CN110436489A - A kind of method for innocent treatment of lithium metal - Google Patents
A kind of method for innocent treatment of lithium metal Download PDFInfo
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- CN110436489A CN110436489A CN201910786382.8A CN201910786382A CN110436489A CN 110436489 A CN110436489 A CN 110436489A CN 201910786382 A CN201910786382 A CN 201910786382A CN 110436489 A CN110436489 A CN 110436489A
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
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Abstract
The invention discloses a kind of method for innocent treatment of lithium metal.The described method includes: (1) is reacted with the reactant of atomization with lithium metal, obtained after reaction containing lithium mixture；(2) it will contain described in step (1) and be reacted in lithium mixture immersion reactant, and obtain lithium-containing solution.This method controls reaction process by the reactant additional amount of control atomization, the passivation layer that the reactant and lithium metal of atomization generate is covered on metallic lithium surface, slow down reaction process, after being immersed what is do not reacted completely in reactant containing lithium mixture, passivation layer is dissolved in reactant, and lithium metal continues in passivation layer solution and reaction reaction, passes through the process of above-mentioned multi-step substep control reaction, the severity for controlling reaction improves the safety of harmless treatment lithium metal.It is passed through the concentration for the passivation composition of layer that carbon dioxide can be avoided in frequently processing or adjustment reactant, the lithium carbonate of easy safe retrieving can also be obtained.
Description
Technical field
The invention belongs to waste processing arts, are related to a kind of method for innocent treatment more particularly to a kind of lithium metal
Method for innocent treatment.
Background technique
Lithium metal has a wide range of applications in lithium electrical domain, and application while brings waste residue containing lithium metal, leftover pieces
The generation of equal waste materials easily occurs with moisture, oxygen, the nitrogen in air complicated in a natural environment since lithium metal is unstable
Chemical reaction:
4Li+O2=2Li2O
Li2O+CO2=Li2CO3
Li2O+H2O=2LiOH
Li+H2O=LiOH+0.5H2
6Li+N2=2Li3N,
Although the heat generated in the unit time is less, if cannot be processed in time, heat cannot discharge in time,
By gathering for a long time, the temperature of scrap heap will be gradually risen until reaching spontaneous combustion or even open fire occur, lithium metal is generally answered
It deposits in the glove box of atoleine, solid paraffin, albolene or applying argon gas, since Li electricity company lithium metal waste material is discarded
Amount cannot reach lithium metal manufacturing enterprise scale but discarded lithium metal needs to carry out safe processing in time so that being difficult to be formed
Lithium metal waste material, is generally stored in dry room using the Li electricity company of metal lithium material, still by scale recycling at present
Accumulation and closely knit accumulation not only occupied space position, also increase the security risk of company.
The processing method of the waste material containing lithium metal specifically includes that in the prior art
1, directly lithium slag is added to the water and is hydrolyzed, control the reaction interval of hydrolysis by controlling the additional amount of lithium slag
Degree.Since lithium slag reacts acutely in water, a large amount of heat and imflammable gas hydrogen can be generated, it is therefore desirable to which strict control is each
The treating capacity of lithium slag, process cycle are longer.Since reaction generates hydrogen and generates amount of heat, safety hazard is high, Yi Fasheng
Explosion.
2, lithium metal is recycled by the method for hydrometallurgic recovery, complex technical process, energy consumption is higher, realizes industrial applications
It is difficult.
3, high temperature burning handling lithium metal waste residue and lithium metal is recycled, easily causes one combust of lithium metal, controlled non-
Often difficult, risk factor is high.Lithium metal can not be directly recycled, while flue gas can be taken away largely containing lithiumation conjunction in lithium metal burning
The dust of object causes air pollution and lithium resource to lose.
CN206368190U provides the recycling reaction unit and processing unit of a kind of lithium metal slag, uses in the program close
Lithium hydroxide solution is saturated to reduce the reaction rate of water and lithium slag, to reduce the risk of lithium metal waste disposal.But it is entire
Process efficiency is low, and lithium metal waste disposal amount is small, and process requirement is pre-configured with lithium hydroxide solution, and lithium hydroxide solution reaches
Reaction rate further decreases after saturation, is whether diluted or replaces saturated solution and both increase the complexity of technique.
CN109248904A discloses the method for innocent treatment and system of a kind of lithium metal waste residue, and the program includes: to mention
For liquid-phase system, the liquid-phase system includes the oily mutually with water phase of layering, oily to be mutually distributed in above water phase, and oil phase and lithium metal
Waste residue does not react；The liquid-phase system is added in lithium metal waste residue, and is distributed in lithium metal waste residue in the oily phase；By metal
Lithium waste residue is pressed into the water phase, reacts lithium metal therein with water, while the lasting hydrogen for removing reaction and generating, and realizes gold
Belong to the harmless treatment of lithium waste residue.But this method is extremely cumbersome, and poor to the control of reaction rate, and in order to control
Water phase temperature, it is necessary to hot water be discharged and refill cold water, this needs to will cause the wasting of resources using a large amount of water.
CN109264750A discloses a kind of method for innocent treatment of lithium metal waste residue, this method comprises: holding accompanying by
In the case where continuous agitation, the mixture of lithium metal waste residue and additive is heated to 250~450 DEG C, and make the mixture with
The harmless treatment of lithium metal waste residue is realized in the reaction of reactant gas continuous contact, and the additive is selected from heat-stable compound,
The reactant gas can react to form stable lithium compound with lithium metal.Although the reaction does not have to water, gas-solid reaction
Reaction efficiency it is low, although safety preferably reaction speed it is too slow, cause time cost higher.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide a kind of harmless treatment side of lithium metal
Method.Method security provided by the invention is high, and reaction speed will not be excessively slow, taken into account the safety of lithium metal recycling with
Efficiency.
To achieve this purpose, the present invention adopts the following technical scheme:
The present invention provides a kind of method for innocent treatment of lithium metal, the described method comprises the following steps:
(1) it is reacted, is obtained after reaction containing lithium mixture with lithium metal with the reactant of atomization；
(2) it will contain described in step (1) and be reacted in lithium mixture immersion reactant, and obtain lithium-containing solution.
It, can be in the Surface Creation one of lithium metal by using the reactant of atomization in the processing method provided by the present invention
Layer passivation layer (such as hydroxide lithium layer), slows down reaction process, prevents and reacts the case where excessively fierceness leads to temperature runaway, simultaneously
It is reacted with the reactant of atomization compared to directly lithium metal is impregnated with reactant, the amount for being limited to reactant is fewer, anti-
It should more easily control, safety can be obviously improved, and the addition speed control temperature of the reactant of atomization can be passed through
And humidity.And when atomization reactant can not with lithium metal the reaction was continued after, passivation layer has covered the table of entire lithium metal
Face, this is that step (1) is described containing lithium mixture, will contain lithium mixture again at this time and be placed in reactant and impregnate, passivation layer dissolution,
The reaction was continued for lithium metal, but the solution of passivation layer (such as lithium hydroxide solution) reduces lithium metal and reacting for reactant is fast
Rate controls reaction process, improves the safety of reaction.Therefore, the processing method provided by the present invention controls swashing for reaction
Strong degree, and process efficiency is also relatively high, is the lithium metal recovery method of a kind of compromise between security and efficiency.
In the present invention, when the temperature of reaction system tends towards stability in step (1), the reactant and lithium metal of atomization are represented
Reaction terminates substantially.
It is used as currently preferred technical solution below, but not as the limitation to technical solution provided by the invention, leads to
Following preferred technical solution is crossed, can preferably reach and realize technical purpose and beneficial effect of the invention.
As currently preferred technical solution, the reactant of step (1) described atomization includes atomized water.Use atomized water
When, lithium hydroxide passivation layer can be formed in metallic lithium surface.
Preferably, the size droplet diameter of the reactant of step (1) described atomization in 2mm hereinafter, such as 2mm, 1.5mm, 1mm,
0.5mm etc..If size droplet diameter is excessive, it will lead to the water that part is reacted with lithium metal and generated margin, the hydroxide of generation
Lithium passivation layer quickly dissolves, and is difficult to control so that reaction is excessively fierce.Restriction size droplet diameter dissolves slow in 2mm or less lithium metal
Point reaction is also slow, avoids reaction process excessively fierce.
Preferably, step (1) lithium metal is lithium metal waste material.
Preferably, the flow velocity of the reactant of step (1) described atomization be 10-100mL/s, such as 10mL/s, 20mL/s,
30mL/s, 40mL/s, 50mL/s, 60mL/s, 70mL/s, 80mL/s, 90mL/s or 100mL/s etc..
As currently preferred technical solution, temperature≤100 DEG C of step (1) described reaction, such as 100 DEG C, 90 DEG C,
80 DEG C, 70 DEG C, 60 DEG C, 50 DEG C, 40 DEG C or 30 DEG C etc., preferably 40-85 DEG C.In the present invention, if the reaction temperature of step (1)
It is excessively high, then it represents that reaction is fiercer, will lead to degree of danger raising, security risk occurs；If reaction temperature is too low, can drop
Low reaction speed, causes process efficiency to reduce.
Preferably, when the temperature of step (1) described reaction is higher than 85 DEG C, reduce the flow velocity of the reactant of atomization, step (1)
When the temperature of the reaction is lower than 40 DEG C, increase the flow velocity of the reactant of atomization.Reaction can effectively be controlled using the above method
Process, and then control exothermic heat of reaction.
Preferably, the humidity of step (1) described reaction be 10-100%, such as 10%, 20%, 30%, 40%, 50%,
60%, 70%, 80%, 90% or 100% etc..
As currently preferred technical solution, step (2) described reactant includes water, and water can dissolve on lithium metal
Passivation layer (such as lithium hydroxide), and continue to react with lithium metal, but passivation layer can inhibit water and gold after being dissolved in water
Belong to the extent of reaction of lithium.
In the present invention, the temperature and time of step (2) described reaction can be selected according to the actual situation, not limited here
Fixed, reaction temperature guarantee will not cause danger.
As currently preferred technical solution, step (1) and step (2) carry out in treatment box.
Preferably, the treatment box includes cooling system.Cooling system can be used and help treatment box cooling.
Preferably, step (1) described lithium metal is placed in the hollow out storage facility in treatment box.It in this way can be to increase gold
Belong to the contact area of the reactant of lithium waste material and atomization.
As currently preferred technical solution, the treatment box is enclosed workshop case.
Preferably, it is lasting in step (1) and step (2) to remove reaction production when the treatment box is enclosed workshop case
Raw hydrogen.
Preferably, when the treatment box is enclosed workshop case, the treatment box includes exhaust valve.Exhaust valve can be passed through
Exclude hydrogen and part reaction heat.The hydrogen of exclusion can be handled by hydrogen treat device.
Preferably, the exhaust valve is equipped with filter device.The lithium-containing compound flue gas that reaction can be generated in this way is by mistake
It filters and is discharged after safe processing.
Preferably, when the treatment box is enclosed workshop case, step (1) and step (2) carry out under an inert atmosphere.
Preferably, the inert atmosphere include in helium atmosphere, neon atmosphere or argon atmosphere any one or at least
Two kinds of combination.
As currently preferred technical solution, the treatment box is non-fully enclosed treatment box.
Preferably, when the treatment box is non-fully enclosed treatment box, step (1) and step (2) are under an oxygen-containing atmosphere
It carries out
Preferably, the oxygen-containing atmosphere includes oxygen and/or air.
Preferably, the hydrogen that step (1) and step (2) generate reaction burns in treatment box.
Combustion of hydrogen is that reaction generates spark, In because lithium metal floats on the water surface in water in non-fully enclosed treatment box
In non-enclosed environment, hydrogen is contacted with oxygen in air and is ignited.
As currently preferred technical solution, the method also includes step (3): being reacted to step (2) is described
Reaction solution in be passed through carbon containing reaction gas, obtain product containing lithium.
It can be passed through carbon containing reaction gas in the reaction process of step (2), and be not necessarily intended to wait after reaction.
As currently preferred technical solution, the carbon containing reaction gas includes carbon dioxide.
Preferably, the product containing lithium is lithium carbonate.
Being passed through carbon dioxide can allow the passivation composition of layer (such as lithium hydroxide) in reactant to be converted into lithium carbonate, avoid
The excessively high reaction speed for making lithium metal and reactant of passivation layer constituent concentration is excessively slow, avoids frequently processing or adjustment reactant
In passivation composition of layer concentration, the lithium carbonate of easy safe retrieving can also be obtained.
As the further preferred technical solution of the method for the invention, the described method comprises the following steps:
(1) it in enclosed workshop case, under inert atmosphere, is reacted with atomized water with lithium metal, the atomized water
Flow velocity is 10-100mL/s, and reaction humidity 10-100%, reaction temperature is 40-85 DEG C, when the temperature of reaction is higher than 85 DEG C, is subtracted
The flow velocity of small atomized water when reaction temperature is lower than 40 DEG C, increases the flow velocity of atomized water, the hydrogen that reaction generates persistently is removed in reaction
Gas is obtained after reaction containing lithium mixture；
Wherein, the size droplet diameter of the atomized water is in 2mm or less；
(2) under inert atmosphere, lithium mixture will be contained described in step (1) in step (1) the enclosed workshop case and immersed
It is reacted in water, the hydrogen that reaction generates persistently is removed in reaction, and Xiang Shuizhong is passed through carbon dioxide, and it is molten to obtain lithium carbonate containing
Liquid；
Or
(1) it in non-fully enclosed treatment box, under oxygen-containing atmosphere, is reacted with atomized water with lithium metal, the atomization
The flow velocity of water is 10-100mL/s, and reaction humidity 10-100%, reaction temperature is 40-85 DEG C, and the temperature of reaction is higher than 85 DEG C
When, reduce the flow velocity of atomized water and increase the flow velocity of atomized water when reaction temperature is lower than 40 DEG C, is obtained after reaction containing lithium mixture,
It burns in treatment box in reaction to the hydrogen of generation；
Wherein, the size droplet diameter of the atomized water is in 2mm or less；
(2) under oxygen-containing atmosphere, lithium mixture will be contained described in step (1) in step (1) the non-fully enclosed treatment box
It is immersed in the water and is reacted, burn, and Xiang Shuizhong is passed through carbon dioxide, obtain in treatment box to the hydrogen of generation in reaction
To lithium carbonate containing solution.
Compared with prior art, the invention has the following advantages:
(1) method provided by the invention controls reaction process by the reactant additional amount of control atomization, atomization it is anti-
The passivation layer (such as lithium hydroxide) for answering agent and lithium metal to generate is covered on metallic lithium surface, slows down reaction process, lithium metal exists
After reaching reaction balance in the reactant of atomization, immersed what is do not reacted completely in reactant containing lithium mixture, passivation layer dissolution
In reactant, lithium metal continues in passivation layer solution and reaction reaction, the metal of the passivation layer constituent reduction in solution
The reaction rate of lithium and reactant, controls reaction process, by the process of above-mentioned multi-step substep control reaction, controls anti-
The severity answered improves the safety of harmless treatment lithium metal.
(2) being passed through carbon dioxide can allow the passivation composition of layer (such as lithium hydroxide) in reactant to be converted into lithium carbonate,
It avoids the excessively high reaction speed for making lithium metal and reactant of passivation layer constituent concentration excessively slow, avoids frequently processing or adjustment is anti-
The concentration for answering the passivation composition of layer in agent, can also obtain the lithium carbonate of easy safe retrieving.Although method provided by the invention increases
The step of being reacted with the reactant being atomized with lithium metal is added, but its treatment effeciency is also higher, can meet industry demand, processing
It is no more than 1h the time required to 500g lithium metal waste material.
Specific embodiment
In order to better illustrate the present invention, it is easy to understand technical solution of the present invention, below further specifically to the present invention
It is bright.But following embodiments is only simple example of the invention, does not represent or limit the scope of the present invention, this
Invention protection scope is subject to claims.
The following are typical but non-limiting embodiments of the invention:
Embodiment 1
The present embodiment carries out the harmless treatment of lithium metal as follows:
(1) it in enclosed workshop case, under argon atmosphere, is reacted with atomized water with lithium metal, the atomized water
Initial flow rate is 50mL/s, and control range of reaction temperature is 40-85 DEG C, when the temperature of reaction is higher than 85 DEG C, reduces atomized water
Flow velocity when reaction temperature is lower than 40 DEG C, increases the flow velocity of atomized water, and the flow rates of atomized water are 10-100mL/s, are reacted wet
Degree is 10-100%, persistently removes the hydrogen that reaction generates with the exhaust valve for the treatment of box in reaction, (reacts and stop substantially after reaction
Only, when temperature tends towards stability) it obtains containing lithium mixture；
Wherein, the size droplet diameter of the atomized water is in about 1.5mm.The exhaust valve for the treatment of box is equipped with filter device, reaction
The lithium-containing compound flue gas of generation is discharged after filtering and safe processing.A part can be discharged by exhaust valve in reaction heat,
It can be cooling by the cooling system being arranged on treatment box.
(2) under argon atmosphere, lithium mixture will be contained described in step (1) in step (1) the enclosed workshop case and immersed
(solid-to-liquid ratio when starting reaction is 20g:1L) is reacted in water, the hydrogen that reaction generates persistently is removed in reaction, and to water
In be passed through carbon dioxide, to (lithium metal is totally consumed) after reaction, obtain Lithium carbonate solution.
The chemical reaction occurred in the present embodiment are as follows:
Li+H2O=LiOH+0.5H2
2LiOH+CO2=Li2CO3+H2O
The safety results of the present embodiment are shown in Table 1.
Embodiment 2
The present embodiment carries out the harmless treatment of lithium metal as follows:
(1) it in non-fully enclosed treatment box, under air atmosphere, is reacted with atomized water with lithium metal, the atomized water
Initial flow rate be 60mL/s, control range of reaction temperature is 40-85 DEG C, when the temperature of reaction is higher than 85 DEG C, reduces atomization
The flow velocity of water when reaction temperature is lower than 40 DEG C, increases the flow velocity of atomized water, and the flow rates of atomized water are 10-100mL/s, instead
Answering humidity is 10-100%, and (i.e. reaction is basic stops, when temperature tends towards stability) obtains containing lithium mixture after reaction, right in reaction
The hydrogen of generation burns in treatment box；
Wherein, the size droplet diameter of the atomized water is about 1mm.Reaction heat can be cooled down by cooling system or by non-complete
Enclosed workshop case natural heat dissipation.
(2) under air atmosphere, lithium mixture will be contained described in step (1) in step (1) the non-fully enclosed treatment box
It is immersed in the water (solid-to-liquid ratio when starting reaction is 25g:1L) to be reacted, the hydrogen of generation is carried out in treatment box in reaction
Burning, and Xiang Shuizhong is passed through carbon dioxide, to (lithium metal is totally consumed) after reaction, obtains lithium carbonate containing solution.
The chemical reaction occurred in the present embodiment are as follows:
Li+H2O=LiOH+0.5H2
2LiOH+CO2=Li2CO3+H2O
2H2+O2=2H2O
The safety results of the present embodiment are shown in Table 1.
Embodiment 3
The present embodiment carries out the harmless treatment of lithium metal as follows:
(1) it in enclosed workshop case, under argon atmosphere, is reacted with atomized water with lithium metal, the atomized water
Initial flow rate is 40mL/s, and control range of reaction temperature is 50-75 DEG C, when the temperature of reaction is higher than 75 DEG C, reduces atomized water
Flow velocity when reaction temperature is lower than 50 DEG C, increases the flow velocity of atomized water, and the flow rates of atomized water are 30-80mL/s, reaction humidity
For 20-90%, the hydrogen that reaction generates persistently is removed with the exhaust valve for the treatment of box in reaction, after reaction (i.e. reaction is basic stops,
When temperature tends towards stability) it obtains containing lithium mixture；
Wherein, the size droplet diameter of the atomized water is about 1.5mm.The exhaust valve for the treatment of box is equipped with filter device, and reaction produces
Raw lithium-containing compound flue gas is discharged after filtering and safe processing.A part can be discharged by exhaust valve in reaction heat, can also
It is cooling by the cooling system being arranged on treatment box.
(2) under argon atmosphere, lithium mixture will be contained described in step (1) in step (1) the enclosed workshop case and immersed
(solid-to-liquid ratio when starting reaction is 25g:1L) is reacted in water, the hydrogen that reaction generates persistently is removed in reaction, and to water
In be passed through carbon dioxide, to (lithium metal is totally consumed) after reaction, obtain lithium-containing solution.
The safety results of the present embodiment are shown in Table 1.
Embodiment 4
In addition in step (1), control range of reaction temperature is except 20-85 DEG C the present embodiment, other operating conditions and anti-
Answer species etc. same as Example 1.
The safety results of the present embodiment are shown in Table 1.
Embodiment 5
The present embodiment other than the size droplet diameter of the atomized water in step (1) reaches 3mm, other operating conditions and
Reactant species etc. are same as Example 1.
The safety results of the present embodiment are shown in Table 1.
Comparative example 1
This comparative example is other than control range of reaction temperature is 70-110 DEG C in the step (1), other operating conditions and anti-
Answer species etc. same as Example 1.
The safety results of this comparative example are shown in Table 1.
Comparative example 2
This comparative example is in addition to the operation without step (1), outside operation that step (2) are directly carried out with lithium metal, other
Operating condition and reactant species etc. are same as Example 1.
The safety results of this comparative example and the rate of recovery structure of lithium metal are shown in Table 1.
Test method
Whether according to temperature controlled complexity and having makes the hydrogen generation danger of reaction generation determine its peace
Quan Xing.
According to the time needed for processing 500g lithium metal, to evaluate the efficiency of processing lithium metal.
Test result see the table below:
Table 1
Based on the above embodiments with comparative example it is found that embodiment 1-3 controls reaction by controlling the additional amount of atomized water
The lithium hydroxide that process, atomized water and lithium metal generate is covered on metallic lithium surface, slows down reaction process, reaches in atomized water
After reaction balance, water is added containing lithium mixture for lithium hydroxide to not reacting completely, the lithium hydroxide for being wrapped in lithium metal is molten
Solution forms lithium hydroxide aqueous solution in water, and lithium metal continues to react with water in lithium hydroxide aqueous solution, and lithium hydroxide is water-soluble
Liquid reduces the reaction rate of lithium metal and water, controls reaction process, and embodiment 1-3 is by multi-step substep control reaction
Process, control the severity of reaction to improve safety；Xiang Shuizhong is passed through carbon dioxide and forms the lithium carbonate for being slightly soluble in water,
This step is both that the concentration of the aqueous solution of control lithium hydroxide is also created as with controlling the reaction rate of lithium metal and water
The lithium carbonate for being slightly soluble in water is formed, avoids lithium hydroxide excessive concentration that lithium metal is made to react excessively slow with water, results in the need for
Frequent processing or adjustment lithium hydroxide aqueous solution concentration, can also obtain the lithium carbonate of easy safe retrieving.
The lower limit that 4 step of embodiment (1) controls temperature is too low, and reaction rate is caused to decrease, slightly affected processing effect
Rate increases processing cost.
The atomization water drop of 5 step of embodiment (1) is excessive, causes the reaction of lithium metal localized contact fierce, after the reaction of surface layer
The lithium hydroxide passivation layer of generation is dissolved, and is reacted lasting and is carried out, and is unfavorable for realizing that reaction is slowly controllable, for reaction unit
Processing heat treatment and hydrogen treat Capability Requirement further increase and just can guarantee safety.
The upper limit that 1 step of comparative example (1) controls temperature is excessively high, causes to be easy to produce security risk, the display reaction of temperature height
It is fierce to compare, weaker for reaction process control, a wide range of burning and risk of explosion easily occurs.
Lithium metal is directly added to the water by comparative example 2 to be hydrolyzed, although the treatment effect of lithium metal is high, reaction
Acutely, a large amount of heat and imflammable gas hydrogen can be generated, safety hazard is high, easily explodes.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (10)
1. a kind of method for innocent treatment of lithium metal, which is characterized in that the described method comprises the following steps:
(1) it is reacted, is obtained after reaction containing lithium mixture with lithium metal with the reactant of atomization；
(2) it will contain described in step (1) and be reacted in lithium mixture immersion reactant, and obtain lithium-containing solution.
2. the method according to claim 1, wherein the reactant of step (1) described atomization includes atomized water；
Preferably, the size droplet diameter of the reactant of step (1) described atomization is in 2mm or less；
Preferably, step (1) lithium metal is lithium metal waste material；
Preferably, the flow velocity of the reactant of step (1) described atomization is 10-100mL/s.
3. method according to claim 1 or 2, which is characterized in that temperature≤100 DEG C of step (1) described reaction, preferably
It is 40-85 DEG C；
Preferably, when the temperature of step (1) described reaction is higher than 85 DEG C, reduce the flow velocity of the reactant of atomization, step (1) is described
When the temperature of reaction is lower than 40 DEG C, increase the flow velocity of the reactant of atomization；
Preferably, the humidity of step (1) described reaction is 10-100%.
4. method according to claim 1-3, which is characterized in that step (2) described reactant includes water.
5. method according to claim 1-4, which is characterized in that step (1) and step (2) are in treatment box
It carries out；
Preferably, the treatment box includes cooling system；
Preferably, step (1) described lithium metal is placed in the hollow out storage facility in treatment box.
6. according to the method described in claim 5, it is characterized in that, the treatment box is enclosed workshop case；
Preferably, it is lasting in step (1) and step (2) to remove what reaction generated when the treatment box is enclosed workshop case
Hydrogen；
Preferably, when the treatment box is enclosed workshop case, the treatment box includes exhaust valve；
Preferably, the exhaust valve is equipped with filter device；
Preferably, when the treatment box is enclosed workshop case, step (1) and step (2) carry out under an inert atmosphere；
Preferably, the inert atmosphere includes any one in helium atmosphere, neon atmosphere or argon atmosphere or at least two
Combination.
7. according to the method described in claim 5, it is characterized in that, the treatment box is non-fully enclosed treatment box；
Preferably, when the treatment box is non-fully enclosed treatment box, step (1) and step (2) carry out under an oxygen-containing atmosphere；
Preferably, the oxygen-containing atmosphere includes oxygen and/or air；
Preferably, the hydrogen that step (1) and step (2) generate reaction burns in treatment box.
8. method according to claim 1-7, which is characterized in that the method also includes: to described in step (2)
It is passed through carbon containing reaction gas in the reaction solution reacted, obtains product containing lithium.
9. preparation method according to claim 8, which is characterized in that the carbon containing reaction gas includes carbon dioxide；
Preferably, the product containing lithium is lithium carbonate.
10. -9 described in any item methods according to claim 1, which is characterized in that the described method comprises the following steps:
(1) it in enclosed workshop case, under inert atmosphere, is reacted with atomized water with lithium metal, the flow velocity of the atomized water
For 10-100mL/s, reaction humidity 10-100%, reaction temperature is 40-85 DEG C, when the temperature of reaction is higher than 85 DEG C, reduces mist
Change the flow velocity of water, when reaction temperature is lower than 40 DEG C, increases the flow velocity of atomized water, the hydrogen that reaction generates persistently is removed in reaction,
It is obtained after reaction containing lithium mixture；
Wherein, the size droplet diameter of the atomized water is in 2mm or less；
(2) it under inert atmosphere, will be immersed in the water described in step (1) containing lithium mixture in step (1) the enclosed workshop case
It is reacted, the hydrogen that reaction generates persistently is removed in reaction, and Xiang Shuizhong is passed through carbon dioxide, obtains lithium carbonate containing solution；
Or
(1) it in non-fully enclosed treatment box, under oxygen-containing atmosphere, is reacted with atomized water with lithium metal, the atomized water
Flow velocity is 10-100mL/s, and reaction humidity 10-100%, reaction temperature is 40-85 DEG C, when the temperature of reaction is higher than 85 DEG C, is subtracted
The flow velocity of small atomized water increases the flow velocity of atomized water when reaction temperature is lower than 40 DEG C, is obtained after reaction containing lithium mixture, reaction
In burn in treatment box to the hydrogen of generation；
Wherein, the size droplet diameter of the atomized water is in 2mm or less；
(2) under oxygen-containing atmosphere, lithium mixture will be contained described in step (1) in step (1) the non-fully enclosed treatment box and immersed
It is reacted in water, burns, and Xiang Shuizhong is passed through carbon dioxide, contained in treatment box to the hydrogen of generation in reaction
Lithium carbonate solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910786382.8A CN110436489A (en) | 2019-08-23 | 2019-08-23 | A kind of method for innocent treatment of lithium metal |
Applications Claiming Priority (1)
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| CN111847486A (en) * | 2020-07-08 | 2020-10-30 | 四川大学 | Method for preparing battery-grade lithium carbonate from metal lithium slag |
| CN112267026A (en) * | 2020-10-13 | 2021-01-26 | 湖南金凯循环科技有限公司 | Method for preparing lithium hydroxide by taking waste lithium metal as raw material |
| CN115725841A (en) * | 2021-08-25 | 2023-03-03 | 宁德时代新能源科技股份有限公司 | Lithium removal method without hydrogen generation |
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