CN104925837A - Method of preparing lithium salt by recovering lithium deposition mother liquor of battery grade lithium carbonate - Google Patents
Method of preparing lithium salt by recovering lithium deposition mother liquor of battery grade lithium carbonate Download PDFInfo
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Abstract
The invention relates to a method of preparing lithium salt by recovering lithium deposition mother liquor of battery grade lithium carbonate. The method includes the steps of A, performing lithium deposition, to be specific, adding phosphoric acid into the lithium deposition mother liquor of battery grade lithium carbonate to adjust pH to 6 to 8, adding NaOH to adjust pH to 10 to 12, and performing lithium deposition; B, preparing slurry, to be specific, adding water or washing liquor to lithium phosphate obtained in the step A to obtain slurry; C, performing acidifying, to be specific, adding HCl to the slurry prepared in the step B to allow acidifying; D, allowing transformation, to be specific, adding calcium salt to the acidified slurry obtained in the step C to allow transformation; E, adjusting pH, to be specific, adjusting the pH of transformed solution obtained in the step D, to 8 to 10, and allowing ageing for 30 to 60 min; and F, performing solid-liquid separation, to be specific, filtering the solution obtained in the step D to obtain high-pure lithium salt solution, washing filter residue, and returning the ingredients for cyclic use. The method has the advantages such that resources are comprehensively recycled, lithium recovery rate is high, energy consumption is low, and the process is simple; the method is suitable for industrial production.
Description
Technical field
The present invention relates to the method reclaiming sinker mother liquor, be specifically related to a kind of method reclaiming fluorinated lithium waste material and prepare lithium salts.
Background technology
Quilonum Retard is the base mateiral of lithium salts industry, has multiple industrial use, not only can directly use, and can also prepare the high lithium salts of various added value and compound thereof as raw material.Be widely used in the emerging Application Areass such as battery industry, ceramics, glass industry, aluminum i ndustry, lubricant, refrigeration agent, nuclear industry and photovoltaic industry.
Battery-level lithium carbonate is mainly for the production of the positive electrode material of the lithium ion batteries such as cobalt acid lithium, iron lithium phosphate, lithium nickelate, lithium manganate, ternary material, nickle cobalt lithium manganate.The preparation method of battery-level lithium carbonate is generally with Li
2sO
4or LiCl is raw material, adopt soda ash sinker or deep carbon dioxide carbonization sinker, after sinker, Li
+with Li
2cO
3precipitate, but still there is a small amount of Li in solution
+, its Li
+be about 2g/L, this solution is called sinker mother liquor.This explained hereafter Quilonum Retard, technique liquid amount balance is the key issue solving the lithium rate of recovery.Liquid measure is uneven, and lithium-containing solution runs off just a lot, causes lithium resource to run off, and the route containing the water reason circulation of lithium is longer, and the loss of lithium is also larger.So this technique solves the key that sinker disposing mother liquor problem is Technology.
Method is the earliest that sinker mother liquor first adds sulfuric acid neutralization, and then evaporation concentration isolates sodium sulfate, and mother liquor returns leaching lithium system.This is also the method for current most enterprises process sinker mother liquor.
Method after improvement is that sinker mother liquor is first freezing, is then separated sal glauberi, then carries out evaporation concentration to mother liquor and isolate Quilonum Retard, and mother liquor carries out freezing again, self-circulation like this.
The treatment process of sinker mother liquor that minority producer adopts is: sodium sulfate is separated out in first cooling, and mother liquor is walked being divided into two portions, and major part is added in leach liquor and participates in purification leach liquor then in evaporation concentration, and remainder soaks lithium system to ore deposit.This processing mode steam consumption quantity is equally very large, and the part of getting back to ore deposit leaching lithium system makes the loss of lithium increase due to circulation route.
Patent of invention (ZL201110122564.9) discloses a kind for the treatment of process of battery-level lithium carbonate sinker mother liquor, adopt the acidifying of sinker mother liquor, evaporation concentration analyse the steps such as sodium, sinker, circulation and reclaim battery-level lithium carbonate mother liquor and prepare battery-level lithium carbonate, this technique steam output is large, evaporation energy consumption is high, and the sinker rate of recovery is not high.
Patent of invention (ZL 201110190405.2) discloses a kind of method utilizing pure Lithium Carbonate sinker mother liquor to prepare battery-grade lithium dihydrogen phosphate, this patent utilization phosphoric acid and phosphoric acid salt tentatively carry lithium to Quilonum Retard sinker mother liquor and the degree of depth carries lithium, obtain Trilithium phosphate and phosphoric acid hydrogen two lithium mixture, recycle this mixture and phosphatase reaction generates monometallic solution, again through concentration and evaporation, crystallisation by cooling, centrifugation, saturated washing, oven dry, comminution by gas stream and packaging, obtain battery-grade lithium dihydrogen phosphate.This Technology is complicated, and lithium comprehensive recovery is not high, and processing cost is also higher.
Summary of the invention
The present invention proposes a kind of method reclaiming fluorinated lithium waste material and prepare lithium salts, and the rate of recovery of the method to lithium is high, and environmental pollution is few, compensate for weak point of the prior art.
Technical scheme of the present invention is achieved in that
Reclaim the method that battery-level lithium carbonate sinker mother liquor prepares lithium salts, comprise the following steps:
A, sinker: sinker mother liquor is warming up to 80 ~ 95 DEG C, add H in solution
3pO
3the pH value of solution regulator solution is 6 ~ 8, and stir 10 ~ 30min, the pH then adding NaOH solution regulator solution is 10 ~ 12, then stirs 10 ~ 30min, filters and obtains Trilithium phosphate and filtrate;
B, batching: add pure water in the Trilithium phosphate obtained in steps A or washing lotion is made into slurry, controlling solid-liquid weight percent is 30% ~ 40%, and stirs;
C, acidifying: in the slurry that step B prepares, add mineral acid, the pH regulating slurry is 0 ~ 4;
D, transition: by Li in slurry in the slurry that step C obtains
3pO
3the concentration that quality excessive 0 ~ 10% adds calculated amount is the calcium salt soln of 300 ~ 400g/L, and stirring reaction 30 ~ 60min, by Li
3pO
3transition is lithium salts;
E, tune pH: in the lithium salt solution that step D obtains, add NaOH solution, the pH of regulator solution is 8 ~ 10, and still aging 30 ~ 60min;
F, solid-liquid separation: solution step e obtained filters, and obtains calcium phosphate slag and lithium salt solution, calcium phosphate slag is added water washing 2 ~ 4 times, washing lotion returns step B batching.
A kind of method reclaiming battery-level lithium carbonate sinker mother liquor and prepare lithium salts of the present invention, can also be:
Further, the mineral acid added in described step C is HCl and HNO
3in one.Its advantage is this several acid is inorganic acid, and consumption is few, and pH response is sensitive.
Further, the concentration of described HCl is 25% ~ 31%, described HNO
3concentration be 40% ~ 60%.Its advantage is, this concentration range is these two kinds sour conventional industrial acids concentration, can allocate and directly add.
Further, the calcium salt that described step D adds is CaCl
2with Ca (NO
3)
2in one.Its advantage is that the restructure result of this several salt is good, improves the lithium rate of recovery.
Further, the concentration of described NaOH solution is 15 ~ 32%, described H
3pO
3the concentration of solution is 60% ~ 85%.Its advantage is, this concentration range is these two kinds sour conventional industrial acids concentration, can allocate and directly add.
The chemical equation of described steps A is as follows:
2Li
2CO
3+2H
3PO
4→2Li
2HPO
4+2H
2O+2CO
2
2Li
2HPO
4+Li
2CO
3+2NaOH→2Li
3PO
4+2H
2O+Na
2CO
3
3Li
2CO
3+2H
3PO
4+2NaOH→2Li
3PO
4+4H
2O+2CO
2
The chemical equation of described step C is as follows:
Li
3PO
4+2HCl→LiH
2PO
4+2LiCl
Li
3PO
4+2HNO
3→LiH
2PO
4+2LiNO
3
The reaction equation of described step D is as follows:
2LiH
2PO
4(l)+CaCl
2(l)→2LiCl(l)+Ca(H
2PO
4)
2
2LiH
2PO
4(l)+Ca(O
3)(l)→2LiNO
3(l)+Ca(H
2PO
4)
2
The reaction equation of described step e is as follows:
3Ca(H
2PO
4)
2(l)+12NaOH(l)→Ca
3(PO
4)
2(s)+4Na
3PO
4(s)+12H
2O
F, solid-liquid separation;
Solution in step e is filtered, obtains lithium chloride and calcium phosphate slag.
G, wash heat are washed
Described step D transformation process, the method for calculation adding the calcium salt of calculated amount are as follows:
The volume supposing battery-level lithium carbonate sinker mother liquor is V L, the Li in solution
+volumetric molar concentration be C
li+mol/L, the excess coefficient adding calcium salt is a, and the volumetric molar concentration of the calcium salt soln added is C mol/L, then the volume V of the calcium salt of the calculated amount added
cafor:
V
Ca＝(V×C
Li+)/(3(1+a)C
Ca)
Beneficial effect of the present invention is: by method of the present invention, namely by steps such as the heavy reason of phosphoric acid, acidifying transition, solid-liquid separation, solve freezing in prior art, evaporation concentration to consume energy large problem, reduce cost, mother liquid disposal amount is large, and phosphoric acid salt sinker is complete, and sinker mother liquor and washing lotion are recycled, define closed circulation, the rate of recovery of lithium can be improved so greatly.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that recovery battery-level lithium carbonate sinker mother liquor of the present invention prepares the method for lithium salts.
Embodiment
Be clearly and completely described technical scheme of the present invention below by embodiment, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1:
A sinker: get 4000L sinker mother liquor and be added to reactor, heats up 80 DEG C, adds the H that concentration is 60% in solution
3pO
3the pH value of regulator solution is 6, and stir 10min, the pH then adding the NaOH solution regulator solution of 15% is 10, then stirs 10min, filters and obtains 53kg Trilithium phosphate wet feed and 3900L filtrate;
B prepares burden: add 150L pure water in the Trilithium phosphate obtained in steps A and be made into slurry, and stir;
C, acidifying: in the slurry that step B prepares, add the HCl that concentration is 25%, the pH regulating slurry is 0;
D, transition: in the slurry obtained toward step C according to calcium ion excess coefficient 1.05, add the CaCl that 222L concentration is 300g/L
2solution, stirring reaction 30min, obtains 350L slurry;
E, tune pH: in the lithium salt solution that step D obtains, add the NaOH solution that concentration is 15%, the pH of regulator solution is 8, and still aging 30min;
F, solid-liquid separation: solution step e obtained filters, and obtains 65kg calcium phosphate wet slag and 340L LiCl solution, calcium phosphate slag is added water washing 2 times, washing lotion returns step B batching.
Embodiment 2:
A sinker: get 6000L sinker mother liquor and be added to reactor, heats up 95 DEG C, adds the H that concentration is 85% in solution
3pO
4the pH value of regulator solution is 8, stirs 30min, and then to add concentration be the pH of the NaOH solution regulator solution of 30% is 12, then stirs 30min, filters and obtains 80.2kg Trilithium phosphate and 5650L filtrate;
B prepares burden: add 160L washing lotion in the Trilithium phosphate obtained in steps A and be made into slurry, and stir;
C, acidifying: in the slurry that step B prepares, add the HCl that concentration is 31%, the pH regulating slurry is 4;
D, transition: be add the CaCl that 259L concentration is 400g/L in 1.08 slurries obtained toward step C by calcium ion excess coefficient
2solution, stirring reaction 60min, obtains about 450L slurry;
E, tune pH: in the lithium salt solution that step D obtains, add the NaOH solution that concentration is 30%, the pH of regulator solution is 12, and still aging 30min;
F, solid-liquid separation: solution step e obtained filters, and obtains 95kg calcium phosphate wet slag and 470L LiCl solution, calcium phosphate slag is added water washing 4 times, washing lotion returns step B batching.
Embodiment 3:
A sinker: get 8000L sinker mother liquor and be added to reactor, heats up 87 DEG C, adds the H that concentration is 75% in solution
3pO
3solution adjust ph is 7, stirs 20min, and then to add concentration be the pH of the NaOH solution regulator solution of 22% is 11, then stirs 20min, filters and obtains 121kg Trilithium phosphate and 8100L filtrate;
B prepares burden: add 280L pure water in the Trilithium phosphate obtained in steps A and be made into slurry, and stir;
C, acidifying: in the slurry that step B prepares, add the HCl that concentration is 30%, the pH regulating slurry is 2;
D, transition: be add the CaCl that 400L concentration is 350g/L in 1.08 slurries obtained toward step C by calcium ion excess coefficient
2solution, stirring reaction 45min, obtains 720L LiCl solution;
E, tune pH: in the lithium salt solution that step D obtains, add the NaOH solution that concentration is 22%, the pH of regulator solution is 11, and still aging 45min;
F, solid-liquid separation: solution step e obtained filters, and obtains 139kg calcium phosphate slag and 670L LiCl solution, calcium phosphate slag is added water washing 3 times, washing lotion returns step B batching.
Embodiment 4:
A sinker: get 4000L sinker mother liquor and be added to reactor, heats up 80 DEG C, adds the H of 60% in solution
3pO
3the pH value of regulator solution is 6, and stir 10min, the pH then adding the NaOH solution regulator solution of 15% is 10, then stirs 10min, filters and obtains 55kg Trilithium phosphate and 4100L filtrate;
B prepares burden: add 170L pure water in the Trilithium phosphate obtained in steps A and be made into slurry, and stir;
C, acidifying: in the slurry that step B prepares, add the HNO that concentration is 60%
3, the pH regulating slurry is 0;
D, transition: be add the Ca (NO that 368L concentration is 300g/L in 1.05 slurries obtained toward step C according to calcium ion excess coefficient
3)
2solution, stirring reaction 30min, obtains 400L slurry;
E, tune pH: in the lithium salt solution that step D obtains, add the NaOH solution that concentration is 15%, the pH of regulator solution is 8, and still aging 30min;
F, solid-liquid separation: solution step e obtained filters, and obtains 59kg calcium phosphate slag and 350L LiNO
3solution, adds water washing 2 times by calcium phosphate slag, washing lotion returns step B batching.
Embodiment 5:
A sinker: get 6000L sinker mother liquor and be added to reactor, heats up 95 DEG C, adds the H that concentration is 85% in solution
3pO
3the pH value of regulator solution is 8, and stir 30min, the pH then adding the NaOH solution regulator solution of 30% is 12, then stirs 30min, filters and obtains 83kg Trilithium phosphate wet feed and 6100L filtrate;
B prepares burden: add 210L washing lotion in the Trilithium phosphate obtained in steps A and be made into slurry, and stir;
C, acidifying: in the slurry that step B prepares, add the HNO that concentration is 60%
3, the pH regulating slurry is 4;
D, transition: in the slurry obtained toward step C according to calcium ion excess coefficient 1.1, add the Ca (NO that 434L concentration is 400g/L
3)
2solution, stirring reaction 60min, obtains 650L slip;
E, tune pH: in the lithium salt solution that step D obtains, add the NaOH solution that concentration is 30%, the pH of regulator solution is 12, and still aging 30min;
F, solid-liquid separation: solution step e obtained filters, and obtains 89kg calcium phosphate slag and 550L LiNO
3solution, adds water washing 4 times by calcium phosphate slag, washing lotion returns step B batching.
This serial case arranges sinker mother liquor Li:1.76g/l used, and the quality condition of the lithium salt solution that above-mentioned five embodiments obtain is as shown in table 1:
Table 1
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. reclaim the method that battery-level lithium carbonate sinker mother liquor prepares lithium salts, it is characterized in that, comprise the following steps:
A, sinker: sinker mother liquor is warming up to 80 ~ 95 DEG C, add H in solution
3pO
3the pH value of solution regulator solution is 6 ~ 8, and stir 10 ~ 30min, the pH then adding NaOH solution regulator solution is 10 ~ 12, then stirs 10 ~ 30min, filters and obtains Trilithium phosphate and filtrate;
B, batching: add pure water in the Trilithium phosphate obtained in steps A or washing lotion is made into slurry, controlling solid-liquid weight percent is 30% ~ 40%, and stirs;
C, acidifying: in the slurry that step B prepares, add mineral acid, the pH regulating slurry is 0 ~ 4;
D, transition: by Li in slurry in the slurry that step C obtains
3pO
3the concentration that quality excessive 0 ~ 10% adds calculated amount is the calcium salt soln of 300 ~ 400g/L, and stirring reaction 30 ~ 60min, by Li
3pO
3transition is lithium salts;
E, tune pH: in the lithium salt solution that step D obtains, add NaOH solution, the pH of regulator solution is 8 ~ 10, and still aging 30 ~ 60min;
F, solid-liquid separation: solution step e obtained filters, and obtains calcium phosphate slag and lithium salt solution, calcium phosphate slag is added water washing 2 ~ 4 times, washing lotion returns step B batching.
2. recovery battery-level lithium carbonate sinker mother liquor according to claim 1 prepares the method for lithium salts, it is characterized in that: the mineral acid added in described step C is HCl and HNO
3in one.
3. recovery battery-level lithium carbonate sinker mother liquor according to claim 2 prepares the method for lithium salts, it is characterized in that: the concentration of described HCl is 25% ~ 31%, described HNO
3concentration be 40% ~ 60%.
4. recovery battery-level lithium carbonate sinker mother liquor according to claim 1 prepares the method for lithium salts, it is characterized in that: the calcium salt that described step D adds is CaCl
2with Ca (NO
3)
2in one.
5. recovery battery-level lithium carbonate sinker mother liquor according to claim 1 prepares the method for lithium salts, it is characterized in that: the concentration of described NaOH solution is 15 ~ 32%, described H
3pO
3the concentration of solution is 60% ~ 85%.
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| CN109264748B (en) * | 2018-09-29 | 2021-04-20 | 广东邦普循环科技有限公司 | Method for preparing lithium carbonate from crude lithium phosphate |
| CN109264748A (en) * | 2018-09-29 | 2019-01-25 | 广东邦普循环科技有限公司 | A method of lithium carbonate is prepared with crude lithium phosphate |
| CN110112463A (en) * | 2019-04-04 | 2019-08-09 | 李秀艳 | A kind of electrolysis additive, high-voltage electrolyte and battery containing the additive |
| CN111498872A (en) * | 2020-04-14 | 2020-08-07 | 赣州虔博新材料科技有限公司 | Lithium phosphate recycling process |
| CN111498872B (en) * | 2020-04-14 | 2022-12-13 | 赣州虔博新材料科技有限公司 | Lithium phosphate recycling process |
| CN113061749A (en) * | 2021-03-01 | 2021-07-02 | 湖南永杉锂业有限公司 | Method for recovering lithium from lithium salt solution and reaction system thereof |
| CN114853037A (en) * | 2022-06-02 | 2022-08-05 | 紫金矿业集团股份有限公司 | Method for recovering lithium from lithium precipitation mother liquor |
| CN114906828A (en) * | 2022-06-28 | 2022-08-16 | 四川思特瑞锂业有限公司 | Method for treating lithium dihydrogen phosphate mother liquor |
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