by Vacuum Thermal Reduction Method

Abstract

A method for preparing a high-purity metal lithium by a vacuum thermal reduction method includes the following steps: obtaining Li.sub.2O.(2-x)CaO by carrying a vacuum thermal decomposition process on a lithium-containing raw material in the presence of a refractory agent and a catalyst; mixing the obtained oxide with the fluxing agent, the catalyst and a reducing agent according to a certain ratio, and then briquetting; carrying out vacuum thermal reduction in a vacuum reduction furnace, and performing centrifugal sedimentation and micron ceramic dust removal on lithium vapor obtained by the thermal reduction to obtain a high-purity metal gas; and removing metal impurities from the gas by controlling a condensation temperature and a condensation speed of the gas so as to purify the lithium vapor, and obtaining a high-purity metal lithium with a rapid cooling technology.

Claims

1. A method for preparing a high-purity metal lithium by a vacuum thermal reduction method, comprising the following steps: 1) The lithium-containing raw material, the refractory agent and the catalyst are mixed and then briqueted in proportion under pressure; thermally decomposing the briquetted mixture in an industrial tube furnace; and generating the unsaturated composite oxide by lithium oxide and the refractory agent, and recycling the sublimated and condensed catalyst; 2) respectively crushing and ball-milling the unsaturated composite oxide generated in step 1), the reducing agent and a fluxing agent, and then briquetting; 3) charging briquettes in step 2) into a vacuum reaction furnace for vacuum reduction, at this time, a reduction product is in the gaseous state and carries solid materials; 4) making the gas carrying the solid materials in step 3) pass through a centrifugal filter in a dust chamber of the temperature control device, and then entering the first condensing chamber, and controlling the temperatures of a centrifugal separator and the first condensing chamber to be 700-800° C. with the gas at an airflow velocity of 1.2-1.8 m/sec; removing the vast majority of solid particles; and then making the gas pass through the micron ceramic filter to purify more than 99.95% of solid particles with the dust, and controlling an outlet temperature to be 650-700° C.; 5) After purification the pure metal gas passes through the second condensing chamber of the quenching device, using a cooling liquid at below −100° C. to thermally exchange with a metal gas on an outer layer of a condenser in the second condensing chamber, and sharply cooling the gas to 50-80° C., in order to condense the metal gas as a metal lithium in a condensed state; and 6) obtaining the high-purity lithium by flux smelting, refining, purifying by distillation of the metal lithium in the condensed state in a pit furnace under the protection of Ar.

2. The method according to claim 1, wherein the lithium-containing raw material is carbonate, nitrate, sulfate, silicate or lithium-containing sulphide, the refractory agent is CaO, Al.sub.2O.sub.3 or a mixture of CaO and Al.sub.2O.sub.3, the Al.sub.2O.sub.3 is industrial aluminium oxide and the catalyst is Sb.sub.2O.sub.3 or Bi.sub.2O.sub.3; and a molar ratio of the lithium-containing raw material to the refractory agent to the catalyst is 32-40:58-67:1-3.

3. The method according to claim 1, wherein the lithium-containing raw material, the refractory agent and the catalyst in step 1) are necessarily ground to be 40-100 μm in a ball mill before being mixed; and each briquette is required to be of an almond shape, at a weight of 25-35 g/Nr., the pressure briquetting condition is 35-45 Mpa, a thermal decomposition temperature is 600-1,300° C., and a carbon content in the material is 40 PPM or below.

4. The method according to claim 1, wherein the unsaturated composite oxide, the reducing agent and the fluxing agent in step 2) are briquetted after being respectively crushed and ball-milled, and the granularity is 40-100 μm after its ball-milling; the briquetting conditions include: briquetting into an almond shape at a weight of 25-35 g/Nr. at 30-45 Mpa.

5. The method according to claim 1, wherein the reducing agent is high silicon iron, aluminium powder having an Al content being more than or equal to 99 wt %, aluminium powder having an activity being more than 70 wt % and the granularity being less than 8 the aluminum silicon powder having an Al—Si content being more than or equal to 98% or carbon powder; the fluxing agent is CaF.sub.2 having a purity being 97.5%; a mass ratio of the unsaturated composite oxide to the reducing agent to the fluxing agent is 79-85:12-20:1-3.

6. The method according to claim 1, wherein a vacuum degree in a vacuum reaction furnace for the thermally decomposed high-temperature steel is 10-20 pa, and a temperature is 600-1300° C.

7. The method according to claim 1, wherein for an industrial heat-resistant tube furnace for thermal reduction, the vacuum degree is 1-15 pa, a temperature is 800-1,300° C., and thermal reduction time is 6-12 h.

8. The method according to claim 1, wherein the quenching temperature control device comprises a reaction zone (1), a dust chamber (2), the first condensing chamber (3), the second condensing chamber (4), a discharge hole (5) of the dust chamber and a vacuum tube (6), and the reaction area (1) thereof is in communication with the dust chamber (2); the centrifugal separator is arranged in the dust chamber (2), a lower end of which is provided with a funnel; a lower end of one side of the funnel is provided with a first heating zone inlet (7), and the slag discharge hole (5) of the dust chamber is defined at the bottom of the funnel; an upper end of one side of the dust chamber (2) is provided with a first heating zone outlet (8), the top of the dust chamber (2) is provided with the first condensing chamber (3), a second heating zone outlet (10) is arranged at an upper end of a connection between the first condensing chamber (3) and the dust chamber (2) and a ceramic micron filter (15) is arranged in the first condensing chamber (3); the first condensing chamber (3) is in communication with the second condensing chamber (4); a second heating zone inlet (9) is defined in a connection with the second condensing chamber (4) in the first condensing chamber (3); the vacuum tube (6) is arranged on a connection with the first condensing chamber (3) within the second condensing chamber (4), and a cooling liquid inlet (12) and a cooling air inlet (13) as well as a cooling liquid outlet (11) and a cooling air outlet (14) are respectively defined at both sides of the second condensing chamber (4).

9. The method according to claim 8, wherein the first condensing chamber (3) and the second condensing chamber (4) are double-casing coolers; in the second condensing chamber (4), a gas velocity in the center of the cooler is 1.5-4 m/sec, the ratio of the cooling area to the metal of the condensate phase is 0.4-0.7 dm.sup.3/kg.

10. The method according to claim 1, wherein a high-purity metal lithium after being refined and purified by distillation is subject to ingot casting to obtain the lithium having a purity being 99.0-99.99 wt %.

Description

[0036] In which, 1—reaction zone, 2—dust chamber, 3—first condensing chamber, 4—second condensing chamber, 5—slag discharge hole of dust chamber, 6—vacuum tube, 7—first heating zone inlet, 8—first heating zone outlet, 9—second heating zone inlet, 10—second heating zone outlet, 11—cooling liquid outlet, 12—cooling liquid inlet, 13—cooling air inlet, 14—cooling air outlet, and 15—ceramic micron filter.

DESCRIPTION OF EMBODIMENTS

[0037] The present invention will be further described in detail in combination with specific implementations for the purpose of clear understanding of the objectives, technical solutions and advantages of the present invention, but it shall not be understood that the scope of the above subject of the present invention is only limited to the following embodiments.

[0038] The quenching device applied in the following embodiments comprises a reaction zone, a dust chamber, a first condensing chamber, a second condensing chamber, a slag discharge hole of the dust chamber and a vacuum tube, and the reaction zone thereof is in communication with the duct chamber; a centrifugal separator is arranged in the dust chamber, a lower end of which is provided with a funnel; a lower end of one side of the funnel is provided with a first heating zone inlet, and the slag discharge hole of the dust chamber is defined at the bottom of the funnel; an upper end of one side of the dust chamber is provided with the first heating zone outlet, the top of the dust chamber is provided with the first condensing chamber, a second heating zone outlet is defined at an upper end of a connection between the first condensing chamber and the dust chamber and a ceramic micron filter is arranged in the first condensing chamber; the first condensing chamber is in communication with the second condensing chamber; a second heating zone inlet is defined on a connection with the second condensing chamber in the first condensing chamber; and the vacuum tube is arranged on a connection with the first condensing chamber in the second condensing chamber, and a cooling liquid inlet and a cooling air inlet as well as a cooling liquid outlet and a cooling air outlet are respectively defined at both sides of the second condensing chamber.

[0039] The first condensing chamber and the second condensing chamber are double-casing coolers; in the second condensing chamber, a gas velocity in the center of the cooler is 1.5-4 m/sec, and the ratio of the cooling area to the metal of the condensate phase is 0.4-0.7 dm.sup.3/kg. % recited in the following embodiments shows wt % thereof, unless particularly stated.

Embodiment 1

[0040] 1) Raw materials are weighed in proportion, wherein a granularity of lithium carbonate is 89 μm, and a granularity of calcium oxide is 74 μm; the lithium carbonate, a refractory agent CaO and a catalyst Sb.sub.2O.sub.3 are mixed in a molar ratio of 1:1.6:0.4, and briquetted under the pressure of 35 Mpa; each briquette is 28 g, and is of an almond shape. The prepared briquettes are charged into a φ330 mm*3,300 mm industrial tube furnace with a vapor-deposited nitrocarbon compound crucible for thermal decomposition, the sublimated and condensed catalyst may be recycled, and an unsaturated composite oxide is generated by lithium oxide and a refractory agent. A vacuum degree of the industrial tube furnace is 10 pa, and a temperature is 860° C. High temperature decomposition time is 5 h, a decomposition rate of the lithium carbonate decomposed into lithium oxide is 99.2%, and a lithium yield reaches 99.5%.

[0041] 2) The unsaturated composite oxide formed by the lithium oxide obtained in step 1) and the refractory agent, a silicon iron and CaF.sub.2 are respectively crushed and ball-milled till a granularity is 60 μm, mixed according to a mass ratio of 81:17:2, and pressed into briquettes at a weight of 28 g/Nr. under 30 Mpa.

[0042] 3) The briquettes in step 2) are charged into a φ330 mm*3,300 mm industrial heat-resistant tube furnace for vacuum reduction, wherein a vacuum degree is 3 pa and a temperature is 1,200° C. in the furnace; and at this time, a reduction product is in a gaseous state and carries solid materials; and a lithium reduction is 99%.

[0043] 4) The gas carrying the solid materials passes through a centrifugal separator in the dust chamber in a temperature control device, and then through the first condensing chamber, wherein the first condensing chamber has a sandwich; and the temperatures of the centrifugal separator and the first condensing chamber are controlled to be 750° C. with the gas at an airflow velocity of 1.5 m/sec; the gas carrying 98% of more than 20 μm solid particles is removed while passing through the first condensing chamber, more than 99.95% of carried dust is purified when the gas passes through 0.5 μm micron ceramic filter, and an outlet temperature is controlled to be 680° C.

[0044] 5) The purified pure metal gas passes through the second condensing chamber of the quenching device; when a temperature of an inner layer of a double-casing cooler of the second condensing chamber is controlled to be 60° C., a low temperature cooling liquid below −110° C. is thermally exchanged with a metal gas on an outer layer; heat is transferred to an inner wall from a center of the cooler by a gas at 3 m/sec, and the cooling area is 0.65 dm.sup.3/kg, so that the metal gas may be rapidly condensed as the condensed phase of the alloy.

[0045] 6) A lithium metal raw ingot having a purity being 99% is obtained by flux smelting and refining of the metal lithium in a condensed phase in a pit furnace under the protection of Ar.

[0046] 7) The lithium metal raw ingot is separated by distillation; a lower temperature of a distiller is controlled to be 550° C., a middle temperature controlled to be 450° C., and an upper temperature controlled to be 70° C.; impurities with a high melting point are removed from a lower part, including Fe, Ni, Co, Si and Ca; and metal impurities with a low melting point are removed from an upper part, including k and Na, and an Li metal cast ingot is discharged from a middle part.

[0047] A chemical component test (ICP test) is carried out for commodities obtained by ingot casting after distillation, and the chemical component test results (wt %) of the lithium ingot are seen in the table below.

TABLE-US-00001 Li K Na Ca Fe Si Al 99.991 0.0004 0.0009 0.0005 0.0005 0.0005 0.0005 Ni Cu Mg Cl− N Pb 0.0004 0.0005 0.0005 0.0008 0.003 0.0005

[0048] As can be seen from Embodiment 1, the pure lithium having a purity of 99.99% prepared by the present invention by virtue of the method is applicable to more pure lithium demand fields.

Embodiment 2

[0049] 1) Raw materials are weighed in proportion, wherein the granularity of lithium carbonate is 80 μm, and the granularity of calcium oxide is 65 μm; the lithium carbonate, a refractory agent CaO and a catalyst Sb.sub.2O.sub.3 are mixed in a molar ratio of 1:1.6:0.4, and briquetted under the pressure of 40 Mpa; each briquette is 28 g, and is of an almond shape. The prepared briquettes are charged into a φ330 mm*3,300 mm industrial tube furnace with a vapor-deposited nitrocarbon compound crucible for thermal decomposition, the sublimated and condensed catalyst may be recycled, and an unsaturated composite oxide is generated by lithium oxide and a refractory agent. A vacuum degree of the industrial tube furnace is 10 pa, and a temperature is 880° C. High temperature decomposition time is 5 h, a decomposition rate of the lithium carbonate decomposed into lithium oxide is 99.3%, and a lithium yield reaches 99.4%.

[0050] 2) The unsaturated composite oxide formed by the lithium oxide obtained in step 1) and the refractory agent, a silicon iron and CaF.sub.2 are respectively crushed and ball-milled till a granularity is 60 μm, mixed according to the mass ratio of 83:15:2, and pressed into briquettes at a weight of 28 g/Nr. under 35 Mpa.

[0051] 3) The briquettes in step 2) are charged into a φ330 mm*3,300 mm industrial heat-resistant tube furnace, and the vacuum degree is controlled to be 3 pa and a temperature to be 1,200° C. in the furnace; and at this time, a reduction product is in a gaseous state and carries solid materials, and a lithium reduction is 99.1%.

[0052] 4) The gas carrying the solid materials passes through a centrifugal separator in the dust chamber in a temperature control device, and then through the first condensing chamber, wherein the first condensing chamber has a sandwich; and the temperatures of the centrifugal separator and the first condensing chamber are controlled to be 780° C. with the gas at an airflow velocity of 1.5 m/sec; and the gas carrying 98% of more than 20 μm solid particles is removed while passing through the first condensing chamber, more than 99.95% of carried dust is purified when the gas passes through 0.5 μm micron ceramic filter, and an outlet temperature is controlled to be 690° C.

[0053] 5) The purified pure metal gas passes through the second condensing chamber of the quenching device; when a temperature of an inner layer of a double-casing cooler of the second condensing chamber is controlled to be 70° C., a low temperature cooling liquid below −110° C. is thermally exchanged with a metal gas on an outer layer; heat is transferred to an inner wall from a center of the cooler by a gas at 2.9 m/sec, and the cooling area is 0.60 dm.sup.3/kg, so that the metal gas may be rapidly condensed as the condensed phase of the alloy..

[0054] 6) A lithium metal raw ingot having a purity being 99% is obtained by flux smelting and refining of the metal lithium in a condensed phase in a pit furnace under the protection of Ar.

[0055] 7) The lithium metal raw ingot is separated by distillation; a lower temperature of a distiller is controlled to be 580° C., a middle temperature controlled to be 480° C., and an upper temperature controlled to be 80° C.; impurities with a high melting point are removed from a lower part, including Fe, Ni, Co, Si and Ca; metal impurities with a low melting point are removed from an upper part, including k, Na, and an Li metal cast ingot is discharged from a middle part.

[0056] A chemical component test (ICP test) is carried out for commodities obtained by ingot casting after distillation, and the chemical component test results of the obtained lithium ingot are seen in the table below.

TABLE-US-00002 Li K Na Ca Fe Si Al 99.991 0.0005 0.0008 0.0005 0.0005 0.0004 0.0004 Ni Cu Mg Cl− N Pb 0.0004 0.0005 0.0005 0.0009 0.0031 0.0005

Embodiment 3

[0057] 1) Raw materials are weighed in proportion, wherein the granularity of lithium carbonate is 76 μm, and the granularity of calcium oxide is 66 μm; the lithium carbonate, CaO and a catalyst Sb.sub.2O.sub.3 are mixed in a molar ratio of 1:1.6:0.4, and briquetted under the pressure of 40 Mpa; each briquette is 28 g, and is of an almond shape. The prepared briquettes are charged into a φ330 mm*3,300 mm industrial tube furnace with the vapor-deposited nitrocarbon compound crucible for thermal decomposition, the sublimated and condensed catalyst is recycled, and an unsaturated composite oxide is generated by lithium oxide and a refractory agent. A vacuum degree of the industrial tube furnace is 10 pa, and a temperature is 880° C. High temperature decomposition time is 5 h, a decomposition rate of the lithium carbonate decomposed into lithium oxide is 99.3%, and a lithium yield reaches 99.3%.

[0058] 2) The unsaturated composite oxide formed by the lithium oxide obtained in step 1) and the refractory agent, a silicon iron and CaF.sub.2 are respectively crushed and ball-milled till a granularity is mixed according to a mass ratio of 82:16:2, and pressed into briquettes at a weight of 32 g/Nr. under 42 Mpa.

[0059] 3) The briquettes in step 2) are charged into a φ330 mm*3,300 mm industrial heat-resistant tube furnace for vacuum reduction; a vacuum degree is controlled to be 3 pa, and temperature to be 1,200° C. in the furnace, at the time, a reduction product is in a gaseous state and carries solid materials, and a lithium reduction is 99.1%.

[0060] 4) The gas carrying the solid materials passes through a centrifugal filter in the dust chamber in a temperature control device, and then through a first condensing chamber, wherein the first condensing chamber has a sandwich; and the temperatures of the centrifugal separator and the first condensing chamber are controlled to be 760° C. with the gas at an airflow velocity of 1.5 m/sec. the gas carrying 98% of more than 20 μm solid particles is removed while passing through the first condensing chamber, more than 99.95% of carried dust is purified when the gas passes through 0.5 μm micron ceramic filter, and an outlet temperature is controlled to be 680° C.

[0061] 5) The purified pure metal gas passes through the second condensing chamber of the quenching device; when the temperature of an inner layer of a double-casing cooler of the second condensing chamber is controlled to be 65° C., a low temperature cooling liquid below −105° C. is thermally exchanged with a metal gas on an outer layer; heat is transferred to an inner wall from a center of the cooler by a gas at 2.9 m/sec, and a cooling area is 0.60 dm.sup.3/kg, so that the metal gas may be rapidly condensed as the condensed phase of the alloy..

[0062] 6) A lithium metal raw ingot having a purity being 99% is obtained by flux smelting and refining of the metal lithium in the condensed phase in a pit furnace under the protection of Ar.

[0063] 7) The lithium metal raw ingot is separated by distillation; a lower temperature of a distiller is controlled to be 560° C., a middle temperature controlled to be 460° C., and an upper temperature controlled to be 70° C.; impurities with a high melting point are removed from a lower part, including Fe, Ni, Co, Si and Ca; metal impurities with a low melting point are removed from an upper part, including k, Na, and an Li metal cast ingot is discharged from a middle part.

[0064] A chemical component test (ICP test) is carried out for commodities obtained by ingot casting after distillation, and the chemical component test results of the lithium ingot are seen in the table below.

TABLE-US-00003 Li K Na Ca Fe Si Al 99.955 0.0005 0.009 0.008 0.002 0.004 0.0005 Ni Cu Mg Cl− N Pb 0.0009 0.0005 0.0049 0.0048 0.009 0.0009

Embodiment 4

[0065] With the granularity of lithium carbonate as 89 μm and the granularity of calcium oxide as 74 μm, the lithium carbonate, CaO and antimonous oxide are mixed in a molar ratio of 1:1.6:0.4, and then briquetted; and a briquetting pressure is 35 MPa, and each briquette is 28 g and is of an elliptical shape. The briquetted substance is charged into a φ330 mm*3,300 mm industrial tube furnace with the vapor-deposited nitrocarbon compound crucible for thermal decomposition, wherein a thermal decomposition temperature is 860° C., a vacuum degree is 10 Pa, high temperature decomposition time is 5 h, and a thermal decomposition rate is 99.2%. The remaining preparation steps are the same as those in Embodiment 1; upon the test, the lithium purity is 99.99% in a commodity obtained by ingot casting after refining.

Embodiment 5

[0066] With the granularity of material lithium carbonate as 74 μm and the granularity of calcium oxide as 61 μm, lithium oxide, calcium oxide and bismuth oxide are mixed in a molar ratio of 1:1.8:0.2, elliptical briquettes are prepared under a briquetting pressure of 45 MPa (each briquette is 35 g). The briquetted substance is charged into a φ330 mm*3,300 mm industrial tube furnace with a vapor-deposited nitrocarbon compound crucible for thermal decomposition, wherein the thermal decomposition temperature is 880° C., the vacuum degree is 10 Pa, high temperature decomposition time is 5 h, and a thermal decomposition rate is 99.5%. The remaining preparation steps are the same as those in Embodiment 1; upon the test, the lithium purity is 99.991% in a commodity obtained by ingot casting after refining.

COMPARATIVE EXAMPLE 1

[0067] 1) An industrial grade lithium nitrate is roasted at a temperature of 680° C. for 7 h to form stable Li.sub.2O.2CaO without briquetting, wherein the decomposition rate of lithium nitrate decomposed into lithium oxide is 98.1%, and a lithium yield reaches 90.1%.

[0068] 2) A unsaturated composite oxide formed by the lithium oxide obtained in step 1) and the refractory agent, a silicon iron and CaF.sub.2 are respectively crushed and ball-milled till a granularity is 60 μm, mixed according to the mass ratio of 80:18:2, and pressed into briquettes at the weight of 28 g/Nr. under 35 Mpa.

[0069] 3) The briquettes in step 2) are charged into a φ330 mm*3,300 mm industrial heat-resistant tube furnace with a vacuum degree of 3 pa and a temperature of 1,200° C. for vacuum reduction; at this time, a reduction product is in a gaseous state and carries solid materials, and a lithium reduction is 98.8%.

[0070] 4) The gas carrying the solid materials passes through a centrifugal filter in a dust chamber in a temperature control device, and then through a first condensing chamber, wherein the first condensing chamber has a sandwich; and the temperatures of the centrifugal separator and the first condensing chamber are controlled to be 720° C. with the gas at an airflow velocity of 1.5 m/sec. The gas carrying 98% of more than 20 μm solid particles is removed while passing through the first condensing chamber, more than 99.95% of carried dust is purified when the gas passes through 0.5 μm micron ceramic filter, and an outlet temperature is controlled to be 660° C.

[0071] 5) The purified pure metal gas passes through the second condensing chamber of the quenching device; when the temperature of an inner layer of a double-casing cooler of the second condensing chamber is controlled to be 550° C., a low temperature cooling liquid below −105° C. is thermally exchanged with the metal gas on an outer layer; heat is transferred to an inner wall from a center of the cooler by a gas at 3 m/sec, and the cooling area is 0.68 dm.sup.3/kg, so that the metal gas may be rapidly condensed as the condensed phase of the alloy.

[0072] 6) A lithium metal raw ingot having a purity being 99% is obtained by flux smelting and refining of the metal lithium in a condensed phase in a pit furnace under the protection of Ar and mixing.

[0073] 7) The lithium metal raw ingot is separated by distillation; a lower temperature of a distiller is controlled to be 530° C., a middle temperature controlled to be 430° C., and an upper temperature controlled to be 60° C.; impurities with a high melting point are removed from a lower part, including Fe, Ni, Co, Si and Ca; metal impurities with a low melting point are removed from an upper part, including k, Na, and an Li metal cast ingot is discharged from a middle part.

[0074] A chemical component test (ICP test) is carried out for commodities obtained by ingot casting after distillation, and the chemical component test results of the lithium ingot are seen in the table below.

TABLE-US-00004 Li K Na Ca Fe Si Al 99.991 0.0004 0.0009 0.0005 0.0005 0.0005 0.0004 Ni Cu Mg Cl− N Pb 0.0004 0.0005 0.0005 0.0007 0.0032 0.0005

[0075] Due to longer thermal decomposition time of lithium nitrate than lithium carbonate, oxynitride gases are produced during the decomposition, but are processed difficultly in an environmental protection process, so that the entire process is complicate. Direct thermal decomposition leads to low lithium yield and high energy consumption ratio. Compared with lithium carbonate, the metal lithium has a low capacity, a complicated process and a low yield, which leads to increasing production cost.

COMPARATIVE EXAMPLE 2

[0076] 1) An industrial grade lithium sulfate is roasted at the temperature of 920° C. for 8 h to form stable Li.sub.2O.1.75 CaO without briquetting, wherein the decomposition rate of lithium sulfate decomposed into lithium oxide is 94.8%, and a yield of lithium reaches 95.6%.

[0077] 2) The unsaturated composite oxide formed by the lithium oxide obtained in step 1) and the refractory agent, a silicon iron and CaF.sub.2 are respectively crushed and ball-milled till a granularity is 60 μm, mixed according to the mass ratio of 82:16:2, and pressed into briquettes at a weight of 30 g/Nr. under 40 Mpa.

[0078] 3) The briquettes in step 2) are charged into a φ330 mm*3,300 mm industrial heat-resistant tube furnace, with the vacuum degree of 3 pa and the temperature of 1,200° C. in the furnace; and at this time, a reduction product is in the gaseous state and carries solid materials, and a lithium reduction is 98.9%.

[0079] 4) The gas carrying the solid materials passes through a centrifugal filter in a dust chamber and the first condensing chamber, wherein the first condensing chamber has a sandwich; and the temperatures of a centrifugal separator and the first condensing chamber are controlled to be 740° C. with the gas at an airflow velocity of 1.5 m/sec; the gas carrying 98% of more than 20 μm solid particles is removed while passing through the first condensing chamber, more than 99.95% of carried dust is purified when the gas passes through 0.5 μm micron ceramic filter, and an outlet temperature is controlled to be 670° C.

[0080] 5) The pure metal gas passes through the second condensing chamber of the quenching device; when a temperature of an inner layer of a double-casing cooler of the second condensing chamber is controlled to be 65° C., a low temperature cooling liquid below −105° C. is thermally exchanged with the metal gas on an outer layer; heat is transferred to an inner wall from a center of the cooler by a gas at 3 m/sec, and the cooling area is 0.63 dm.sup.3/kg, so that the metal gas may be rapidly condensed as the condensed phase of the alloy.

[0081] 6) A lithium metal raw ingot having a purity being 99% is obtained by flux smelting and refining of the metal lithium in a condensed phase in a pit furnace under the protection of Ar.

[0082] 7) The lithium metal raw ingot is separated by distillation; a lower temperature of a distiller is controlled to be 560° C., a middle temperature controlled to be 440° C., and an upper temperature controlled to be 75° C.; impurities with a high melting point are removed from a lower part, including Fe, Ni, Co, Si and Ca; metal impurities with a low melting point are removed from an upper part, including k, Na, and an Li metal cast ingot is discharged from a middle part.

[0083] A chemical component test (ICP test) is carried out for commodities obtained by ingot casting after distillation, and the chemical component test results of the lithium ingot are seen in the table below.

TABLE-US-00005 Li K Na Ca Fe Si Al 99.991 0.0004 0.0009 0.0005 0.0005 0.0005 0.0005 Ni Cu Mg Cl− N Pb 0.0005 0.0005 0.0005 0.0009 0.0028 0.0005

[0084] Due to the fact that the lithium sulfate is decomposed more difficultly in comparison with lithium carbonate and cannot be completely decomposed, direct thermal decomposition will lead to low lithium yield, high energy consumption, long time, low reduction rate, low metal yield, complicated process, low yield and increasing production cost.

[0085] Through repeated verification, the impurity contents in the lithium metal are better than those specified in Standards GB/T4369-2015, Li-1 and Li-2.

Experiment 1

[0086] The same methods and steps in Embodiment 1 are used for experiment to determine influences on the form of the lithium in the condensed state that is finally prepared due to different temperatures within the first and second condensing chambers of the temperature control device and at an outlet of the first condensing chamber. These specific results are as follows:

TABLE-US-00006 Outlet of first Second First condensing condensing chamber condensing chamber (° C.) (° C.) chamber (° C.) Configuration Test result 850 750 90 Fluffy, condensed metal General 750 680 70 Condensed metal, easily Good collected 650 600 40 Condensed metal, Poor uneasily collected

[0087] It can be seen from the tests that a condensed metal of the magnesium-lithium alloy, formed when a temperature of the first condensing chamber is 750° C. and a temperature of the second condensing chamber is 70° C., is the best and easily collected. When the temperatures of the first and second condensing chambers are high, the magnesium-lithium alloy is fluffy and has a general form. If the temperatures of the first and second condensing chambers are too low, the formed condensed metal is collected uneasily, and cannot form the briquettes.

Experiment 2

[0088] The same methods and steps in Embodiment 1 are used for experiment to determine the influences of different reduction temperatures and time, and different reduction vacuum degrees on the lithium reduction, as shown in the table below:

TABLE-US-00007 Reduction Reduction Reduction temperature time vacuum degree Li reduction (° C.) (min) (pa) rate (%) 1000 600 3 61.1 1050 600 2 71.8 1100 600 4 81.6 1150 600 3 91.5 1200 600 2 99.3

[0089] as can be seen from the table, the lithium reduction rate is better when the temperature is 1,200° C. and the reduction time is 10 h.

[0090] Those skilled in the art should be able to implement or use the present invention, after reading the description of the embodiments disclosed above. Various modifications to these embodiments will be obvious to those skilled in the art. The general principle defined herein can be implemented in other embodiments without departing from the spirit or scope of the present invention. Thus, the present invention will not be intended to be limited to these embodiments herein, and the broadest scope consistent with the principles and novel features disclosed herein shall prevail.