CN104925837B - 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 PDF

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CN104925837B
CN104925837B CN201510374978.9A CN201510374978A CN104925837B CN 104925837 B CN104925837 B CN 104925837B CN 201510374978 A CN201510374978 A CN 201510374978A CN 104925837 B CN104925837 B CN 104925837B
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lithium
solution
step
slurry
ph
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CN201510374978.9A
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CN104925837A (en
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李良彬
章小明
付晓春
许鑫
符龙
陈玲
廖萃
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江西赣锋锂业股份有限公司
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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

It is a kind of to reclaim the method that battery-level lithium carbonate sinker mother solution prepares lithium salts

Technical field

The present invention relates to the method for reclaiming sinker mother solution, and in particular to a kind of recovery waste material containing lithium fluoride prepares the side of lithium salts Method.

Background technology

Lithium carbonate is the basic material of lithium salts industry, has various industrial uses, not only can directly use, be also used as Raw material prepares the high lithium salts of various added values and its compound.Be widely used in battery industry, ceramics, glass industry, aluminum i ndustry, The emerging application such as lubricant, cold-producing medium, nuclear industry and photovoltaic industry.

Battery-level lithium carbonate is mainly for the production of cobalt acid lithium, LiFePO4, lithium nickelate, LiMn2O4, ternary material, nickel cobalt manganese The positive electrode of the lithium ion batteries such as sour lithium.The preparation method of battery-level lithium carbonate is typically with Li2SO4Or LiCl is raw material, is adopted Soda sinker or deep carbon dioxide carbonization sinker, after sinker, Li+With Li2CO3Precipitate, but in solution, still suffer from a small amount of Li+, its Li+About 2g/L, the solution are referred to as sinker mother solution.The technique productions lithium carbonate, technique liquid amount balance are to solve the lithium response rate Key issue.Liquid measure is uneven, and lithium-containing solution is just lost in a lot, causes lithium resource to be lost in, the route of the reason circulation of the water containing lithium Longer, the loss of lithium is also bigger.So the technique solves the problems, such as that sinker disposing mother liquor is the key of Technology.

Earliest method is that sinker mother solution first adds sulphuric acid to neutralize, and then re-evaporation concentrating and separating goes out sodium sulfate, and mother solution is returned Leaching lithium system.This is also the method that current most enterprises process sinker mother solution.

Method after improvement is that sinker mother solution is first freezed, and is then peeled off sal glauberi, then concentration is evaporated to mother solution Lithium carbonate is isolated, mother solution is freezed again, such self-loopa.

The processing method of sinker mother solution that minority producer adopts is:First cooling separates out sodium sulfate, and mother solution is being divided into two parts Walk, major part participates in purification leachate and then in evaporation and concentration in being added to leachate, remainder to ore deposit soaks lithium system.This place Reason mode steam consumption quantity is equally very big, and return to ore deposit leaching lithium system partially due to circulation route and increase the loss of lithium.

Patent of invention (ZL201110122564.9) discloses a kind of processing method of battery-level lithium carbonate sinker mother solution, adopts With the acidifying of sinker mother solution, evaporation and concentration and analyse the steps such as sodium, sinker, circulation and reclaim battery-level lithium carbonate mother solution preparation LITHIUM BATTERY carbon Sour lithium, the technique evaporation capacity are big, and evaporation energy consumption is high, and the sinker response rate is not high.

Patent of invention (ZL 201110190405.2) discloses a kind of using pure Lithium Carbonate sinker mother solution preparation LITHIUM BATTERY The method of lithium dihydrogen phosphate, the patent utilization phosphoric acid and phosphate are tentatively carried lithium to lithium carbonate sinker mother solution and depth is carried Lithium, obtains two lithium mixture of lithium phosphate and phosphoric acid hydrogen, recycles the mixture to generate lithium dihydrogen phosphate solution with phosphatase reaction, then Through concentration and evaporation, crystallisation by cooling, centrifugation, saturation washing, drying, comminution by gas stream and packaging, LITHIUM BATTERY di(2-ethylhexyl)phosphate is obtained Hydrogen lithium.The Technology is complicated, and lithium comprehensive recovery is not high, and processing cost is also higher.

The content of the invention

The present invention proposes a kind of method that recovery waste material containing lithium fluoride prepares lithium salts, and the method is high to the response rate of lithium, right It is low in the pollution of the environment, compensate for weak point of the prior art.

The technical scheme is that what is be achieved in that:

It is a kind of to reclaim the method that battery-level lithium carbonate sinker mother solution prepares lithium salts, comprise the following steps:

A, sinker:Sinker mother solution is warming up to into 80~95 DEG C, H is added toward solution3PO3It is 6 that solution adjusts the pH value of solution ~8,10~30min is stirred, the pH for being subsequently adding NaOH solution regulation solution is 10~12, is stirred for 10~30min, filters To lithium phosphate and filtrate;

B, dispensing:Add pure water or washing liquid to be made into slurry in the lithium phosphate obtained toward step A, control solid-liquid weight percent Than for 30%~40%, and stir;

C, acidifying:Mineral acid is added in the slurry prepared toward step B, the pH for adjusting slurry is 0~4;

D, transition:By Li in slurry in the slurry obtained toward step C3PO3Quality excessive 0~10% adds the dense of amount of calculation Spend the calcium salt soln for 300~400g/L, 30~60min of stirring reaction, by Li3PO3It is transformed into lithium salts;

E, tune pH:NaOH solution is added in the lithium salt solution obtained toward step D, the pH for adjusting solution is 8~10, and is stood 30~60min of ageing;

F, solid-liquid separation:The solution that step E is obtained is filtered, and obtains calcium phosphate slag and lithium salt solution, calcium phosphate slag is added Water washing 2~4 times, washing liquid return to step B dispensing.

The method that a kind of recovery battery-level lithium carbonate sinker mother solution of the present invention prepares lithium salts, can also be:

Further, the mineral acid for adding in step C is HCl and HNO3In one kind.Its advantage is this several acid For inorganic acid, consumption is few, and pH responses are sensitive.

Further, the concentration of the HCl is 25%~31%, the HNO3Concentration be 40%~60%.Its advantage It is that the concentration range is the conventional industrial acid concentration of both acid, can be directly added into without allotment.

Further, the calcium salt that step D is added is CaCl2With Ca (NO3)2In one kind.Its advantage is this several salt Transition effect it is good, improve the lithium response rate.

Further, the concentration of the NaOH solution is 15~32%, the H3PO3The concentration of solution is 60%~85%. Its advantage is that the concentration range is the conventional industrial acid concentration of both acid, can be directly added into without allotment.

The chemical equation of step A is as follows:

2Li2CO3+2H3PO4→2Li2HPO4+2H2O+2CO2

2Li2HPO4+Li2CO3+2NaOH→2Li3PO4+2H2O+Na2CO3

3Li2CO3+2H3PO4+2NaOH→2Li3PO4+4H2O+2CO2

The chemical equation of step C is as follows:

Li3PO4+2HCl→LiH2PO4+2LiCl

Li3PO4+2HNO3→LiH2PO4+2LiNO3

The reaction equation of step D is as follows:

2LiH2PO4(l)+CaCl2(l)→2LiCl(l)+Ca(H2PO4)2

2LiH2PO4(l)+Ca(O3)(l)→2LiNO3(l)+Ca(H2PO4)2

The reaction equation of step E is as follows:

3Ca(H2PO4)2(l)+12NaOH(l)→Ca3(PO4)2(s)+4Na3PO4(s)+12H2O

F, solid-liquid separation;

Solution in step E is filtered, lithium chloride and calcium phosphate slag is obtained.

G, wash heat are washed

The step D transformation process, adds the computational methods of the calcium salt of amount of calculation as follows:

The volume of hypothesis battery-level lithium carbonate sinker mother solution is V L, the Li in solution+Molar concentration be CLi+Mol/L, The excess coefficient for adding calcium salt is a, and the molar concentration of the calcium salt soln of addition is C mol/L, then the calcium salt of the amount of calculation for adding Volume VCaFor:

VCa=(V × CLi+)/(3(1+a)CCa)

Beneficial effects of the present invention are:By the method for the present invention, i.e., by the heavy reason of phosphoric acid, acidifying transition, solid-liquid separation Etc. step, solve the problems, such as that freezing in prior art, evaporation and concentration power consumption are big, reduce cost, mother liquid disposal amount is big, and phosphorus Hydrochlorate sinker completely, recycle, and defines the circulation of closing by sinker mother solution and washing liquid, can so greatly improve returning for lithium Yield.

Description of the drawings

Fig. 1 is the process chart of the method that recovery battery-level lithium carbonate sinker mother solution of the present invention prepares lithium salts.

Specific embodiment

Technical scheme is clearly and completely described below by embodiment, it is clear that described enforcement Example is only a part of embodiment of the invention, rather than the embodiment of whole.Based on the embodiment in the present invention, this area is common The every other embodiment obtained under the premise of creative work is not made by technical staff, belongs to the model of present invention protection Enclose.

Embodiment 1:

A sinkers:Take 4000L sinker mother solutions to add to reactor, heat up 80 DEG C, toward solution, add concentration to be 60% H3PO3The pH value for adjusting solution is 6, stirs 10min, and the pH for being subsequently adding 15% NaOH solution regulation solution is 10, is stirred for 10min, is filtrated to get 53kg lithium phosphates wet feed and 3900L filtrates;

B dispensings:Add 150L pure water to be made into slurry in the lithium phosphate obtained toward step A, and stir;

C, acidifying:The HCl that concentration is 25% is added in the slurry prepared toward step B, the pH for adjusting slurry is 0;

D, transition:It is 300g/L according to 222L concentration is added in the slurry that calcium ion excess coefficient 1.05 is obtained toward step C CaCl2Solution, stirring reaction 30min obtain 350L slurries;

E, tune pH:In the lithium salt solution obtained toward step D add concentration be 15% NaOH solution, adjust solution pH be 8, and still aging 30min;

F, solid-liquid separation:The solution that step E is obtained is filtered, and obtains 65kg calcium phosphate wet slag and 340L LiCl solution, will Calcium phosphate slag adds water and washs 2 times, washing liquid return to step B dispensing.

Embodiment 2:

A sinkers:Take 6000L sinker mother solutions to add to reactor, heat up 95 DEG C, toward solution, add concentration to be 85% H3PO4The pH value for adjusting solution is 8, stirs 30min, and the pH for being subsequently adding the NaOH solution regulation solution that concentration is 30% is 12, 30min is stirred for, 80.2kg lithium phosphates and 5650L filtrates is filtrated to get;

B dispensings:Add 160L washing liquids to be made into slurry in the lithium phosphate obtained toward step A, and stir;

C, acidifying:The HCl that concentration is 31% is added in the slurry prepared toward step B, the pH for adjusting slurry is 4;

D, transition:It is to add in 1.08 slurries obtained toward step C 259L concentration to be 400g/L by calcium ion excess coefficient CaCl2Solution, stirring reaction 60min obtain about 450L slurries;

E, tune pH:In the lithium salt solution obtained toward step D add concentration be 30% NaOH solution, adjust solution pH be 12, and still aging 30min;

F, solid-liquid separation:The solution that step E is obtained is filtered, and obtains 95kg calcium phosphate wet slag and 470L LiCl solution, will Calcium phosphate slag adds water and washs 4 times, washing liquid return to step B dispensing.

Embodiment 3:

A sinkers:Take 8000L sinker mother solutions to add to reactor, heat up 87 DEG C, toward solution, add concentration to be 75% H3PO3It is 7 that solution adjusts pH value, stirs 20min, and the pH for being subsequently adding the NaOH solution regulation solution that concentration is 22% is 11, then Stirring 20min, is filtrated to get 121kg lithium phosphates and 8100L filtrates;

B dispensings:Add 280L pure water to be made into slurry in the lithium phosphate obtained toward step A, and stir;

C, acidifying:The HCl that concentration is 30% is added in the slurry prepared toward step B, the pH for adjusting slurry is 2;

D, transition:It is to add in 1.08 slurries obtained toward step C 400L concentration to be 350g/L by calcium ion excess coefficient CaCl2Solution, stirring reaction 45min obtain 720L LiCl solution;

E, tune pH:In the lithium salt solution obtained toward step D add concentration be 22% NaOH solution, adjust solution pH be 11, and still aging 45min;

F, solid-liquid separation:The solution that step E is obtained is filtered, and obtains 139kg calcium phosphate slag and 670L LiCl solution, will Calcium phosphate slag adds water and washs 3 times, washing liquid return to step B dispensing.

Embodiment 4:

A sinkers:Take 4000L sinker mother solutions to add to reactor, heat up 80 DEG C, 60% H is added toward solution3PO3Adjust The pH value of solution is 6, stirs 10min, and the pH for being subsequently adding 15% NaOH solution regulation solution is 10, is stirred for 10min, mistake Filter obtains 55kg lithium phosphates and 4100L filtrates;

B dispensings:Add 170L pure water to be made into slurry in the lithium phosphate obtained toward step A, and stir;

C, acidifying:The HNO that concentration is 60% is added in the slurry prepared toward step B3, the pH for adjusting slurry is 0;

D, transition:It is to add in 1.05 slurries obtained toward step C 368L concentration to be 300g/ according to calcium ion excess coefficient Ca (the NO of L3)2Solution, stirring reaction 30min obtain 400L slurries;

E, tune pH:In the lithium salt solution obtained toward step D add concentration be 15% NaOH solution, adjust solution pH be 8, and still aging 30min;

F, solid-liquid separation:The solution that step E is obtained is filtered, and obtains 59kg calcium phosphate slag and 350L LiNO3Solution, will Calcium phosphate slag adds water and washs 2 times, washing liquid return to step B dispensing.

Embodiment 5:

A sinkers:Take 6000L sinker mother solutions to add to reactor, heat up 95 DEG C, toward solution, add concentration to be 85% H3PO3The pH value for adjusting solution is 8, stirs 30min, and the pH for being subsequently adding 30% NaOH solution regulation solution is 12, is stirred for 30min, is filtrated to get 83kg lithium phosphates wet feed and 6100L filtrates;

B dispensings:Add 210L washing liquids to be made into slurry in the lithium phosphate obtained toward step A, and stir;

C, acidifying:The HNO that concentration is 60% is added in the slurry prepared toward step B3, the pH for adjusting slurry is 4;

D, transition:It is 400g/L's according to 434L concentration is added in the slurry that calcium ion excess coefficient 1.1 is obtained toward step C Ca(NO3)2Solution, stirring reaction 60min obtain 650L slips;

E, tune pH:In the lithium salt solution obtained toward step D add concentration be 30% NaOH solution, adjust solution pH be 12, and still aging 30min;

F, solid-liquid separation:The solution that step E is obtained is filtered, and obtains 89kg calcium phosphate slag and 550L LiNO3Solution, will Calcium phosphate slag adds water and washs 4 times, washing liquid return to step B dispensing.

This sinker mother solution Li used by serial case row:1.76g/l, the quality feelings of the lithium salt solution that above-mentioned five embodiments are obtained Condition is as shown in table 1:

Table 1

Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention Within god and principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.

Claims (5)

1. it is a kind of to reclaim the method that battery-level lithium carbonate sinker mother solution prepares lithium salts, it is characterised in that to comprise the following steps:
A, sinker:Sinker mother solution is warming up to into 80~95 DEG C, H is added toward solution3PO3It is 6~8 that solution adjusts the pH value of solution, 10~30min of stirring, the pH for being subsequently adding NaOH solution regulation solution is 10~12, is stirred for 10~30min, is filtrated to get phosphorus Sour lithium and filtrate;
B, dispensing:Pure water or washing liquid is added to be made into slurry in the lithium phosphate obtained toward step A, controlling solid-liquid percentage by weight is 30%~40%, and stir;
C, acidifying:Mineral acid is added in the slurry prepared toward step B, the pH for adjusting slurry is 0~4;
D, transition:By Li in slurry in the slurry obtained toward step C3PO3Quality excessive 0~10% adds the concentration of amount of calculation to be The calcium salt soln of 300~400g/L, 30~60min of stirring reaction, by Li3PO3It is transformed into lithium salts;
E, tune pH:NaOH solution is added in the lithium salt solution obtained toward step D, the pH for adjusting solution is 8~10, and still aging 30~60min;
F, solid-liquid separation:The solution that step E is obtained is filtered, and is obtained calcium phosphate slag and lithium salt solution, calcium phosphate slag is added water and is washed Wash 2~4 times, washing liquid return to step B dispensing.
It is 2. according to claim 1 to reclaim the method that battery-level lithium carbonate sinker mother solution prepares lithium salts, it is characterised in that:Institute The mineral acid added in stating step C is HCl and HNO3In one kind.
It is 3. according to claim 2 to reclaim the method that battery-level lithium carbonate sinker mother solution prepares lithium salts, it is characterised in that:Institute The concentration for stating HCl is 25%~31%, the HNO3Concentration be 40%~60%.
It is 4. according to claim 1 to reclaim the method that battery-level lithium carbonate sinker mother solution prepares lithium salts, it is characterised in that:Institute The calcium salt for stating the addition of step D is CaCl2With Ca (NO3)2In one kind.
It is 5. according to claim 1 to reclaim the method that battery-level lithium carbonate sinker mother solution prepares lithium salts, it is characterised in that:Institute The concentration for stating NaOH solution is 15~32%, the H3PO3The concentration of solution is 60%~85%.
CN201510374978.9A 2015-03-18 2015-07-01 Method of preparing lithium salt by recovering lithium deposition mother liquor of battery grade lithium carbonate CN104925837B (en)

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WO2017213272A1 (en) * 2016-06-07 2017-12-14 재단법인 포항산업과학연구원 Method for manufacturing metal lithium
CN106395863A (en) * 2016-08-30 2017-02-15 山东瑞福锂业有限公司 Method for preparing battery-grade lithium salt through recovering lithium bromide waste liquor
KR101918234B1 (en) * 2016-09-05 2018-11-13 주식회사 포스코 Method for manufacturing lithium chloride and method for manufacturing lithium carbonate
CN108002410B (en) * 2016-10-31 2019-10-18 湖南金源新材料股份有限公司 Lithium is recycled from low content extraction tail water and extracts the circulation utilization method of tail water
CN106586995B (en) * 2016-12-23 2019-04-09 江西合纵锂业科技有限公司 A kind of method of efficient process lithium phosphate reclaimed materials
CN108928839A (en) * 2017-05-25 2018-12-04 自贡同发荣实业有限公司 The method of lithium phosphate production lithium chloride solution
CN108928840A (en) * 2017-05-25 2018-12-04 自贡同发荣实业有限公司 The method of lithium fluoride production lithium chloride solution
CN108550939B (en) * 2018-04-19 2019-10-22 江西理工大学 A method of selective recovery lithium and lithium carbonate is prepared from waste lithium cell
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

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CN102351160B (en) * 2011-05-06 2013-10-30 江西赣锋锂业股份有限公司 Method for preparing battery grade lithium dihydrogen phosphate with high-purity lithium carbonate lithium depositing mother solution
CN102897803B (en) * 2012-10-22 2014-04-16 四川天齐锂业股份有限公司 Method for recycling mother solution generated in lithium iron phosphate preparation based on liquid phase method
CN102891345B (en) * 2012-10-22 2014-07-16 四川天齐锂业股份有限公司 Method for recycling lithium chloride from waste lithium iron phosphate
CN103400983B (en) * 2013-07-29 2015-07-08 海门容汇通用锂业有限公司 Method for synthesizing nano lithium iron phosphate without water of crystallization through atmospheric water phase

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