CN107954455A - A kind of method for preparing battery-level lithium carbonate using waste liquid containing lithium - Google Patents
A kind of method for preparing battery-level lithium carbonate using waste liquid containing lithium Download PDFInfo
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- CN107954455A CN107954455A CN201711277088.1A CN201711277088A CN107954455A CN 107954455 A CN107954455 A CN 107954455A CN 201711277088 A CN201711277088 A CN 201711277088A CN 107954455 A CN107954455 A CN 107954455A
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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
- C01D15/08—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of method for preparing battery-level lithium carbonate using waste liquid containing lithium.This method is by distilling, cleaning, evaporating, dissolving, sinker, washing and dry several simple and practicable operating procedures, you can battery-level lithium carbonate is prepared into from the waste liquid containing lithium of complicated component, and the rate of recovery is up to more than 96%.The method of the present invention rationally utilizes alcohols solvent, without adding BaCl2The impurity removal reagents of additional impurities are easily introduced with ammonium oxalate etc., just can effectively remove the impurity in lithium carbonate, technique is simple, easy to operation, good product quality, and the rate of recovery is high, cost is low, pollution-free.Waste liquid containing lithium caused by being suitable in the particularly medicine intermediate production process of the waste liquid containing lithium in industrial production is handled, and has important industrial utility value.
Description
Technical field
The invention belongs to battery material technical field, and in particular to a kind of to prepare battery-level lithium carbonate using waste liquid containing lithium
Method.
Background technology
Lithium, silvery white non-ferrous metal, symbol of element Li, atomic number 3, atomic weight 6.941.Density 0.534g/cm3, it is density
Minimum metal.180 DEG C of fusing point, 1340 DEG C of boiling point.Dew empties gradual change yellow or black in gas.Meet water vigorous reaction generation hydrogen-oxygen
Change lithium and hydrogen, react releasing hydrogen rapidly with dilute hydrochloric acid and dilute sulfuric acid, it is slower with cold effect of sulfuric acid, it is fierce with nitric acid effect.
The nitridation lithium layer for generating protectiveness is not reacted with nitrogen with oxygen reaction under room temperature.It is heated to generation oxidation at more than 100 DEG C
Lithium, when red heat, can act on hydrogen.Can be with halogen and the direct chemical combination of sulphur under certain condition.
Lithium compound has the effect such as calmness, analgesia, diuresis, in terms of having been used for medicine for many years, can treat mental disease, wind
The diseases such as wet arthritis.During medicine intermediate containing lithium is produced, a large amount of waste liquids containing lithium can be produced, and lithium salts price is held high
It is expensive, there is higher recovery value.
Lithium carbonate is important industrial products, and the important intermediate of the other lithium salts of production, in chemical industry, metal smelting
It is widely used in the traditional industries such as refining, ceramic material manufacture, health care and air conditioner refrigerating.In recent years, due to electronic information, lithium
Battery and atom energy field develop rapidly, and especially new-energy automobile industry in China's has been enter into rapid growth period, cathode
Material production capacity is expanded, and the fast development and demand for driving upstream battery-level lithium carbonate industry increase rapidly.Battery-level lithium carbonate
Compared with the product index of industrial level lithium carbonate, in addition to purity requirement is high, dopant species and concentration requirement are more stringent.
Patent application CN1781847 discloses a kind of method using the production lithium chloride of waste liquid containing lithium, and lithium alkylide is produced
During produce waste liquid containing lithium and be separated through grease, water mutually neutralizes filtering and impurity removing, then the spray-dried lithium chloride that directly obtains is brilliant
Body, its purity can reach 98%, can be directly used for the production of lithium metal.But in the method dedoping step, add precipitating reagent chlorination
Barium, ammonium oxalate etc. because lithium oxalate solubility is not too much high, may cause part lithium ion in the form of lithium oxalate with impurity together
It is removed the reduction rate of recovery, and adds and remaining iron, barium plasma are the impurity additionally introduced, is not pocessed influencing
The quality of last lithium chloride products.
Patent application CN1211546 discloses method for treating waste liquid containing lithium caused by a kind of synthesis of alkyl lithium compound,
It will contain lithium waste liquid at a temperature of the protection of 0.01~0.03MPa nitrogen pressures and 0~60 DEG C to be hydrolyzed, pH is adjusted twice through hydrochloric acid
For value with after filtering twice, filtrate adds Na2CO3, reacted at a temperature of 90~95 DEG C and Li be made2CO3Product, or filtrate is dehydrated
Be electrolysed to obtain lithium metal after LiCl crystallizations, solve that lithium slag in the prior art is difficult to recycle or recovery process is unstable, dangerous
The problems such as, have the advantages that technique be simple and convenient to operate, securely and reliably, the rate of recovery is high and good product quality, be widely used in closing
Into lithium alkylide technique application.But the method is reacted since hydrochloric acid is used for multiple times, the impurity such as more iron, magnesium are introduced, if
Prepare the high battery grade lithium product of purity requirement, it is also necessary to extend technological process, increase removal step, reduce the rate of recovery；
New impurity can be introduced using traditional removal step again at the same time, purifying cost is too high.
Patent application public affairs CN102874849 discloses a kind of from the special anhydrous chlorine of the recycling lithium production electrolysis of pharmacy waste water containing lithium
Change the method for lithium, including following technological process：A, dispensing cleans；B, just except organic；C, light electrolysis depth is except organic；D, concentration analysis
Sodium；E, evaporative crystallization；F, centrifuge；G, drying；H, cooling packing.This method is directly from the recycling lithium production of pharmacy waste water containing lithium
Be electrolysed special anhydrous lithium chloride, product purity it is high (>99%), sodium content it is low (<0.25%), product whiteness is good.But cleaning
When equally introduce BaCl2With the impurity such as ammonium oxalate；And sodium is analysed only with concentration, sodium content is higher in obtained lithium chloride；This
Outside, electricity consumption releases organic matter, high energy consumption.
The content of the invention
There is the new impurity of introducing, it is necessary to repeatedly clean in the method that the prior art recycles lithium from waste liquid containing lithium, increase cost,
But also the problem of lithium product quality can be influenced.For the technical problem, utilized it is an object of the invention to provide one kind and contain lithium
The method that waste liquid prepares battery-level lithium carbonate.This method improves the rate of recovery and recycles the quality of product, simplifies recovery process, reduces
Cost.
The above-mentioned purpose of the present invention is achieved through the following technical solutions：
A kind of method for preparing battery-level lithium carbonate using waste liquid containing lithium, comprises the following steps：
1) distill：Distillation processing is carried out to waste liquid containing lithium, obtains distillate and mother liquor；
2) clean：With alkali regulating step 1) the obtained pH to 9.5~12 of mother liquor, add carbonic acid while pH is adjusted
Salt, separates solid-liquid, leaves and takes clear liquid；The pH to 0.5~6.0 of clear liquid is adjusted with hydrochloric acid；Boil the pH for adjusting clear liquid after clear liquid with alkali
Removal of impurities liquid is obtained after to 6.0~9.0, the H that mass fraction is 25~50% is added into removal of impurities liquid2O2, it is purified after reaction
Liquid；
3) evaporate：Gained scavenging solution in step 2) is evaporated, obtains LiCl crude products；
4) dissolve：The obtained LiCl crude products of step 3) are dissolved with organic solvent, after dissolving, separation of solid and liquid is left and taken molten
Liquid, solid are dried to obtain auxiliary product, and the organic solvent is absolute methanol or absolute ethyl alcohol；
5) sinker：Carbonate solution is added to the solution of step 4) to be reacted, and separates solid-liquid, and mother liquor distill
The absolute ethyl alcohol reusable edible arrived；
6) wash：Obtained solid in step 5) is stirred with water and is washed more than twice, then separation of solid and liquid obtains solid；
7) it is dry：The solid of step 6) is dried, obtains battery-level lithium carbonate.
The above-mentioned method that battery-level lithium carbonate is prepared using waste liquid containing lithium of the present invention is particularly suitable for medicine intermediate production
During caused complicated component waste liquid containing lithium.
In some embodiments of the invention, caused complicated component contains lithium in the medicine intermediate production process
Waste liquid contains：10-30g/L Li+、0.05-1g/L SO4 2-、0-0.1g/L Fe2、0-0.5g/L Ca2+、0-0.5g/L Mg2+、
0-0.1g/L K+、100-250g/L Cl-, pH 0.1-4.
The above-mentioned method for preparing battery-level lithium carbonate using waste liquid containing lithium of the present invention, wherein the step 2) alkali are independently
NaOH solution, KOH solution, LiOH solution etc.；The carbonate is sodium carbonate, potassium carbonate etc..
The above-mentioned method for preparing battery-level lithium carbonate using waste liquid containing lithium, wherein the step 2) H2O2Volume for removal of impurities
0.01~1 times of liquid product, reaction time 1-240min；
The above-mentioned method for preparing battery-level lithium carbonate using waste liquid containing lithium, wherein the step 4) auxiliary product be NaCl,
KCl or its mixture, the drying temperature of solid is 80-400 DEG C, time 0.5-48h.
The above-mentioned method for preparing battery-level lithium carbonate using waste liquid containing lithium, the wherein step 5) carbonate solution is carbonic acid
Sodium or solution of potassium carbonate, solution concentration 100-330g/L, the amount of addition be the excess coefficient that reacts completely for -20% to
150%, reaction temperature is 20-100 DEG C, reaction time 10-300min.
The above-mentioned method for preparing battery-level lithium carbonate using waste liquid containing lithium, wherein step 6) is stirred when washing, solid-to-liquid ratio 2:1-
1:20, temperature is 20-100 DEG C, stirs and washes time 10-300min.
The above-mentioned method for preparing battery-level lithium carbonate using waste liquid containing lithium, wherein step 7) drying temperature are 80-400 DEG C,
Time is 0.5-48h.
The above-mentioned method for preparing battery-level lithium carbonate using waste liquid containing lithium of the present invention is certain with being added after hydrochloric acid, alkali removal of impurities
The H of amount2O2Remaining a small amount of organic matter in further oxidation removal evaporated mother liquor, ensure that no organic matter is brought into LITHIUM BATTERY carbon
In sour lithium；With absolute ethyl alcohol or methanol dissolving LiCl crude products, the NaCl that exists originally in initial gross separation crude product or introduce by soda acid,
KCl、CaCl2、FeCl2、MgCl2Or the impurity such as boron-containing compound so that each impurity element index of gained lithium carbonate is through follow-up step
Meet battery-level lithium carbonate standard after rapid processing；Carrier by the use of absolute ethyl alcohol as sinker solution, lithium carbonate dissolve in ethanol
Degree is low compared with water, therefore solution need not be heated as traditional handicraft and can guarantee that remaining lithium is relatively low in solution,
The rate of recovery of lithium carbonate is improved, and with absolute ethyl alcohol sinker, further increases impurity-eliminating effect.The method technique letter of the present invention
It is single, it is easy to operation, other impurity are not introduced, and good product quality, the rate of recovery is high, cost is low, pollution-free, gained battery-level lithium carbonate
The rate of recovery may be up to more than 96%.
Brief description of the drawings
Fig. 1 is the process flow chart of the method for the present invention.
Embodiment
The method that the present invention prepares battery-level lithium carbonate using waste liquid containing lithium, suitable for handling waste liquid containing lithium, particularly medicine
The waste liquid containing lithium of caused complicated component in intermediate production process.
In some embodiments of the invention, caused complicated component contains lithium in the medicine intermediate production process
Waste liquid mainly forms as shown in table 1 below：
Table 1
The method that battery-level lithium carbonate is prepared using waste liquid containing lithium, is comprised the following steps：
1) distill：Distillation processing is carried out to waste liquid containing lithium, obtains distillate and mother liquor；
2) clean：With alkali regulating step 1) the obtained pH to 9.5~12 of mother liquor, add carbonic acid while pH is adjusted
Salt, separates solid-liquid, leaves and takes clear liquid；The pH to 0.5~6.0 of clear liquid is adjusted with hydrochloric acid；Boil the pH for adjusting clear liquid after clear liquid with alkali
Removal of impurities liquid is obtained to 6.0~9.0, the hydrogen peroxide that mass fraction is 25~50% is added into removal of impurities liquid, reaction is after a certain period of time
It is purified liquid；
3) evaporate：Gained scavenging solution in step 2) is evaporated, obtains LiCl crude products；
4) dissolve：The obtained LiCl crude products of step 3) are dissolved with organic solvent, after dissolving, separation of solid and liquid is left and taken molten
Liquid, solid drying is auxiliary product NaCl, KCl or NaCl and KCl mixtures, and the organic solvent is absolute methanol or anhydrous second
Alcohol；
5) sinker：Carbonate solution is added to the solution of step 4) to be reacted, and separates solid-liquid, and mother liquor distill
The absolute ethyl alcohol reusable edible arrived；
6) wash：Obtained solid in step 5) is stirred with water and is washed more than twice, then separation of solid and liquid obtains solid；
7) it is dry：The solid of step 6) is dried, obtains battery-level lithium carbonate.
As preferable technical solution, the wherein step 2) alkali is independently NaOH solution, KOH solution, LiOH solution
Deng；The carbonate is for sodium carbonate, potassium carbonate etc., the H2O2Volume is 0.01-1 times of scavenging solution volume, reaction time 1-
240min, wherein step 4) sodium chloride, the drying temperature of potassium chloride are 80-400 DEG C, time 0.5-48h.Wherein step 5) institute
The concentration for stating carbonate solution is 100-330g/L, and the amount of addition is that the excess coefficient reacted completely is -20% to 150%, instead
It is 20-100 DEG C to answer temperature, reaction time 10-300min.Wherein step 6) is stirred when washing, solid-to-liquid ratio 2:1―1:20, temperature
For 20-100 DEG C, stir and wash 10-300min of time.Wherein step 7) drying temperature is 80-400 DEG C, time 0.5-48h.
Explained below by way of specific embodiment is further to the content of the invention of the present invention, but should not be construed as the present invention
Scope be only limitted to following example, invention thinking according to the present invention and entire contents, can will be each in following instance
Technical characteristic makes appropriate combination/replacement/adjustment/modification etc., this is easy to those skilled in the art, is still fallen within
The category that the present invention protects.The test method of actual conditions is not specified in the following example, usually according to normal condition.
Embodiment 1
(1) distill
The waste liquid of 100L is taken, carries out vacuum distillation, vacuum 400mbar.Distillation end point control is in distillate and mother liquor
Volume ratio is 1：1, stop distillation, obtain the evaporated mother liquor of about 50L.
(2) clean
The evaporated mother liquor obtained in (1) is first adjusted into pH to 12 with the NaOH solution of 10mol/L or so, is added at the same time
Na2CO3It is stirred separation of solid and liquid after 30min；Gained clear liquid industry HCl is adjusted into pH to 2.0, boils 30min；Use saturation
LiOH solution adjusts pH to 7.0 and is purified liquid；Volume according to scavenging solution adds 0.01 times of volume H thereto2O2(quality point
Number 30%) after be stirred 30min, obtain colourless scavenging solution.
(3) evaporate
Gained scavenging solution in (2) is evaporated, obtains LiCl crude products.
(4) absolute ethyl alcohol dissolves
Obtained LiCl crude products in (3) are dissolved in the ratio of 1L absolute ethyl alcohols according to 170g LiCl, add anhydrous second
Alcohol, stirring and dissolving 30min or so, separation of solid and liquid obtain the ethanol solution and NaCl solids of LiCl.
(5) sodium carbonate liquor that concentration is 100g/L is added in the liquid obtained to step (4), the amount of addition is to be excessive
Number -20%, reaction temperature are 50 DEG C, reaction time 100min.It is separated by filtration to obtain the mixing of lithium carbonate and solid sodium chloride
Thing and mother liquor；
(6) hybrid solid obtained in step (5) is stirred with water and washed, it is solid-to-liquid ratio 2 to stir the ratio of washing:1, stir and wash temperature 25
DEG C, stir and wash time 10min.Stir wash it is secondary after the completion of, separation of solid and liquid obtains lithium carbonate wet product and stirs wash water；
(7) lithium carbonate obtained in step (6) is dried, 100 DEG C of drying temperature, drying time 2h, obtains carbonic acid
Lithium product；NaCl solids in step (4) are dried, 100 DEG C of drying temperature, drying time 2h, obtains NaCl auxiliary products.
By above-mentioned technique, the rate of recovery of lithium carbonate is up to 97.1%, and quality reaches battery-level lithium carbonate standard, and analysis data are shown in
Table 2.
Embodiment 2
(1) distill
The waste liquid of 100L is taken, carries out vacuum distillation, distillation pressure 1000mbar, distillation end point is controlled in distillate and mother liquor
Volume ratio be 4：Stop distillation when 1, obtain the evaporated mother liquor of about 20L.
(2) clean
The evaporated mother liquor obtained in (1) is first adjusted into pH to 12 with the NaOH of 20mol/L or so while adds Na2CO3Carry out
Separation of solid and liquid after stirring 30min；Gained clear liquid industry HCl is adjusted into pH to 0.5 or so, boils 60min；It is molten with saturation LiOH
Liquid adjusts pH to 6.0 and is purified liquid；Volume according to scavenging solution adds 0.5 times of volume H thereto2O2(mass fraction 25%)
After be stirred 60min, obtain colourless scavenging solution.
(3) evaporate
Gained scavenging solution in (2) is evaporated, obtains LiCl crude products.
(4) methanol dissolves
Obtained LiCl crude products in (3) are dissolved in the ratio of 1L methanol according to 100g LiCl, add methanol, stirring is molten
30min or so is solved, separation of solid and liquid obtains the methanol solution and NaCl solids of LiCl.
(5) sodium carbonate liquor that concentration is 180g/L is added in the liquid obtained to step (4), the amount of addition is to be excessive
Number -15%, reaction temperature are 55 DEG C, reaction time 110min.It is separated by filtration to obtain the mixing of lithium carbonate and solid sodium chloride
Thing and mother liquor；
(6) hybrid solid obtained in step (5) is stirred with water and washed, it is solid-to-liquid ratio 1 to stir the ratio of washing:2, stir and wash temperature 75
DEG C, stir and wash time 40min.Stir wash it is secondary after the completion of, separation of solid and liquid obtains lithium carbonate wet product and stirs wash water；
(7) lithium carbonate obtained in step (6) is dried, 120 DEG C of drying temperature, drying time 2h, obtains carbonic acid
Lithium product；NaCl solids in step (4) are dried, 120 DEG C of drying temperature, drying time 2h, obtains NaCl auxiliary products.
By above-mentioned technique, the rate of recovery of lithium reaches 96.2%, and product quality reaches battery-level lithium carbonate standard, analyzes data
It is shown in Table 2.
Embodiment 3
(1) distill
The waste liquid of 100L is taken, carries out vacuum distillation, vacuum 200mbar.Distillation end point control is in distillate and mother liquor
Volume ratio is 1：4 or so, stop distillation, obtain the evaporated mother liquor of about 80L.
(2) clean
The evaporated mother liquor obtained in (1) is first adjusted into pH to 12 with the lithium hydroxide of 1mol/L or so while adds potassium carbonate
It is stirred separation of solid and liquid after 50min；Gained clear liquid industry HCl is adjusted into pH to 0.5, boils 10min；It is molten with saturation LiOH
Liquid adjusts pH to 9.0 and obtains removal of impurities liquid；Volume according to removal of impurities liquid adds 1.0 times of volume H thereto2O2(mass fraction 50%)
After be stirred 45min, obtain colourless scavenging solution.
(3) evaporate
Gained scavenging solution in (2) is evaporated, obtains LiCl crude products.
(4) absolute ethyl alcohol dissolves
Obtained LiCl crude products in (3) are dissolved in the ratio of 1L absolute ethyl alcohols according to 150g LiCl, add anhydrous second
Alcohol, stirring and dissolving 60min or so.Separation of solid and liquid obtains the ethanol solution and KCl and NaCl solids of LiCl.
(5) sodium carbonate liquor that concentration is 300g/L is added in the liquid obtained to step (4), the amount of addition is to be excessive
Number 5%, reaction temperature are 95 DEG C, reaction time 150min.It is separated by filtration to obtain lithium carbonate and the mixture of solid sodium chloride
And mother liquor；
(6) hybrid solid obtained in step (5) is stirred with water and washed, it is solid-to-liquid ratio 1 to stir the ratio of washing:3, stir and wash temperature 90
DEG C, stir and wash time 45min.Stir wash it is secondary after the completion of, separation of solid and liquid obtains lithium carbonate wet product and stirs wash water；
(7) lithium carbonate obtained in step (6) is dried, 110 DEG C of drying temperature, drying time 4h, obtains carbonic acid
Lithium product；NaCl solids in step (4) are dried, 110 DEG C, drying time 4h of drying temperature, obtains NaCl and KCl is attached
Product.
By above-mentioned technique, the rate of recovery of lithium carbonate is up to 97.5%, and quality reaches battery-level lithium carbonate standard, and analysis data are shown in
Table 2.
Embodiment 4
(1) distill
The waste liquid of 100L is taken, carries out vacuum distillation, vacuum 220mbar.Distillation end point control is in distillate and mother liquor
Volume ratio is 1：2 or so, stop distillation, obtain the evaporated mother liquor of about 66.7L.
(2) clean
The evaporated mother liquor obtained in (1) is first adjusted into pH to 12 with the lithium hydroxide of 1.5mol/L or so while adds carbonic acid
Potassium is stirred separation of solid and liquid after 40min；Gained clear liquid industry HCl is adjusted into pH to 0.5, boils 20min；With saturation LiOH
Solution adjusts pH to 9.0 and obtains removal of impurities liquid；Volume according to removal of impurities liquid adds 0.6 times of volume H thereto2O2(mass fraction
50%) 40min is stirred after, obtains colourless scavenging solution.(3) evaporate
Gained scavenging solution in (2) is evaporated, obtains LiCl crude products.
(4) absolute ethyl alcohol dissolves
Obtained LiCl crude products in (3) are dissolved in the ratio of 1L absolute ethyl alcohols according to 150g LiCl, add anhydrous second
Alcohol, stirring and dissolving 60min or so.Separation of solid and liquid obtains the ethanol solution and KCl solids of LiCl.
(5) solution of potassium carbonate that concentration is 300g/L is added in the liquid obtained to step (4), the amount of addition is to be excessive
Number 5%, reaction temperature are 92 DEG C, reaction time 150min.It is separated by filtration to obtain lithium carbonate and the mixture of solid sodium chloride
And mother liquor；
(6) hybrid solid obtained in step (5) is stirred with water and washed, it is solid-to-liquid ratio 1 to stir the ratio of washing:3, stir and wash temperature 92
DEG C, stir and wash time 30min.Stir wash it is secondary after the completion of, separation of solid and liquid obtains lithium carbonate wet product and stirs wash water；
(7) lithium carbonate obtained in step (6) is dried, 150 DEG C of drying temperature, drying time 3h, obtains carbonic acid
Lithium product；KCl solids in step (4) are dried, 150 DEG C of drying temperature, drying time 4h, obtains KCl auxiliary products.
By above-mentioned technique, the rate of recovery of lithium carbonate is up to 96.9%, and quality reaches battery-level lithium carbonate standard, and analysis data are shown in
Table 2.
Table 2
Claims (9)
- A kind of 1. method for preparing battery-level lithium carbonate using waste liquid containing lithium, it is characterised in that comprise the following steps：1) distill：Distillation processing is carried out to waste liquid containing lithium, obtains distillate and mother liquor；2) clean：With alkali regulating step 1) the obtained pH to 9.5~12 of mother liquor, carbonate is added while pH is adjusted, point From solid-liquid, clear liquid is left and taken；The pH to 0.5~6.0 of clear liquid is adjusted with hydrochloric acid；Boil the pH to 6.0 for adjusting clear liquid after clear liquid with alkali Removal of impurities liquid is obtained after~9.0, the H that mass fraction is 25~50% is added into removal of impurities liquid2O2, liquid is purified after reaction；3) evaporate：Gained scavenging solution in step 2) is evaporated, obtains LiCl crude products；4) dissolve：The obtained LiCl crude products of step 3) to be dissolved with organic solvent, after dissolving, separation of solid and liquid leaves and takes solution, Gu Body is dried to obtain auxiliary product, and the organic solvent is absolute methanol or absolute ethyl alcohol；5) sinker：Carbonate solution is added to the solution of step 4) to be reacted, and separates solid-liquid, what mother liquor was distilled Absolute ethyl alcohol reusable edible；6) wash：Obtained solid in step 5) is stirred with water and is washed more than twice, then separation of solid and liquid obtains solid；7) it is dry：The solid of step 6) is dried, obtains battery-level lithium carbonate.
- 2. the method according to claim 1 for preparing battery-level lithium carbonate using waste liquid containing lithium, it is characterised in that described to contain Lithium waste liquid is waste liquid containing lithium caused by medicine intermediate production process.
- 3. the method according to claim 2 for preparing battery-level lithium carbonate using waste liquid containing lithium, it is characterised in that described to contain Lithium waste liquid contains：10-30g/L Li+、0.05-1g/L SO4 2-、0-0.1g/L Fe2、0-0.5g/L Ca2+、0-0.5g/L Mg2 +、0-0.1g/L K+、100-250g/L Cl-, pH 0.1-4.
- 4. the method according to claim 1 for preparing battery-level lithium carbonate using waste liquid containing lithium, it is characterised in that wherein walk Rapid 2) described alkali is independently NaOH solution, KOH solution or LiOH solution；The carbonate is sodium carbonate or potassium carbonate.
- 5. the method according to claim 1 for preparing battery-level lithium carbonate using waste liquid containing lithium, it is characterised in that wherein walk Rapid 2) described H2O2Volume for removal of impurities liquid product 0.01~1 times, reaction time 1-240min.
- 6. the method according to claim 1 for preparing battery-level lithium carbonate using waste liquid containing lithium, it is characterised in that wherein walk Rapid 4) described auxiliary product is NaCl, KCl or its mixture, and the drying temperature of solid is 80-400 DEG C, time 0.5-48h.
- 7. the method according to claim 1 for preparing battery-level lithium carbonate using waste liquid containing lithium, it is characterised in that wherein walk Rapid 5) described carbonate solution is sodium carbonate or solution of potassium carbonate, and solution concentration 100-330g/L, the amount of addition is completely anti- The excess coefficient answered is -20% to 150%, and reaction temperature is 20-100 DEG C, reaction time 10-300min.
- 8. the method according to claim 1 for preparing battery-level lithium carbonate using waste liquid containing lithium, it is characterised in that wherein walk It is rapid 6) to stir when washing, solid-to-liquid ratio 2:1-1:20, temperature is 20-100 DEG C, stirs and washes time 10-300min.
- 9. the method according to claim 1 for preparing battery-level lithium carbonate using waste liquid containing lithium, it is characterised in that wherein walk Rapid 7) drying temperature is 80-400 DEG C, time 0.5-48h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115466842A (en) * | 2021-11-12 | 2022-12-13 | 金为环保科技(常州)有限公司 | Treatment method and application of waste lithium battery waste liquid |
| CN116002726A (en) * | 2023-03-06 | 2023-04-25 | 四川轻化工大学 | Lithium carbonate and method for preparing lithium carbonate by using low-lithium chloride sodium-containing feed liquid |
| WO2023169022A1 (en) * | 2022-03-07 | 2023-09-14 | 华中科技大学 | Method for processing and recycling ultrathin lithium foil, and product |
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