CN106629787A - Preparation method of cell-grade lithium hydroxide - Google Patents
Preparation method of cell-grade lithium hydroxide Download PDFInfo
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- CN106629787A CN106629787A CN201611187272.2A CN201611187272A CN106629787A CN 106629787 A CN106629787 A CN 106629787A CN 201611187272 A CN201611187272 A CN 201611187272A CN 106629787 A CN106629787 A CN 106629787A
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- lithium hydrate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/02—Oxides; Hydroxides
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Abstract
The invention belongs to the field of materials, and particularly relates to a preparation method of cell-grade lithium hydroxide. The preparation method of cell-grade lithium hydroxide has the advantages of being high in product purity, few in production process, low in production energy consumption and the like. The preparation method comprises the following steps that 1, a pre-prepared mixed solution is prepared, wherein a lithium sulfate solution and a sodium hydroxide solution are mixed according to the mole ratio 2:(1-1.2) of lithium sulfate to sodium hydroxide; 2, the pre-prepared mixed solution is frozen, wherein the pre-prepared mixed solution is frozen and crystallized for 1-2 h at the temperature of minus 15 DEG C to minus 10 DEG C, and solid-liquid separation is conducted to obtain sodium sulfafe decahydrate crystals and lithium hydroxide freezing liquid; 3, the lithium hydroxide freezing liquid obtained in the step 2 is subjected to evaporation concentration and solid-liquid separation to obtain a crude lithium hydroxide product; 4, the crude lithium hydroxide product obtained in the step 3 is redissolved to remove impurities and then subjected to evaporation concentration and solid-liquid separation to obtain lithium hydroxide with the coarse grain cell grade quality. The product is high in purity, few in impurity, coarse in grain and good in appearance, and the operation method is simple, few in production process, low in cost and low in energy consumption.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of preparation method of LITHIUM BATTERY Lithium hydrate.
Background technology
Through the development of more than ten years, the overall technological process of existing country's ore deposit method production Lithium hydrate is:Front operation is from Ore
In carry lithium using sulfuric acid process, rear operation produces Lithium hydrate for separation.At present, both at home and abroad Lithium hydrate produced by spodumene
Method mainly have a two methods of sulfuric acid process and lime method (i.e. front operation), various countries various places according to the condition of oneself select wherein it
One.It is a kind of that foreign countries only retain sulfuric acid process from after the seventies, substantially.China's limestone-based process yield and product quality aspect are all
Into world's rank of advanced units.Thus, still there are several limestone-based process production lines.The country starts lithium salts factory and builds high after the nineties
Tide, each newly to found the factory using Production By Sulfuric Acid Process technique, the production line of limestone-based process is progressively eliminated.Sulfuric acid process is given birth to limestone-based process
Production. art is compared, and it has energy consumption low (only the 1/3 of limestone-based process), and (foreign countries reach as high as 90-91% to high income, and the country reaches
83-86%), the advantages of utilization rate of equipment and installations is high, the quantity of slag few (for the 1/4 of limestone-based process), and not tight to grade of ore requirement,
Thus at home and abroad more and more paid attention to.
At present, sulfuric acid process prepare Lithium hydrate main technique it is as follows:
(1) by lithium brightness ore deposit is fired, acidifying, slurrying, the lithium sulfate solution of leaching and initial concentration;
(2) sodium hydroxide is added in lithium sulfate solution, sodium sulfate and lithium hydroxide solution mixture is obtained;
(3) by sodium sulfate and the cooling freezing of Lithium hydrate mixed solution, solution temperature drops to 5~-10 DEG C, it is crystallized after
Isolate sodium sulfate;
(4) clear liquid come by freeze and separate, heating, evaporation and concentration;
(5) crystallization and centrifugation, obtain Lithium hydrate crude product;
(6) barium hydroxide is added in crude product Lithium hydroxide monohydrate lysate, insoluble barium sulfate is formed, it is heavy to be filtered to remove
Starch and debris, filter liquor Jing evaporation and concentration, crystallization, separation, obtain wet Lithium hydroxide monohydrate:
(7) dry Lithium hydroxide monohydrate.
But time-consuming for preceding method, high energy consumption, the Lithium hydrate of LITHIUM BATTERY can be just obtained by multiple purification, the present invention
It is intended to provide a kind of preparation method of brand-new Lithium hydrate, reaching improving product quality, reducing production process and reducing production
The purpose of energy consumption.
The content of the invention
Technical problem solved by the invention is to provide a kind of preparation method of LITHIUM BATTERY Lithium hydrate, with product purity
High, production process is short, the low advantage of energy consumption.
The preparation method of LITHIUM BATTERY Lithium hydrate of the present invention, comprises the steps:
A, the prefabricated mixed liquor of preparation:By lithium sulfate solution and sodium hydroxide solution according to lithium sulfate and sodium hydroxide mole
Than for 2:1~1.2 mixing;
B, the prefabricated mixed liquor of freezing:The step A prefabricated mixed liquor of gained at a temperature of -15 DEG C~-10 DEG C freezing and crystallizing 1~
2h, solid-liquid separation obtains sal glauberi crystal and Lithium hydrate freezing liquid;
, through evaporation and concentration, solid-liquid separation obtains Lithium hydrate crude product for C, step B gained Lithium hydrate freezing liquid;
D, step C Lithium hydrate crude product dissolve remove impurity again, then evaporation and concentration, and solid-liquid separation obtains coarse grain LITHIUM BATTERY product
The Lithium hydrate of matter.
In above-mentioned technical proposal, the concentration of lithium sulfate solution described in step A is 25-27g/L;Sodium hydroxide described in step A
The concentration of solution be 45-55%, the concentration 50% (g/g) of preferred sodium hydroxide solution.
Lithium sulfate solution and sodium hydroxide solution according to lithium sulfate and sodium hydroxide mol ratio 2:1~1.2 mixing, i.e. table
In showing prefabricated mixed liquor, the mol ratio of lithium sulfate and sodium hydroxide is n (Li2SO4):N (NaOH)=2:1~1.2.
Evaporation and concentration described in step C and D adopts vapor recompression circulating evaporator, i.e. MVR vaporizers.It is a kind of weight
The energy of the new indirect steam produced using its own, so as to reduce the vaporizer of energy demand to external world.
The key point of preparation method of the present invention is:
(1) content of impurity element in Lithium hydrate crude product weight solvent soln is reduced so as to which Na, K plasma content is reduced
To within 3g/L;Specific control key has:
(a) by controlling freezing liquid in sulfate radical be, less than 35g/L, or even to can be controlled in less than 25g/L;By using temperature
The reason for freezing conditions of -15 DEG C~-10 DEG C of degree can be to reduce once to dissolve again, shorten the effect of production process.If cold
It is higher than -10 DEG C to freeze temperature, and the sulfate radical content directly resulted in the lithium hydroxide solution that freezing is obtained is too high, then only through once
Dissolving remove impurity again cannot obtain the monohydrate lithium hydroxide of LITHIUM BATTERY quality, if being less than -15 DEG C, for reduction lithium hydroxide solution
The effect of middle sulfate radical is not obvious, but energy consumption can be greatly increased.
When () step C evaporation and concentration Lithium hydrate freezing liquid obtains crude product b, freezing liquid cycles of concentration is controlled for 1.5-2.2
Times, preferred cycles of concentration is 1.8 times.
C () step C solid-liquid separation obtains Lithium hydrate crude product, per 300kg crude product 10-20L, temperature is at 65-75 DEG C
Distillation water wash 1-3 time;It is preferred that per 300kg crude product 15L, temperature 70 DEG C distillation water wash once.
(2) improve Lithium hydrate secondary crystallization condition, improve crystallization particle diameter;Specific control key has:
Li in (a) control Lithium hydrate freezing liquid2O content, need to control in 55-65g/L.
Temperature when () control Lithium hydrate crude product weight solvent soln enters vaporizer b should >=80 DEG C, it is therefore desirable to it is right
Solution storage tank carries out good isothermal holding and enters before vaporizer to be preheated.
(3) the reason for 40~50 DEG C of step D solid-liquid separation temperature control, selection said temperature scope can be to greatest extent
The monohydrate lithium hydroxide that makes separate out, while can also reduce impurity precipitation effect.Although if being easy to hydroxide less than 40 DEG C
Lithium is separated out, but continues to lower the temperature its changes in solubility less, less economical, and if above 50 DEG C Lithium hydrate dissolubility meeting can be caused
There is large change, reduce unit output, and other impurity can increase.Single water both can have to greatest extent been made at this temperature
Lithium hydrate is separated out, while impurity precipitation can also be reduced, so as to ensure that final Lithium hydrate index can disposably reach battery
Level is required.Specific control key has:
A the changes in solubility that 0 DEG C~40 DEG C of () monohydrate lithium hydroxide is only 0.3g/100g water, molten between 40 DEG C~100 DEG C
Xie Du changes turn to 4.5g/100g water, therefore from the point of view of changes in solubility, can select 40-50 DEG C for step D Lithium hydrate solid-liquid
Separation temperature.
B the rinsing step of () after the solid-liquid separation of step D, the Lithium hydrate obtained per 300kg step D solid-liquid separation is used
The distillation water wash at least 2 times of 10-15L, temperature at 50 DEG C.It is preferred that, the Lithium hydrate 15L that obtains per 300kg solid-liquid separation,
Distillation water wash of the temperature at 50 DEG C.
To sum up, the good LITHIUM BATTERY of the few coarse grain of purity height, impurity, looks is obtained using above-mentioned steps and state modulator
The Lithium hydrate of quality, operational approach has simple, reduction production process, low cost, less cost of power.
Specific embodiment
By the following examples the specific embodiment of form, remakes further specifically to the above of the present invention
It is bright, illustrate but do not limit the present invention.
Following examples prepare Lithium hydrate using following preparation method, comprise the steps:
A, the prefabricated mixed liquor of preparation:Lithium sulfate solution and sodium hydroxide solution are mixed;
B, the prefabricated mixed liquor of freezing:The prefabricated mixed liquor of step A gained freezing and crystallizing certain hour at a certain temperature, Gu
The isolated sal glauberi crystal of liquid and Lithium hydrate freezing liquid;
, through evaporation and concentration, solid-liquid separation obtains Lithium hydrate crude product for C, step B gained Lithium hydrate freezing liquid;
D, step C Lithium hydrate crude product dissolve remove impurity again, then evaporation and concentration, and solid-liquid separation obtains coarse grain LITHIUM BATTERY product
The Lithium hydrate of matter.
Wherein, each embodiment has investigated respectively the quality of product under the conditions of different parameters.
Investigate test 1:Cryogenic temperature and time
1st, group is investigated
Embodiment 1:Lithium sulfate and sodium hydroxide are according to mol ratio n (Li2SO4):N (NaOH) is 2:1, cryogenic temperature control
At -10 DEG C, cooling time is 1h.
Embodiment 2:Lithium sulfate and sodium hydroxide are according to mol ratio n (Li2SO4):N (NaOH) is 2:1, cryogenic temperature control
At -15 DEG C, cooling time is 2h.
Embodiment 3:The lithium sulfate of process conditions 3 and sodium hydroxide are according to mol ratio n (Li2SO4):N (NaOH) is 2:1, freezing
At -12 DEG C, cooling time is 1.5h to temperature control.
Comparative example 1:Lithium sulfate and sodium hydroxide are according to mol ratio n (Li2SO4):N (NaOH) is 2:1, cryogenic temperature control
At -6 DEG C, cooling time is 1h.
Embodiment 1-3, remaining of comparative example is consistent, and it is 1.8 times to be step C cycles of concentration, Lithium hydrate crude product
Per 300kg crude product 15L, temperature 70 DEG C distillation water wash once;Lithium hydrate crude product weight solvent soln enters evaporation
Temperature during device should >=80 DEG C;40~50 DEG C of step D solid-liquid separation temperature control, the hydrogen-oxygen obtained per 300kg solid-liquid separation
Change the distillation water wash of lithium finished product 10-15L, temperature at 50 DEG C, be dried, be repeated 2 times.
2nd, test method
1) according to embodiment 1-3, the lithium sulfate and sodium hydroxide ratio of comparative example 1 weigh sample, make prefabricated mixing
Liquid;
2) according to embodiment 1-3, the process conditions of comparative example 1 are freezed to prefabricated mixed liquor, are centrifugally separating to obtain solid
Body crystallizes sal glauberi and Lithium hydrate liquid;
3) solid-liquid separation after concentration and evaporation is carried out to lithium hydroxide solution, obtains crude product Lithium hydrate, drip washing is once;
4) crude product Lithium hydrate is once dissolved after remove impurity again, embodiment 1-3 is steamed using vapor recompression circulation
The system of sending out carries out concentration and evaporation, and then comparative example 1 obtains wet product Lithium hydrate using traditional triple effect evaporator after solid-liquid separation,
Lithium hydrate finished product is obtained final product after drying.
3rd, result of the test:It is shown in Table 1.
The product quality result of table 1
Freezing liquid sulfate radical content (g/L) | Quality of finished | Finished product grain size and looks | |
Embodiment 1 | 24.8g/L | LITHIUM BATTERY quality | Granule is thick, better crystallinity degree |
Embodiment 2 | 23.5g/L | LITHIUM BATTERY quality | Granule is thick, better crystallinity degree |
Embodiment 3 | 23.1g/L | LITHIUM BATTERY quality | Granule is thick, better crystallinity degree |
Comparative example 1 | 31.8g/L | Technical grade quality | Granule is thinner, degree of crystallinity skewness |
Conclusion (of pressure testing):Using traditional processing parameter control and equipment, once dissolved again to obtain comparative example 1
To the Lithium hydrate of LITHIUM BATTERY quality;And use the processing parameter control and special freezing of the present invention, concentrate condition, no
Only once can again dissolve the Lithium hydrate that can just produce LITHIUM BATTERY quality, and the looks crystal of Lithium hydrate product
Grain is thick, and better crystallinity degree significantly improves the quality of product, realizes and be once recrystallized to give LITHIUM BATTERY Lithium hydrate.
Investigate test 2:
1st, test method
1) embodiment 4-6 and comparative example 2 according to lithium sulfate and sodium hydroxide according to mol ratio n (Li2SO4):N (NaOH) is
2:1.2 ratios weigh sample, make prefabricated mixed liquor;
2) according to -10 DEG C of cryogenic temperature, cooling time is 1h freezings to the prefabricated mixed liquor of embodiment 4-6, is centrifugally separating to obtain
Solid crystal sal glauberi and Lithium hydrate liquid;Comparative example 2 is controlled at -6 DEG C according to cryogenic temperature, and cooling time is that 1h is cold
Freeze.
3) solid-liquid separation after concentration and evaporation is carried out to lithium hydroxide solution, obtains crude product Lithium hydrate, embodiment 4-6 crude product
Per 300kg crude product 15L, temperature 70 DEG C distillation water wash once, the not drip washing of comparative example 2;
4) crude product Lithium hydrate is once dissolved after remove impurity again, embodiment 4-6 is steamed using vapor recompression circulation
The system of sending out carries out concentration and evaporation, and using traditional triple effect evaporator, then after solid-liquid separation, secondary separation temperature is shown in Table comparative example 2
2, isolated wet product Lithium hydrate obtains final product Lithium hydrate finished product after drying.
Wherein, embodiment 4-6, remaining of comparative example 2 is consistent, is step C cycles of concentration for 1.8 times;Hydroxide
Lithium crude product weight solvent soln enter vaporizer when temperature should >=80 DEG C;The Lithium hydrate obtained per 300kg solid-liquid separation into
The distillation water wash of product 10-15L, temperature at 50 DEG C, is dried, and is repeated 2 times.
2nd, result of the test:It is shown in Table 2.
Table 2
Conclusion (of pressure testing):Understood by starting to improve freezing liquid from freezing process by table 2Control freezing liquid concentration times
Number is certain value, a drip washing and wet product centrifugation drip washing twice is centrifuged in addition crude product, while controlling the modes such as separation temperature
Afterwards, the ratio of the disposable output D3 product of Lithium hydrate (i.e. LITHIUM BATTERY Lithium hydrate) can significantly be lifted.
By long-felt, the present invention provides a kind of brand-new Lithium hydrate production technology, realizes only pass through one first
Secondary recrystallization just obtains high-quality, the LITHIUM BATTERY Lithium hydrate in coarse grain footpath.
Claims (8)
1. the preparation method of LITHIUM BATTERY Lithium hydrate, it is characterised in that:Comprise the steps:
A, the prefabricated mixed liquor of preparation:It is according to the mol ratio of lithium sulfate and sodium hydroxide by lithium sulfate solution and sodium hydroxide solution
2:1~1.2 mixing;
B, the prefabricated mixed liquor of freezing:The prefabricated mixed liquor 1~2h of freezing and crystallizing at a temperature of -15 DEG C~-10 DEG C of step A gained,
Solid-liquid separation obtains sal glauberi crystal and Lithium hydrate freezing liquid;
, through evaporation and concentration, solid-liquid separation obtains Lithium hydrate crude product for C, step B gained Lithium hydrate freezing liquid;
D, step C Lithium hydrate crude product dissolve remove impurity again, then evaporation and concentration, and solid-liquid separation obtains coarse grain LITHIUM BATTERY quality
Lithium hydrate.
2. the preparation method of LITHIUM BATTERY Lithium hydrate according to claim 1, it is characterised in that:Lithium sulfate described in step A
The concentration of solution is 25-27g/L;The concentration of sodium hydroxide solution described in step A is 45-55%;Further preferably, step A institute
The concentration for stating sodium hydroxide solution is 50%.
3. the preparation method of LITHIUM BATTERY Lithium hydrate according to claim 1, it is characterised in that:Steam described in step C and D
Send out concentration and adopt vapor recompression circulating evaporator.
4. the preparation method of LITHIUM BATTERY Lithium hydrate according to claim 1, it is characterised in that:Step C controls freezing liquid
Cycles of concentration is 1.5-2.2 times, and preferred steps C control freezing liquid cycles of concentration for 1.8 times.
5. the preparation method of LITHIUM BATTERY Lithium hydrate according to claim 1, it is characterised in that:Step C solid-liquid separation is obtained
To Lithium hydrate crude product, per 300kg crude product 10-20L, distillation water wash 1-3 time of the temperature at 65-75 DEG C;
Preferably, per 300kg crude product 15L, temperature 70 DEG C distillation water wash once.
6. the preparation method of LITHIUM BATTERY Lithium hydrate according to claim 1, it is characterised in that:Step D controls hydroxide
Lithium crude product weight solvent soln enters temperature >=80 DEG C during vaporizer.
7. the preparation method of LITHIUM BATTERY Lithium hydrate according to claim 1, it is characterised in that:Step D solid-liquid separation temperature
Degree control is at 40~50 DEG C.
8. the preparation method of LITHIUM BATTERY Lithium hydrate according to claim 1, it is characterised in that:The solid-liquid separation of step D
Rinsing step afterwards, distillation of Lithium hydrate wet product 10-15L, temperature obtained per 300kg step D solid-liquid separation at 50 DEG C
Water wash at least 2 times;
Preferably, distillation water wash of Lithium hydrate wet product 15L, temperature for obtaining per 300kg solid-liquid separation at 50 DEG C.
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CN114956128A (en) * | 2022-03-08 | 2022-08-30 | 宁夏中化锂电池材料有限公司 | Method and system for preparing battery-grade lithium hydroxide and lithium carbonate |
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EP3686300A1 (en) * | 2017-08-02 | 2020-07-29 | JX Nippon Mining & Metals Corporation | Sodium removal method, metal concentrating method, and metal recovery method |
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CN109761251A (en) * | 2019-04-11 | 2019-05-17 | 天齐锂业资源循环技术研发(江苏)有限公司 | A method of lithium hydroxide is prepared using waste and old lithium ion battery |
CN114956128A (en) * | 2022-03-08 | 2022-08-30 | 宁夏中化锂电池材料有限公司 | Method and system for preparing battery-grade lithium hydroxide and lithium carbonate |
CN115432721A (en) * | 2022-07-08 | 2022-12-06 | 江苏容汇通用锂业股份有限公司 | Process for preparing lithium hydroxide |
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Effective date of registration: 20210106 Address after: Xuankou Town, Wenchuan County, Aba Tibetan and Qiang Autonomous Prefecture, Sichuan Province Patentee after: SICHUAN STATE LITHIUM MATERIALS Co.,Ltd. Address before: 623001 ABA Zhongsheng Lithium Industry Co., Ltd., Xuankou Town, Wenchuan County, Aba Tibetan and Qiang Autonomous Prefecture, Sichuan Province Patentee before: ABA ZHONGSHENG LITHIUM Co.,Ltd. |