CN104388688A - Device and method for smelting lithium through vacuum thermal reduction of metal - Google Patents
Device and method for smelting lithium through vacuum thermal reduction of metal Download PDFInfo
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Abstract
The invention discloses a device and method for smelting lithium through vacuum thermal reduction of metal. The device comprises a heating resistance furnace and a reaction tank, wherein a charging basket, a movable support and a supporting cylinder are placed in the reaction tank; the movable support is placed at the top of the charging basket, and the supporting cylinder is placed on the movable support; and a collector is placed on a fixed support, and a condenser is placed on the collector. The method comprises the following steps of (1) placing reaction materials for smelting lithium into the charging basket; (2) sealing the reaction tank, vacuumizing, introducing cooling water, heating the materials in the charging basket, and carrying out vacuum thermal reduction reaction; condensing lithium metal steam on the condenser, and then, enabling the lithium metal steam to enter the collector; and (3) stopping heating, introducing inert gases to a normal-pressure environment, and cooling the reaction tank to normal temperature to obtain lithium metal in the collector. The device disclosed by the invention is simple in structure, convenient to operate and suitable for large-scale production; and due to the combination of the charging basket, the movable support and the supporting cylinder, the materials can be more conveniently placed and taken out.
Description
Technical field
The invention belongs to metallurgical technology field, particularly a kind of device and method of vacuum metal thermal reduction refining lithium.
Background technology
Metallic lithium has unique physicochemical property, is widely used in the emerging fields such as aerospace, nuclear energy power generation, energy battery, and demand increases severely in recent years.The production method of metallic lithium mainly contains fused salt electrolysis process and vacuum-thermal method.Fused salt electrolysis process is the main method of current commercial production of metals lithium, technical maturity, but the raw materials for production of this technique are industrial grade methanol, and cost is higher; In first product, the detrimental impurity such as sodium, potassium content is higher; Anodic gas is chlorine, contaminate environment, etching apparatus; Technical process is long.And vacuum-thermal method can directly with technical grade Quilonum Retard or lithium hydroxide for raw materials cost is lower; And due to metallic lithium different from the different crystallization position that causes of vapour pressure of sodium and potassium, therefore the content of detrimental impurity is extremely low; Without harmful gas generation in production process; So vacuum-thermal method is a kind of refining lithium method having prospects for commercial application.
Vacuum-thermal method can be divided into carbothermic method, hydrogen hot reducing method and metallothermics according to the difference of reductive agent.Carbothermic method and hydrogen hot reducing method are not easy to carry out commercial introduction due to reasons such as reduction temperature are high, not easy to operate, metallic lithium grade is low; And with the metallothermics of silicon, Aluminum-aluminum alloy refining lithium, there is industrial application value most, the pilot-plant test of existing metallothermic reduction refining lithium is seen in bibliographical information at present.But the major cause that restriction the method is promoted is that the collection technique of metallic lithium is immature, affect production efficiency, cause the production energy consumption of unit mass metallic lithium comparatively greatly, production cost is higher.
Summary of the invention
For the existing method above shortcomings preparing metallic lithium, the invention provides the device and method of a kind of vacuum metal thermal reduction refining lithium, condenser and collector are arranged in retort, metallic lithium steam is produced by adding heat refining lithium material, directly collect in retort, while enhancing productivity, significantly improve the yield of metallic lithium.
The device of vacuum metal thermal reduction refining lithium of the present invention comprises heating resistor stove and retort; The bottom of retort is positioned at heating resistor stove, and the top of retort is provided with watercooling jacket; Top and the blind flange of retort are tightly connected, and blind flange is provided with vacuum port and aeration aperture; Wherein be placed with charging basket, travel(l)ing rest and support tube in retort; Charging basket to be positioned at bottom retort and to be positioned at the inside of heating resistor stove, and travel(l)ing rest is placed on charging basket top, and support tube is placed on travel(l)ing rest; Support tube inwall is provided with fixed support, and collector is placed on fixed support, and condenser is placed on the collector, and collector and condenser are positioned at the top of heating resistor stove; In first thermopair and the second thermopair insertion reaction tank, the bottom of the first thermopair is between collector and condenser, and the bottom of the second thermopair is positioned at charging basket.
Above-mentioned collector is integrally formed structure by an annular bottom plate and inside and outside cylinder, and the base of inner cylinder is connected with the inner edge of annular bottom plate, and the base of out cylinder is connected with the outside of annular bottom plate.
Above-mentioned condenser is made up of at least one condensate film, and condensate film is ring structure, and the upper and lower surface of condensate film is identical with the side structure of round platform, and the vertical projection structure of condensate film is identical with the vertical projection structure of collector; When condenser is made up of multiple condensate film, each condensate film is arranged from top to bottom and is fixed together by condensation support, except the condensate film of the superiors, all the other each condensate films is equipped with through hole.
In said apparatus, retort outside is also provided with insulation resistance furnace, between heating resistor stove and watercooling jacket.
The method of vacuum metal thermal reduction refining lithium of the present invention adopts said apparatus, carries out according to the following steps:
1, refining lithium reaction mass is placed in charging basket; The preparation method of described refining lithium reaction mass is: be pressed into ball-type agglomerate after mixing containing lithium raw material and additive, and calcining 1 ~ 2h under 700 ~ 1000 DEG C and vacuum tightness≤100Pa condition, obtains containing lithium grog; Will be broken respectively and levigate to granularity≤80 μm containing lithium grog and reductive agent, remix evenly obtains mixed powder, mixed powder is pressed into ball-type agglomerate as refining lithium reaction mass;
2, the retort that charging basket is housed is closed, by vacuum port, retort is evacuated to pressure≤10Pa, water coolant is passed in watercooling jacket, by heating resistor stove by the heating material in charging basket, the temperature measured when the second thermopair is 1000 ~ 1250 DEG C, and controlling the temperature that the first thermopair measures is 200 ~ 600 DEG C, and carry out vacuum-thermal reduction reaction, the reaction times is at 1.5 ~ 6h; The metallic lithium steam produced in reaction process enters collector after condensation on condenser;
3, reacted rear stopping heating, when the temperature in retort is down to temperature that the first thermopair measures lower than metallic lithium fusing point, in retort, has passed into rare gas element to normal pressure by aeration aperture, retort is down to normal temperature, in collector, obtain metallic lithium.
In aforesaid method, during preparation refining lithium reaction mass, what select is Quilonum Retard containing lithium raw material; The additive selected is calcium oxide, and the reductive agent selected is ferro-silicon; Containing lithium raw material and additive blending ratio in molar ratio for containing lithium raw material
:additive=1:(2 ~ 3), be (3.3 ~ 4) containing the blending ratio of lithium grog and reductive agent by the mol ratio containing the lithium in lithium grog and the silicon in reductive agent: 1.
In aforesaid method, incorporate rare gas element to normal pressure in retort after, for ensureing that the metallic lithium on condenser is fully collected, by the insulation resistance furnace outside retort, retort is heated, control temperature that the first thermopair measures at 200 ~ 300 DEG C, insulation 0.5 ~ 2h, then closes insulation resistance furnace and retort is down to normal temperature.
In aforesaid method, yield >=95% of metallic lithium.
In above-mentioned ferro-silicon, the weight content of silicon is between 70 ~ 100%.
Above-mentioned rare gas element selects argon gas.
Apparatus structure of the present invention is simple, easy to operate, is applicable to scale operation, passes through charging basket, the combination of travel(l)ing rest and support tube, makes the placement of material and takes out more convenient, method of the present invention can production energy consumption few, cost is low, and product yield and purity are all higher, have a good application prospect.
Accompanying drawing explanation
Fig. 1 is the apparatus structure schematic diagram of vacuum metal thermal reduction of the present invention refining lithium; In figure, 1, heating resistor stove, 2, refining lithium reaction mass, 3, charging basket, 4, travel(l)ing rest, 5, insulation resistance furnace, 6, retort, 7, watercooling jacket, 8, holding bolt, 9, aeration aperture, the 10, first thermopair, 11, vacuum port, 12, gasket, 13, condenser, 14, metallic lithium, 15, collector, 16, fixed support, 17, support tube, 18, the second thermopair, 19, condenser brackets, 20, blind flange;
Fig. 2 is the collector cross-sectional view in the embodiment of the present invention;
Fig. 3 is the vertical view of Fig. 2;
Fig. 4 is the top layer condensate film structural representation in the embodiment of the present invention;
Fig. 5 is the vertical view of Fig. 4;
Move back 6 for the condensate film structural representation with through hole in the embodiment of the present invention 1;
Fig. 7 is the condensate film structural representation with through hole in the embodiment of the present invention 2.
Embodiment
The material of the charging basket adopted in the embodiment of the present invention, travel(l)ing rest, support tube, collector and condenser is high temperature resistant stainless steel.
The Quilonum Retard adopted in the embodiment of the present invention, calcium oxide and ferro-silicon are commercial technical grade product.
In the embodiment of the present invention, rare gas element selects argon gas.
The travel(l)ing rest adopted in the embodiment of the present invention is annular.
In the embodiment of the present invention when condenser is made up of multiple condensate film, the through hole be provided with on the condensate film of through hole is uniformly distributed on condensate film, and the total area of each through hole is 15 ~ 70% of the condensate film upper surface total area.
In the embodiment of the present invention, in condensate film, circular diameter meets simultaneously by the first thermopair and the second thermopair, and the height of condensate film is 1/4 ~ 3/2 of outside diameter.
Embodiment 1
The apparatus structure of vacuum metal thermal reduction refining lithium as shown in Figure 1, comprises heating resistor stove 1 and retort 6; The bottom of retort 6 is positioned at heating resistor stove 1, and the top of retort 6 is provided with watercooling jacket 7; Top and the blind flange 20 of retort 6 are tightly connected, and blind flange 20 is provided with vacuum port 11 and aeration aperture 9;
Blind flange 20 is fixed together by holding bolt 8 and retort 6, is provided with gasket 12 between blind flange 20 and retort 6;
Wherein be placed with charging basket 3, travel(l)ing rest 4 and support tube 17 in retort 6; Charging basket 3 to be positioned at bottom retort 6 and to be positioned at the inside of heating resistor stove 1, and travel(l)ing rest 4 is placed on charging basket 3 top, and support tube 17 is placed on travel(l)ing rest 4;
Support tube 17 inwall is provided with fixed support 16, and collector 15 is placed on fixed support 16, and condenser 13 is placed on collector 15, and collector 15 and condenser 13 are positioned at the top of heating resistor stove 1;
In first thermopair 10 and the second thermopair 18 insertion reaction tank 6, the bottom of the first thermopair 10 is between collector 15 and condenser 13, and the bottom of the second thermopair 18 is positioned at charging basket 3;
As shown in Figures 2 and 3, be integrally formed structure by an annular bottom plate and inside and outside cylinder, the base of inner cylinder is connected with the inner edge of annular bottom plate collector structure, and the base of out cylinder is connected with the outside of annular bottom plate;
Condenser 13 forms by by 3 condensate films, and condensate film is ring structure, and the upper and lower surface of condensate film is identical with the side structure of round platform, and the vertical projection structure of condensate film is identical with the vertical projection structure of collector; Each condensate film is arranged from top to bottom and is fixed together by condensation support 19, except the condensate film of the superiors, all the other each condensate films is equipped with through hole; Wherein the superiors' condensate film structure as shown in Figures 4 and 5, and all the other condensate film structures as shown in Figure 6;
Retort 6 outside is also provided with insulation resistance furnace 5, between heating resistor stove 1 and watercooling jacket 7;
The method of vacuum metal thermal reduction refining lithium adopts said apparatus, carries out according to the following steps:
1, refining lithium reaction mass is placed in charging basket; The preparation method of described refining lithium reaction mass is: by Quilonum Retard and calcium oxide in molar ratio 1:2 be pressed into ball-type agglomerate after mixing, under 700 DEG C and vacuum tightness≤100Pa condition, calcine 2h, obtain containing lithium grog; Will be broken respectively and levigate to granularity≤80 μm containing lithium grog and ferro-silicon, remix evenly obtains mixed powder, and blending ratio is 3.3:1 by the mol ratio containing the lithium in lithium grog and the silicon in ferro-silicon; Mixed powder is pressed into ball-type agglomerate as refining lithium reaction mass; The wherein weight content 70% of silicon in ferro-silicon;
2, the retort that charging basket is housed is closed, by vacuum port, retort is evacuated to pressure≤10Pa, water coolant is passed in watercooling jacket, by heating resistor stove by the heating material in charging basket, the temperature measured when the second thermopair is 1000 ~ 1250 DEG C, and controlling the temperature that the first thermopair measures is 200 ~ 600 DEG C, and carry out vacuum-thermal reduction reaction, the reaction times is at 6h; The metallic lithium steam produced in reaction process enters collector after condensation on condenser;
3, reacted rear stopping heating, when the temperature in retort is down to temperature that the first thermopair measures lower than metallic lithium fusing point, in retort, has passed into rare gas element to normal pressure by aeration aperture, retort is down to normal temperature, in collector, obtain metallic lithium;
Incorporate rare gas element to normal pressure in retort after, for ensureing that the metallic lithium on condenser is fully collected, by the insulation resistance furnace outside retort, retort is heated, control temperature that the first thermopair measures at 200 ~ 300 DEG C, insulation 0.5h, then closes insulation resistance furnace and retort is down to normal temperature;
The yield 97% of metallic lithium.
Embodiment 2
The apparatus structure of vacuum metal thermal reduction refining lithium is with embodiment 1, and difference is:
Condenser forms by by 2 condensate films, is provided with the condensate film structure of through hole as shown in Figure 7;
The method of vacuum metal thermal reduction refining lithium is with embodiment 1, and difference is:
The 1:2.5 mixing in molar ratio of Quilonum Retard and calcium oxide, calcines 1.5h under 850 DEG C and vacuum tightness≤100Pa condition, obtains containing lithium grog;
Be 3.6:1 containing lithium grog and ferro-silicon blending ratio by the mol ratio containing the lithium in lithium grog and the silicon in ferro-silicon; In ferro-silicon, the weight content of silicon is 85%;
Vacuum-thermal reduction is reacted, and the reaction times is at 4h;
By the insulation resistance furnace outside retort, retort is heated, control temperature that the first thermopair measures at 200 ~ 300 DEG C, insulation 1h;
The yield 96% of metallic lithium.
Embodiment 3
The apparatus structure of vacuum metal thermal reduction refining lithium is with embodiment 1, and difference is:
Condenser forms by by 1 condensate film, is not provided with the condensate film of through hole;
The method of vacuum metal thermal reduction refining lithium is with embodiment 1, and difference is:
The 1:3 mixing in molar ratio of Quilonum Retard and calcium oxide, calcines 1h under 1000 DEG C and vacuum tightness≤100Pa condition, obtains containing lithium grog;
Be 4:1 containing lithium grog and ferro-silicon blending ratio by the mol ratio containing the lithium in lithium grog and the silicon in ferro-silicon; In ferro-silicon, the weight content of silicon is 98%;
Vacuum-thermal reduction is reacted, and the reaction times is at 1.5h;
By the insulation resistance furnace outside retort, retort is heated, control temperature that the first thermopair measures at 200 ~ 300 DEG C, insulation 2h;
The yield 95% of metallic lithium.
Claims (8)
1. a device for vacuum metal thermal reduction refining lithium, comprises heating resistor stove and retort; The bottom of retort is positioned at heating resistor stove, and the top of retort is provided with watercooling jacket; Top and the blind flange of retort are tightly connected, and blind flange is provided with vacuum port and aeration aperture; It is characterized in that: in retort, be placed with charging basket, travel(l)ing rest and support tube; Charging basket to be positioned at bottom retort and to be positioned at the inside of heating resistor stove, and travel(l)ing rest is placed on charging basket top, and support tube is placed on travel(l)ing rest; Support tube inwall is provided with fixed support, and collector is placed on fixed support, and condenser is placed on the collector, and collector and condenser are positioned at the top of heating resistor stove; In first thermopair and the second thermopair insertion reaction tank, the bottom of the first thermopair is between collector and condenser, and the bottom of the second thermopair is positioned at charging basket.
2. the device of a kind of vacuum metal thermal reduction refining lithium according to claim 1, it is characterized in that described collector is integrally formed structure by an annular bottom plate and inside and outside cylinder, the base of inner cylinder is connected with the inner edge of annular bottom plate, and the base of out cylinder is connected with the outside of annular bottom plate.
3. the device of a kind of vacuum metal thermal reduction refining lithium according to claim 1, it is characterized in that described condenser is made up of at least one condensate film, condensate film is ring structure, the upper and lower surface of condensate film is identical with the side structure of round platform, and the vertical projection structure of condensate film is identical with the vertical projection structure of collector; When condenser is made up of multiple condensate film, each condensate film is arranged from top to bottom and is fixed together by condensation support, except the condensate film of the superiors, all the other each condensate films is equipped with through hole.
4. the device of a kind of vacuum metal thermal reduction refining lithium according to claim 1, is characterized in that described retort outside is also provided with insulation resistance furnace, between heating resistor stove and watercooling jacket.
5. a method for vacuum metal thermal reduction refining lithium, is characterized in that adopting device according to claim 1, carries out according to the following steps:
(1) refining lithium reaction mass is placed in charging basket; The preparation method of described refining lithium reaction mass is: be pressed into ball-type agglomerate after mixing containing lithium raw material and additive, and calcining 1 ~ 2h under 700 ~ 1000 DEG C and vacuum tightness≤100Pa condition, obtains containing lithium grog; Will be broken respectively and levigate to granularity≤80 μm containing lithium grog and reductive agent, remix evenly obtains mixed powder, mixed powder is pressed into ball-type agglomerate as refining lithium reaction mass;
(2) retort that charging basket is housed is closed, by vacuum port, retort is evacuated to pressure≤10Pa, water coolant is passed in watercooling jacket, by heating resistor stove by the heating material in charging basket, the temperature measured when the second thermopair is 1000 ~ 1250 DEG C, and controlling the temperature that the first thermopair measures is 200 ~ 600 DEG C, and carry out vacuum-thermal reduction reaction, the reaction times is at 1.5 ~ 6h; The metallic lithium steam produced in reaction process enters collector after condensation on condenser;
(3) reacted rear stopping heating, when the temperature in retort is down to temperature that the first thermopair measures lower than metallic lithium fusing point, in retort, has passed into rare gas element to normal pressure by aeration aperture, retort is down to normal temperature, in collector, obtain metallic lithium.
6. the method for a kind of vacuum metal thermal reduction refining lithium according to claim 5, when it is characterized in that preparation refining lithium reaction mass, what select is Quilonum Retard containing lithium raw material; The additive selected is calcium oxide, and the reductive agent selected is ferro-silicon; Containing lithium raw material and additive blending ratio in molar ratio for containing lithium raw material: additive=1:(2 ~ 3), be (3.3 ~ 4) containing the blending ratio of lithium grog and reductive agent by the mol ratio of the lithium contained in lithium grog and the silicon in reductive agent: 1.
7. the method for a kind of vacuum metal thermal reduction refining lithium according to claim 5, after it is characterized in that incorporating rare gas element to normal pressure in retort, for ensureing that the metallic lithium on condenser is fully collected, by the insulation resistance furnace outside retort, retort is heated, control temperature that the first thermopair measures at 200 ~ 300 DEG C, insulation 0.5 ~ 2h, then closes insulation resistance furnace and retort is down to normal temperature.
8. the method for a kind of vacuum metal thermal reduction refining lithium according to claim 5, is characterized in that yield >=95% of metallic lithium.
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| CN107385230A (en) * | 2017-07-31 | 2017-11-24 | 重庆科技学院 | A kind of steel-making dust recoverying and utilizing method and its vacuum reduction furnace equipment used |
| CN108165768A (en) * | 2018-01-15 | 2018-06-15 | 东北大学 | The apparatus and method of lithium are produced in a kind of vacuum metal thermal reduction |
| CN109482892A (en) * | 2018-12-28 | 2019-03-19 | 山东重山光电材料股份有限公司 | A kind of production method and process units of Li-Si alloy |
| CN116426770A (en) * | 2023-03-24 | 2023-07-14 | 宜春国轩电池有限公司 | Metal lithium high-temperature steam collecting device and metal lithium reduction tank using same |
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