CN104388688B - A kind of device and method of vacuum metal thermal reduction refining lithium - Google Patents
A kind of device and method of vacuum metal thermal reduction refining lithium Download PDFInfo
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Abstract
The device and method of a kind of vacuum metal thermal reduction refining lithium, device includes heating resistor stove and retort；Charging basket, travel(l)ing rest and support tube it is placed with in retort；Travel(l)ing rest is placed on charging basket top, and support tube is placed on travel(l)ing rest；Catcher is placed on fixed support, and condenser is placed on the collector；Method sequentially includes the following steps: (1) and is placed in charging basket by refining lithium reaction mass；(2) capping tank, evacuation, pass into cooling water, by the heating material in charging basket, carry out vacuum-thermal reduction reaction；Lithium metal steam enters catcher after condensing on condenser；(3) stop heating, pass into noble gas to normal pressure, retort is down to room temperature, catcher obtains lithium metal.Assembly of the invention simple in construction, easy to operate, it is adaptable to large-scale production, by the combination of charging basket, travel(l)ing rest and support tube, make the placement of material and take out more convenient.
Description
Technical field
The invention belongs to metallurgical technology field, refine the device and method of lithium particularly to a kind of vacuum metal thermal reduction.
Background technology
Lithium metal has the physicochemical property of uniqueness, is widely used in the emerging fields such as Aero-Space, nuclear energy power generation, energy battery, and demand increases severely in recent years.The production method of lithium metal mainly has 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, relatively costly；In primary production, the objectionable impurities such as sodium, potassium content is higher；Anodic gas is chlorine, contaminated environment, etching apparatus；Technological process is long.And vacuum-thermal method can be directly relatively low for cost of material with technical grade lithium carbonate or Lithium hydrate；And cause that crystallization position is different owing to lithium metal is different from the vapour pressure of sodium and potassium, therefore the content of objectionable impurities is extremely low；In production process without harmful gas generation；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 thermal reduction and metallothermic processes according to the difference of reducing agent.Carbothermic method and hydrogen thermal reduction owing to reduction temperature is high, not easily operation, lithium metal grade be low etc., and reason is not easy to carry out commercial introduction；And refine lithium with the metallothermic processes of silicon, aluminum and alloy thereof and there is most industrial application value, the pilot-plant test of existing metallothermic reduction refining lithium is seen in bibliographical information at present.But the collection technique that the main cause that restriction the method is promoted is lithium metal is immature, affects production efficiency, cause that the energy consumption of unit mass lithium metal is relatively big, production cost is higher.
Summary of the invention
For the existing method above shortcomings preparing lithium metal, the present invention provides the device and method of a kind of vacuum metal thermal reduction refining lithium, condenser and catcher are arranged in retort, lithium metal steam is produced by adding heat refining lithium material, directly collect in retort, while improving production efficiency, the yield of lithium metal is greatly improved.
The device of the vacuum metal thermal reduction refining lithium of the present invention includes heating resistor stove and retort；The bottom of retort is positioned at heating resistor stove, and the top of retort is provided with cooling jacket；The top of retort and blind flange are tightly connected, and blind flange is provided with vacuum port and air-filled pore；Wherein it is placed with charging basket, travel(l)ing rest and support tube in retort；Charging basket is positioned at bottom retort and is 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 catcher is placed on fixed support, and condenser is placed on the collector, and catcher and condenser are positioned at the top of heating resistor stove；In first thermocouple and the second thermocouple insertion reaction tank, the bottom of the first thermocouple is between catcher and condenser, and the bottom of the second thermocouple is positioned at charging basket.
Above-mentioned catcher 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 outer 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 loop configuration, and the upper and lower surface of condensate film is identical with the side wall construction of round platform, and the upright projection structure of condensate film is identical with the upright projection structure of catcher；When condenser is made up of multiple condensate films, each condensate film arranges from top to bottom and is fixed together by condensing support, except the condensate film of the superiors, all the other each condensate films is equipped with through hole.
In said apparatus, outside retort, it is additionally provided with insulation resistance furnace, between heating resistor stove and cooling jacket.
The method of the vacuum metal thermal reduction refining lithium of the present invention is to adopt said apparatus, sequentially includes the following steps:
1, refining lithium reaction mass is placed in charging basket；The preparation method of described refining lithium reaction mass is: being pressed into ball-type agglomerate containing after lithium raw material and additive mix homogeneously, when 700 ~ 1000 DEG C and vacuum≤100Pa, calcining 1 ~ 2h, obtains containing lithium grog；Will be broken and levigate to granularity≤80 μm respectively with reducing agent containing lithium grog, remix and uniformly obtain mixed powder, mixed powder is pressed into ball-type agglomerate as refining lithium reaction mass；
2, the retort equipped with charging basket is closed, by vacuum port, retort is evacuated to pressure≤10Pa, cooling water is passed in cooling jacket, by heating resistor stove by the heating material in charging basket, the temperature measured when the second thermocouple is 1000 ~ 1250 DEG C, and controlling the temperature that the first thermocouple measures is 200 ~ 600 DEG C, carries out vacuum-thermal reduction reaction, and the response time is at 1.5 ~ 6h；The lithium metal steam produced in course of reaction enters catcher after condensing on condenser；
3, stop heating after having reacted, when the temperature in retort is down to temperature that the first thermocouple measures lower than lithium metal fusing point, in retort, passes into noble gas to normal pressure by air-filled pore, retort is down to room temperature, catcher obtains lithium metal.
In said method, during preparation refining lithium reaction mass, selection is lithium carbonate containing lithium raw material；The additive selected is calcium oxide, and the reducing agent of selection is Antaciron；Containing lithium raw material and additive mixed proportion be containing lithium raw material in molar ratio:Additive=1:(2 ~ 3), it is (3.3 ~ 4) that the mixed proportion containing lithium grog with reducing agent presses the mol ratio containing the lithium in lithium grog with the silicon in reducing agent: 1.
In said method, noble gas is incorporated to normal pressure in retort, for ensureing that the lithium metal on condenser is fully collected, retort is heated by the insulation resistance furnace outside by retort, control temperature that the first thermocouple measures at 200 ~ 300 DEG C, insulation 0.5 ~ 2h, is then shut off insulation resistance furnace and retort is down to room temperature.
In said method, yield >=95% of lithium metal.
In above-mentioned Antaciron, the weight content of silicon is between 70 ~ 100%.
Above-mentioned noble gas selects argon.
Assembly of the invention simple in construction, easy to operate, it is adaptable to large-scale production, pass through charging basket, the combination of travel(l)ing rest and support tube, makes the placement of material and takes out more convenient, the method for the present invention can 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 the vacuum metal thermal reduction refining lithium of the present invention；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, cooling jacket, 8, fastening bolt, 9, air-filled pore, the 10, first thermocouple, 11, vacuum port, 12, sealing gasket, 13, condenser, 14, lithium metal, 15, catcher, 16, fixed support, 17, support tube, 18, the second thermocouple, 19, condenser brackets, 20, blind flange；
Fig. 2 is the catcher cross-sectional view in the embodiment of the present invention；
Fig. 3 is the top 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 top 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.
Detailed description of the invention
The material of the charging basket, travel(l)ing rest, support tube, catcher and the condenser that adopt in the embodiment of the present invention is high temperature resistant stainless steel.
The lithium carbonate, calcium oxide and the Antaciron that adopt in the embodiment of the present invention are commercial technical grade product.
In the embodiment of the present invention, noble gas selects argon.
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 films, the through hole being provided with on the condensate film of through hole is uniformly distributed on condensate film, and the gross area of each through hole is the 15 ~ 70% of the condensate film upper surface gross area.
In the embodiment of the present invention, in condensate film, diameter of a circle meets simultaneously by the first thermocouple and the second thermocouple, and the height of condensate film is the 1/4 ~ 3/2 of outside diameter.
Embodiment 1
The apparatus structure of vacuum metal thermal reduction refining lithium is as it is shown in figure 1, include 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 cooling jacket 7；The top of retort 6 and blind flange 20 are tightly connected, and blind flange 20 is provided with vacuum port 11 and air-filled pore 9；
Blind flange 20 is fixed together with retort 6 by fastening bolt 8, is provided with sealing gasket 12 between blind flange 20 and retort 6；
Wherein it is placed with charging basket 3, travel(l)ing rest 4 and support tube 17 in retort 6；Charging basket 3 is positioned at bottom retort 6 and is 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 catcher 15 is placed on fixed support 16, and condenser 13 is placed on catcher 15, and catcher 15 and condenser 13 are positioned at the top of heating resistor stove 1；
In first thermocouple 10 and the second thermocouple 18 insertion reaction tank 6, the bottom of the first thermocouple 10 is between catcher 15 and condenser 13, and the bottom of the second thermocouple 18 is positioned at charging basket 3；
Collector structure as shown in Figures 2 and 3, 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 outer cylinder is connected with the outside of annular bottom plate；
Condenser 13 is formed by by 3 condensate films, and condensate film is loop configuration, and the upper and lower surface of condensate film is identical with the side wall construction of round platform, and the upright projection structure of condensate film is identical with the upright projection structure of catcher；Each condensate film arranges from top to bottom and is fixed together by condensing 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 is as shown in Figures 4 and 5, and all the other condensate film structures are as shown in Figure 6；
Retort 6 is outside is additionally provided with insulation resistance furnace 5, between heating resistor stove 1 and cooling jacket 7；
The method of vacuum metal thermal reduction refining lithium is to adopt said apparatus, sequentially includes the following steps:
1, refining lithium reaction mass is placed in charging basket；The preparation method of described refining lithium reaction mass is: being pressed into ball-type agglomerate after lithium carbonate and calcium oxide 1:2 mix homogeneously in molar ratio, when 700 DEG C and vacuum≤100Pa, calcining 2h, obtains containing lithium grog；Will be broken and levigate to granularity≤80 μm respectively with Antaciron containing lithium grog, remix and uniformly obtain mixed powder, mixed proportion is 3.3:1 by the mol ratio containing the lithium in lithium grog with the silicon in Antaciron；Mixed powder is pressed into ball-type agglomerate as refining lithium reaction mass；The wherein weight content 70% of silicon in Antaciron；
2, the retort equipped with charging basket is closed, by vacuum port, retort is evacuated to pressure≤10Pa, cooling water is passed in cooling jacket, by heating resistor stove by the heating material in charging basket, the temperature measured when the second thermocouple is 1000 ~ 1250 DEG C, and controlling the temperature that the first thermocouple measures is 200 ~ 600 DEG C, carries out vacuum-thermal reduction reaction, and the response time is at 6h；The lithium metal steam produced in course of reaction enters catcher after condensing on condenser；
3, stop heating after having reacted, when the temperature in retort is down to temperature that the first thermocouple measures lower than lithium metal fusing point, in retort, passes into noble gas to normal pressure by air-filled pore, retort is down to room temperature, catcher obtains lithium metal；
Noble gas is incorporated to normal pressure in retort, for ensureing that the lithium metal on condenser is fully collected, retort is heated by the insulation resistance furnace outside by retort, control temperature that the first thermocouple measures at 200 ~ 300 DEG C, insulation 0.5h, is then shut off insulation resistance furnace and retort is down to room temperature；
The yield 97% of lithium metal.
Embodiment 2
The apparatus structure of vacuum metal thermal reduction refining lithium is with embodiment 1, and difference is in that:
Condenser is formed 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 in that:
Lithium carbonate and calcium oxide 1:2.5 in molar ratio mixes, and when 850 DEG C and vacuum≤100Pa, calcining 1.5h, obtains containing lithium grog；
It is 3.6:1 containing lithium grog and Antaciron mixed proportion by the mol ratio containing the lithium in lithium grog with the silicon in Antaciron；In Antaciron, the weight content of silicon is 85%；
Vacuum-thermal reduction is reacted, and the response time is at 4h；
Retort is heated by the insulation resistance furnace outside by retort, controls temperature that the first thermocouple measures at 200 ~ 300 DEG C, is incubated 1h；
The yield 96% of lithium metal.
Embodiment 3
The apparatus structure of vacuum metal thermal reduction refining lithium is with embodiment 1, and difference is in that:
Condenser is formed by by 1 condensate film, it does not have be provided with the condensate film of through hole；
The method of vacuum metal thermal reduction refining lithium is with embodiment 1, and difference is in that:
Lithium carbonate and calcium oxide 1:3 in molar ratio mixes, and when 1000 DEG C and vacuum≤100Pa, calcining 1h, obtains containing lithium grog；
It is 4:1 containing lithium grog and Antaciron mixed proportion by the mol ratio containing the lithium in lithium grog with the silicon in Antaciron；In Antaciron, the weight content of silicon is 98%；
Vacuum-thermal reduction is reacted, and the response time is at 1.5h；
Retort is heated by the insulation resistance furnace outside by retort, controls temperature that the first thermocouple measures at 200 ~ 300 DEG C, is incubated 2h；
The yield 95% of lithium metal.
Claims (8)
1. a device for vacuum metal thermal reduction refining lithium, including heating resistor stove and retort；The bottom of retort is positioned at heating resistor stove, and the top of retort is provided with cooling jacket；The top of retort and blind flange are tightly connected, and blind flange is provided with vacuum port and air-filled pore；It is characterized in that: in retort, be placed with charging basket, travel(l)ing rest and support tube；Charging basket is positioned at bottom retort and is 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 catcher is placed on fixed support, and condenser is placed on the collector, and catcher and condenser are positioned at the top of heating resistor stove；In first thermocouple and the second thermocouple insertion reaction tank, the bottom of the first thermocouple is between catcher and condenser, and the bottom of the second thermocouple is positioned at charging basket.
2. the device of a kind of vacuum metal thermal reduction according to claim 1 refining lithium, it is characterized in that described catcher 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 outer cylinder is connected with the outside of annular bottom plate.
3. the device of a kind of vacuum metal thermal reduction according to claim 1 refining lithium, it is characterized in that described condenser is made up of at least one condensate film, condensate film is loop configuration, the upper and lower surface of condensate film is identical with the side wall construction of round platform, and the upright projection structure of condensate film is identical with the upright projection structure of catcher；When condenser is made up of multiple condensate films, each condensate film arranges from top to bottom and is fixed together by condensing 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 according to claim 1 refining lithium, it is characterised in that be additionally provided with insulation resistance furnace outside described retort, between heating resistor stove and cooling jacket.
5. the method for a vacuum metal thermal reduction refining lithium, it is characterised in that adopt the device described in claim 1, sequentially include the following steps:
(1) refining lithium reaction mass is placed in charging basket；The preparation method of described refining lithium reaction mass is: being pressed into ball-type agglomerate containing after lithium raw material and additive mix homogeneously, when 700 ~ 1000 DEG C and vacuum≤100Pa, calcining 1 ~ 2h, obtains containing lithium grog；Will be broken and levigate to granularity≤80 μm respectively with reducing agent containing lithium grog, remix and uniformly obtain mixed powder, mixed powder is pressed into ball-type agglomerate as refining lithium reaction mass；
(2) retort equipped with charging basket is closed, by vacuum port, retort is evacuated to pressure≤10Pa, cooling water is passed in cooling jacket, by heating resistor stove by the heating material in charging basket, the temperature measured when the second thermocouple is 1000 ~ 1250 DEG C, and controlling the temperature that the first thermocouple measures is 200 ~ 600 DEG C, carries out vacuum-thermal reduction reaction, and the response time is at 1.5 ~ 6h；The lithium metal steam produced in course of reaction enters catcher after condensing on condenser；
(3) stop heating after having reacted, when the temperature in retort is down to temperature that the first thermocouple measures lower than lithium metal fusing point, in retort, passes into noble gas to normal pressure by air-filled pore, retort is down to room temperature, catcher obtains lithium metal.
6. the method for a kind of vacuum metal thermal reduction according to claim 5 refining lithium, it is characterised in that during preparation refining lithium reaction mass, selection is lithium carbonate containing lithium raw material；The additive selected is calcium oxide, and the reducing agent of selection is Antaciron；Mixed proportion containing lithium raw material Yu additive is containing lithium raw material in molar ratio: additive=1:(2 ~ 3), it is (3.3 ~ 4) that the mixed proportion containing lithium grog with reducing agent presses the mol ratio containing the lithium in lithium grog with the silicon in reducing agent: 1.
7. the method for a kind of vacuum metal thermal reduction according to claim 5 refining lithium, it is characterized in that in retort, incorporating noble gas to normal pressure, for ensureing that the lithium metal on condenser is fully collected, retort is heated by the insulation resistance furnace outside by retort, control temperature that the first thermocouple measures at 200 ~ 300 DEG C, insulation 0.5 ~ 2h, is then shut off insulation resistance furnace and retort is down to room temperature.
8. the method for a kind of vacuum metal thermal reduction according to claim 5 refining lithium, it is characterised in that yield >=95% of lithium metal.
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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 |
| CN109482892B (en) * | 2018-12-28 | 2024-01-23 | 山东重山光电材料股份有限公司 | Production method and production device of lithium silicon alloy |
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