CN106745102A - A kind of preparation technology of lithium carbonate - Google Patents
A kind of preparation technology of lithium carbonate Download PDFInfo
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- CN106745102A CN106745102A CN201710041119.7A CN201710041119A CN106745102A CN 106745102 A CN106745102 A CN 106745102A CN 201710041119 A CN201710041119 A CN 201710041119A CN 106745102 A CN106745102 A CN 106745102A
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Abstract
The invention discloses a kind of preparation technology of lithium carbonate, comprise the following steps：Step S1 removal of impurities enrichment process：After salt lake bittern removal of impurities concentration, concentrate containing lithium is formed；Step S2 carbonization sinker operations：To the accessory substance washing soda Crystallization reaction solution added in the concentrate containing lithium of step S1 during urea method production biruea, during original state, sodium carbonate and the mol ratio of lithium are 1.2~1.6 in reaction solution：2, reacted rear generation lithium carbonate precipitation；Step S3 postorder treatment process：The lithium carbonate precipitation of step S2 generations is isolated, it is scrubbed, be dried to obtain lithium carbonate product.The present invention produces the accessory substance washing soda crystal of biruea using urea method, solves the problems, such as the recycling to the material, saves its long-distance transport cost.The preparation cost of lithium carbonate is also saved simultaneously, with economic benefit higher.Using preparation technology of the invention, moreover it is possible to obtain high-quality lithium carbonate product, used beneficial to the later stage.
Description
Technical field
The present invention relates to the technical field that bittern carries lithium, and in particular to a kind of preparation technology of lithium carbonate.
Background technology
Lithium is most light metal in nature, strong etc. unique physico with high specific heat, high conductivity and chemism
Characteristic is learned, there is extensive purposes.At present, lithium metal and its compound are in glass ceramics, electrolytic aluminium, lubricating grease, air conditioner refrigerating
With the application sustainable growth in the traditional industry field such as organic synthesis, metallurgy, medicine, chemical industry, reagent, in aluminium lithium alloy, lithium battery
Application with civilian industry, high-tech and the military industry field such as nuclear fusion is also rapidly expanded.Because of its answering in terms of lithium battery
With lithium metal is also known as " 21 century energy upstart ".
At present, the most common method for lithium being extracted from nature is that ore puies forward lithium method, and the method refers to spodumene, lithium cloud
The solid such as mother lithium ore is raw material, production lithium carbonate and other lithium products, and spodumene is main containing one of lithium minerals, also known as α
Type spodumene, theoretical amount containing lithium is 3.75%.Ore puies forward lithium method includes limestone sintering process and sulfuric acid process, based on cost and technique
Consideration, now generally use sulfuric acid process, its technique is that α type spodumenes are calcined during to 1000 DEG C or so, it is changed into β
Type spodumene, then mixes β type spodumenes with sulfuric acid, acidified roasting, generates solvable lithium sulfate, and sulfuric acid is obtained by leaching
Lithium solution, purified, evaporation and concentration, sinker are obtained primary lithium carbonate product after drying.The method was by the development work of more than 50 years
Skill is ripe, but in the method, sulfuric acid can only leach β type spodumenes, and can not be reacted with α types spodumene, therefore, need
α type spodumenes are converted into by the more loose β type spodumenes of structure by high-temperature roasting first, therefore from the angle of reaction principle
Consider, it is impossible to reduce sulfuric acid process and carry the cost that lithium technique is spent.And the production of country's lithium salts and equipment are uneven at present,
Most enterprise's equipments fall behind, seriously polluted, are unfavorable for the extensive development of sulfuric acid process.
Lithium from Salt Lake Brine resource accounts for the 70~80% of nature lithium resource total amount, therefore, lithium is extracted from salt lake bittern
It is the main direction for putting forward lithium technique now.
The content of the invention
It is an object of the invention to provide a kind of preparation technology of lithium carbonate, lithium method cost is carried for solving existing ore
Height, complex process, with serious pollution problem.
To achieve these goals, the present invention provides following technical scheme：A kind of preparation technology of lithium carbonate, its feature exists
In comprising the following steps：
Step S1 removal of impurities enrichment process：
After salt lake bittern removal of impurities is concentrated, concentrate containing lithium is formed；
Step S2 carbonization sinker operations：
Reaction solution is formed to addition sodium carbonate material in the concentrate containing lithium, during reaction original state, the reaction solution
Middle sodium carbonate is 1.2~1.6 with the mol ratio of lithium：2, it is reacted after, in the reaction solution generate lithium carbonate precipitation,
Wherein, the sodium carbonate material is the accessory substance washing soda crystal during urea method production biruea；
Step S3 postorder treatment process：
The lithium carbonate precipitation is isolated, final product lithium carbonate product is obtained after scrubbed, drying.
Preferably, the step S1 removal of impurities enrichment process comprises the following steps：
Step a1：Salt lake bittern feeding is equipped with the adsorption-desorption device of lithium adsorbent, by absorption, drip washing
And desorption manipulation, lithium desorption liquid is obtained；
Step b1：Magnesium ion in the lithium desorption liquid is removed by cationic ion-exchange resin, removal of impurities liquid is obtained；
Step c1：The removal of impurities liquid is realized to concentrate using reverse osmosis concentration operation and evaporation and concentration operation, is formed and is contained lithium
Concentrate.
Further, the lithium concentration containing lithium concentrate described in step S1 is 20~25g/L.
Preferably, the sodium carbonate material in the step S2 carbonizations sinker operation is through the sodium carbonate seminal fluid after treatment, institute
The treatment process for stating sodium carbonate material comprises the following steps：
Step a2：It is the accessory substance washing soda placement during urea method production biruea by the sodium carbonate material
In dissolving tank, dissolve it by heating complete, sodium carbonate liquor is obtained；
Step b2：The sodium carbonate liquor is set to realize removal of impurities by millipore filter, filter pressure is 0.05~0.1MPa,
Sodium carbonate seminal fluid is obtained.
Specifically, the heating-up temperature of sodium carbonate liquor described in step a2 is 30~40 DEG C.
Preferably, step S2 carbonization sinker operation in, reaction solution stir speed (S.S.) during the course of the reaction be 30~
60r/min, reaction temperature is 30~40 DEG C, and the reaction time continues 20~40min.
Preferably, in step S2 carbonizations sinker operation, during reaction original state, sodium carbonate and lithium rubs in the reaction solution
You are than being 1.4：2.
Preferably, the separate mode in step S3 postorders treatment process is crystallized to heat up, the intensification crystallization mode
In crystal solution temperature rise to 75~85 DEG C.
Further, after the liquid that the intensification crystallization mode is isolated uses hydrochloric acid to be neutralized to pH for 5.5~6.5, make
It is played back to salt pan.
Preferably, the mode of washing in step S3 subsequent treatments operation is filtering and washing, and the drying mode is gas
Stream is dried and fluidized drying merges utilization.
Compared to prior art, the preparation technology of lithium carbonate of the present invention has the advantage that：Urea method production connection
Accessory substance washing soda crystal produced during two ureas, because containing a small amount of caustic soda and sodium chloride etc. in the accessory substance
Impurity, is extremely limited in traditional soda ash with field, and crystal water content accounts for total material proportion and is in the accessory substance
62.93%, therefore the cost of its long-distance transport is very high.The accessory substance is applied in the preparation process of lithium carbonate, it is right to solve
The problem that accessory substance washing soda is recycled, and the consumption saved in the preparation of lithium carbonate to soda ash is applied,
So as to effectively reduce the preparation cost of lithium carbonate, with economic benefit higher.Meanwhile, the lithium carbonate provided using the present invention
Preparation technology, obtained lithium carbonate quality is high, and impurity is few, beneficial to the later-stage utilization of lithium carbonate.
The preparation technology operation of lithium carbonate provided by the present invention is simple and easy to control, can whole-course automation carry out, beneficial to production
Stabilization is continued for.
Specific embodiment
The invention provides many applicable creative concepts, the creative concept can be reflected in a large number of on specific
Hereinafter.Specific embodiment described in following embodiments of the present invention is only as specific embodiment of the invention
Exemplary illustration, and be not meant to limit the scope of the invention.
With reference to specific embodiment, the invention will be further described.
The present embodiment provides a kind of preparation technology of lithium carbonate, comprises the following steps：
Step S1 removal of impurities enrichment process：
Step a1：First, by salt lake bittern adsorption-desorption device of the feeding equipped with lithium adsorbent so that salt lake bittern
Absorption, drip washing and desorption manipulation are sequentially passed through, lithium desorption liquid is obtained.Lithium concentration in the lithium desorption liquid is 0.4~0.6g/
L, magnesium ion concentration is 0.5~1.5g/L, and Na ion concentration is 0.3~0.5g/L, and chlorine ion concentration is 2.5~4.0g/L.
Above-mentioned absorption to salt lake bittern, drip washing, desorption manipulation are well known to those skilled in the art, therefore no longer detailed herein
State, the lithium adsorbent that the present embodiment is used including but not limited to manganese systems adsorbent, aluminium system adsorbent, titanium system adsorbent and compound
Stibate adsorbent, above-mentioned adsorbent is adsorbent common on the market, and price is low.
Step b1:Make above-mentioned lithium desorption liquid by calcium and magnesium polymeric adsorbent, so as to remove the magnesium ion in lithium desorption liquid so that
Magnesium ion concentration is less than 0.02mg/L.Above-mentioned calcium and magnesium polymeric adsorbent is the one kind in cationic ion-exchange resin.Selected by the present embodiment
Polymeric adsorbent is faintly acid (hydroxyl) resin cation, and resulting feed liquid is removal of impurities liquid.
Step c1：Removal of impurities liquid is concentrated, so as to improve the concentration of lithium ion.Conventional concentration method include the precipitation method,
Absorption method, hyperfiltration method, dialysis, the way of distillation, seasoning etc., the enrichment process in the present embodiment be preferably reverse osmosis concentration and
Evaporation and concentration is combined.
Counter-infiltration, also known as reverse osmosis, is the UF membrane behaviour for isolating solvent from solution typically with pressure differential as motive force
Make.Counter-infiltration operation applies pressure by the high concentration feed liquid to film side, and when pressure exceedes its osmotic pressure, solvent can be inverse
Inverse osmosis is made in the direction for naturally osmotic, and so as to the solvent passed through in the low-pressure side of film, i.e. penetrating fluid, high-pressure side obtains
The solution of concentration, i.e. concentrate.It is light that the hyperfiltration used in the present embodiment includes but is not limited to low pressure RO method, seawater
Change hyperfiltration, high pressure hyperfiltration and super-pressure hyperfiltration.
The removal of impurities liquid in the present embodiment is processed using hyperfiltration, light salt brine is obtained in the low-pressure side of film, in high-pressure side then
Obtain one section of lithium concentrate.Lithium concentration can be improved 8~12 times, generally 4.0~6.0g/L by one section of lithium concentrate.
Light salt brine obtained by hyperfiltration low-pressure side is reclaimed, in putting forward lithium operation for ion exchange adsorption,
Can be used as leacheate or de- analysis liquid, greatly reduce the water consumption of adsorption/desorption operation in lithium chloride production process, from
And reduces cost.
Because the concentrated effect of hyperfiltration is unable to reach requirement of the concentrate containing lithium to lithium concentration, therefore in the present embodiment
Further using evaporation and concentration operation to carrying out concentration containing one section of lithium concentrate after counter-infiltration operation.In the present embodiment
It is concentrated by evaporation operation and is preferably pressure vacuum cycle evaporation and concentration operation, compared to common evaporation and concentration work in concentration process
It is in hgher efficiency that sequence is concentrated, and the consumption of electric power, steam and cooling water is lower, is obtained containing lithium via being concentrated by evaporation after operation is processed
Concentrate, lithium concentration is 20~25g/L.
Because reverse osmosis concentration disposal ability is limited, and it is more to be concentrated by evaporation heat dissipation, therefore, the present embodiment uses counter-infiltration
Concentration and it is concentrated by evaporation the mode that is combined removal of impurities liquid is processed, heat can be saved, can also reaches to eventually forming
The requirement of lithium concentration in concentrate containing lithium.
Step S2 carbonization sinker operations：
In this step generation lithium carbonate sediment, the present embodiment institute are reacted by using sodium carbonate material and concentrate containing lithium
The oxide spinel sodium material for using is the accessory substance washing soda during urea method production biruea, urea method production di-
The reaction of urea and technique are well known to those skilled in the art, and it is first to produce hydrazine hydrate as raw material using urea, is then produced
Thing hydrazine hydrate continues to produce biruea with urea reaction after treatment, wherein producing the reaction of hydrazine hydrate as raw material using urea
Equation is as follows：
NaClO+2NaOH+H2NCONH2→N2H4·H2O+Na2CO3+NaCl
In order to product hydrazine hydrate is separated, common processing mode is that product feed liquid is lowered the temperature, so that
The washing soda crystal containing a small amount of sodium chloride is wrapped up in formation, and the washing soda crystal is separated using centrifugation.
The sodium carbonate material that this step is used is the above-mentioned accessory substance washing soda isolated.In order to improve this reality
Sodium carbonate material and the reaction efficiency containing lithium concentrate in example are applied, while the purity of the present embodiment final product lithium carbonate is improved,
The present embodiment is that accessory substance washing soda carries out corresponding treatment and becomes sodium carbonate seminal fluid to sodium carbonate material, then makes it
With the hybrid reaction of concentrate containing lithium in step S1.
The present embodiment is as follows to the process step of accessory substance washing soda：
Step a2：The accessory substance washing soda that urea method is produced during biruea is placed in dissolving tank, is passed through
It is heated so that washing soda all dissolves, and in order to avoid hot-spot, the present embodiment is preferably steam indirectly heat
Mode.Further, in order to avoid temperature to sodium carbonate liquor influence so influence the later stage lithium carbonate generation and in solution
In solubility, the sodium carbonate temperature of charge during the present embodiment controls dissolving tank during the heating is 30~40 DEG C.
Step b2：Sodium carbonate liquor in step a2 is set to realize removal of impurities by millipore filter, filter pressure is 0.05~
0.1MPa, to remove the cotton-shaped crystal of the magnesium hydroxide in sodium carbonate liquor and mechanical admixture, so as to application is obtained in step s 2
Sodium carbonate seminal fluid.
Millipore filter is the general designation of the membrane filter that aperture is 0.2~1um, its 0.1um that can filter liquid, gas
More than particulate and bacterium, with filtering accuracy is high, the rate of filtration fast, absorption comes off less, without medium, acid-alkali-corrosive-resisting etc. it is excellent
Point.Millipore filter used in the present embodiment is the millipore filter of macromolecule engineering plastic material, is added on the filter
The pressure of 0.05~0.1MPa of note, so as to realize to the filtering more than 0.5um crystalline solid.
To the sodium carbonate semen sample obtained through treatment, it is preferred to use the mode of addition calcium chloride is determined in sodium carbonate seminal fluid
Carbonate content, and make it be 1.2~1.6 according to the mol ratio of sodium carbonate and lithium：In 2 addition concentrates containing lithium, in reaction
During, reaction solution is in the excessive form of sodium carbonate, so as to improve the yield to lithium ion in concentrate containing lithium, and due to carbon
Sour sodium is soluble in water, therefore is easy to the later stage to sodium carbonate and the separating treatment of lithium carbonate.It is noted that experiments verify that,
When the mol ratio of sodium carbonate and lithium is 1.4：When 2, the yield highest of lithium.
Sodium carbonate seminal fluid and concentrate containing lithium are mixed to form reaction solution in a kettle., and are reacted as follows：Na2CO3+
2LiCl→Li2CO3+ 2NaCl, so as to form lithium carbonate precipitation in reactor.
Additionally, it is noted that above-mentioned reaction solution is during reaction, control the stir speed (S.S.) of reaction solution for 30~
60r/min, reaction temperature is 30~40 DEG C, and the reaction time continues 20~40min.
Above-mentioned response parameter is to be drawn through many experiments, under above-mentioned process conditions, can cause the carbonic acid in the present embodiment
Lithium rate of deposition is more than 95%, so as to increase the yield of lithium carbonate.
Step S3 postorder treatment process：
By the material output in step S2 reactors, lithium carbonate therein is isolated.Because the solubility of lithium carbonate is with temperature
The rising of degree and diminish, therefore the present embodiment using heat up crystallization by the way of to lithium carbonate realize separate.
Crystal solution is warming up to 75~85 DEG C, now the dissolving of lithium carbonate by the material exported in reactor as crystal solution
Degree 0.85g/ (100g water) left and right, so as to further increase the percent crystallization in massecuite of lithium carbonate, after by way of separation of solid and liquid will
It is separated.Simultaneously as topmost impurity component is sodium chloride and sodium carbonate in crystal solution, crystallized by heating up,
Can cause that the impurity in crystal solution dissolves in the solution as much as possible, so as to improve the purity of crystallization of lithium carbonate body.
The solution of lithium carbonate is dissolved with because containing substantial amounts of sodium chloride, so as to cause the lithium carbonate in solution to separate,
So the liquid material after Crystallization Separation is adjusted into pH in after 5.5~6.5 using hydrochloric acid, it is set to be played back to salt pan i.e.
Can.
The sodium carbonate crystallization isolated is used without ion desalted water filtering and washing, to rinse out the molten of crystal surface attachment
Liquid, afterwards, makes that crystallization passes sequentially through airstream drying tower and fluid bed is dried, and drying temperature is controlled to 110~120 DEG C, from
And final product lithium carbonate product is obtained.
Filtering and washing refers to that, using Buchner funnel, bottle,suction and aspiration pump, the filler tube of Buchner funnel is arranged on bottle,suction
Single hole plug in and be closely connected with bottle,suction, bottle,suction is connected with aspiration pump, treats that cleaning product is placed in Buchner funnel, on one side
To filling cleaning fluid in Buchner funnel while reducing the pressure in bottle,suction using suction filtration machine, so that the liquid in Buchner funnel
Body is flowed into bottle,suction along filler tube, so that the product in Buchner funnel is washed.
The method that pneumatic conveying drying is used in airstream drying tower, pneumatic conveying drying refers to that the dispersion of scattered particulate solid material is outstanding
In floating over high velocity air, a kind of method being dried under Geldart-D particle；The method that fluid bed uses fluidized drying, stream
It refers to make particle in fluidization during hot-air is blasted into the bed for be placed with wet granular to change drying, and heat is delivered to particle from air
Heat needed for moisture evaporation is provided, so that particle drying, because the ratio of heat transfer coefficient fixed bed under fluidization is big, therefore
The efficiency of fluidized drying is more much greater than fixed bed drying.Using the dry combination of above two, both reduced dried
Overall heat dissipation, in turn ensure that the drying effect of material, while also accelerating the drying efficiency of material so that by this reality in journey
Applying the drying device in example can continuously export qualified lithium carbonate product.
Via the preparation-obtained final product lithium carbonate product of the preparation technology of the present embodiment lithium carbonate, through analysis, carbon
The mass fraction of sour lithium is more than 99.26%, impurity component：Na2The mass fraction of O is 0.061~0.081%, Fe2O3Matter
Amount fraction is 0.040~0.082%, SO for the mass fraction of 0.0003~0.0005%, CaO4 2-Mass fraction for 0~
0.011%, Cl-Mass fraction be 0.014~0.040%, H2The mass fraction of O is 0.040~0.120%, hydrochloric acid insoluble substance
Mass fraction for 0.001~0.003%, MgO mass fraction be 0.019~0.034%.It is computed, the present embodiment is to carbon
The yield of sour lithium is generally 70~80%.
The state quality standard of industrial lithium carbonate is：The mass fraction more than 99.0% of lithium carbonate, impurity component：Na2O's
Mass fraction is less than 0.25%, Fe2O3Mass fraction for less than 0.015%, CaO mass fraction be less than 0.10%,
SO4 2-Mass fraction be less than 0.50%, Cl-Mass fraction be less than 0.020%, H2The mass fraction of O be 0.8% with
Under, the mass fraction of hydrochloric acid insoluble substance is less than 0.025% for the mass fraction of less than 0.050%, MgO.
Through comparing, using the lithium carbonate product quality prepared by the preparation technology in the present embodiment apparently higher than industrial carbonic acid
The state quality standard of lithium, therefore, using the lithium carbonate product quality drawn prepared by the present embodiment preferably, can be widely applied to
Industrial production.
Embodiment one
Step S1 removal of impurities enrichment process：
Step a1：By in salt lake bittern adsorption-desorption device of the feeding equipped with lithium adsorbent so that salt lake bittern is passed through successively
Absorption, drip washing and desorption manipulation are crossed, lithium desorption liquid is obtained.Lithium concentration in the lithium desorption liquid is 0.4g/L, and magnesium ion is dense
It is 0.5g/L to spend, and Na ion concentration is 0.3g/L, and chlorine ion concentration is 2.5g/L.
Step b1：Make above-mentioned lithium desorption liquid by calcium and magnesium polymeric adsorbent, so as to remove the magnesium ion in lithium desorption liquid so that
The magnesium ion concentration of lithium desorption liquid is 0.018mg/L, obtains removal of impurities liquid.
Step c1:Removal of impurities liquid is realized using reverse osmosis concentration method concentrating, obtain one section of lithium concentrate, one section of lithium concentration
Lithium concentration in liquid is 5.0g/L, and afterwards, continuation uses evaporating and concentrating process to one section of lithium concentrate, so as to obtain this implementation
Concentrate containing lithium in example, the lithium concentration for containing lithium concentrate is 20g/L.
Step S2 carbonization sinker operations：
Washing soda crystal is processed first, process step is as follows：
Step a2：The accessory substance washing soda crystal that urea method is produced during biruea is placed in dissolving tank,
Cause that washing soda crystal all dissolves using steam-heated mode, form sodium carbonate liquor, during heating, control
Temperature of charge in dissolving tank processed is 30 DEG C.
Step b2：The sodium carbonate liquor in step a2 is set to realize removal of impurities by millipore filter, filter pressure is set as
0.05MPa, to remove the cotton-shaped crystal of the magnesium hydroxide in sodium carbonate liquor and mechanical admixture, so that be obtained can be former as lithium carbonate
The sodium carbonate seminal fluid of material.
To sodium carbonate semen sample, the carbonate content in sodium carbonate seminal fluid, the sodium carbonate obtained by the present embodiment are determined
The concentration of seminal fluid is 5.06mol/L.
To contain in lithium concentrate input reactor, be 1.2 according to the mol ratio of sodium carbonate and lithium：2, the present embodiment is made
Standby sodium carbonate seminal fluid is added in reactor, hybrid reaction, and in the course of reaction of reaction solution, the stir speed (S.S.) of reaction solution sets
It is set to 30r/min, reaction temperature is 30 DEG C, persistently terminates reaction after 40min altogether.This step generates lithium carbonate in a kettle.
Precipitation.
Step S3 postorder treatment process：
Material in step S2 reactors is transferred in crystallization kettle, material is heated, with the increase of temperature of charge, knot
Crystalline solid in brilliant kettle gradually increases, after material is warming up to 75 DEG C, to the material in crystallization kettle by the way of centrifugation
Separated.
The solid material isolated using filtering and washing is carried out without ion desalted water, is then inputted pneumatic conveying drying first
It is dried in tower, then makes to be dried in its input fluid bed again, Two stage dryer temperature is disposed as 110 DEG C.Last thing
Material is exported from fluid bed, and natural cooling obtains final product the final product lithium carbonate product prepared by the present embodiment.
The liquid material isolated is played back to salt pan after its pH is adjusted into 6.5 using hydrochloric acid.
In the lithium carbonate product that the present embodiment is produced, the content of lithium carbonate is 99.32%, and impurity content is as follows：Na2O
Mass fraction be 0.0804%, Fe2O3Mass fraction for 0.0004%, CaO mass fraction be 0.0436%, SO4 2-'s
Mass fraction is 0, Cl-Mass fraction be 0.024%, H2The mass fraction of O is 0.12%, the mass fraction of hydrochloric acid insoluble substance
The mass fraction for being 0.002%, MgO is 0.0339%.It is computed, yield 73% of the present embodiment to lithium carbonate.
Embodiment two
Each step in the present embodiment is identical with embodiment one, and simply in the present embodiment, sodium carbonate material is used not
It is the accessory substance washing soda crystal during urea method production biruea, but soda ash solution, therefore omit to accessory substance
Process step a2~the b2 of washing soda, directly makes soda ash solution and the hybrid reaction of concentrate containing lithium.
In the lithium carbonate product that the present embodiment is produced, the mass fraction of lithium carbonate is 99.09%, and impurity content is as follows：
Na2The mass fraction of O is 0.1174%, Fe2O3Mass fraction for 0, CaO mass fraction be 0.0332, SO4 2-Quality point
Number is 0.0245, Cl-Mass fraction be 0.1313%, H2The mass fraction of O is 0.063%, the mass fraction of hydrochloric acid insoluble substance
The mass fraction for being 0.040%, MgO is 0.0392%.
Embodiment three
Step S1 removal of impurities enrichment process：
Step a1：By in salt lake bittern adsorption-desorption device of the feeding equipped with lithium adsorbent so that salt lake bittern is passed through successively
Absorption, drip washing and desorption manipulation are crossed, lithium desorption liquid is obtained.Lithium concentration in the lithium desorption liquid is 0.6g/L, and magnesium ion is dense
It is 1.5g/L to spend, and Na ion concentration is 0.5g/L, and chlorine ion concentration is 4.0g/L.
Step b1：Make above-mentioned lithium desorption liquid by calcium and magnesium polymeric adsorbent, so as to remove the magnesium ion in lithium desorption liquid so that
The magnesium ion concentration of lithium desorption liquid is 0.020mg/L, obtains removal of impurities liquid.
Step c1：Removal of impurities liquid is realized using reverse osmosis concentration method concentrating, obtain one section of lithium concentrate, one section of lithium concentration
Lithium concentration in liquid is 6.0g/L, and afterwards, continuation uses evaporating and concentrating process to one section of lithium concentrate, so as to obtain this implementation
Concentrate containing lithium in example, the lithium concentration for containing lithium concentrate is 25g/L.
Step S2 carbonization sinker operations：
Washing soda is processed first, process step is as follows：
Step a2：The accessory substance washing soda that urea method is produced during biruea is placed in dissolving tank, is used
Steam-heated mode causes that washing soda crystal all dissolves, and forms sodium carbonate liquor, during heating, controls molten
Temperature of charge in solution groove is 40 DEG C.
Step b2：The sodium carbonate liquor in step a2 is set to realize removal of impurities by millipore filter, filter pressure is set as
0.1MPa, to remove the cotton-shaped crystal of the magnesium hydroxide in sodium carbonate liquor and mechanical admixture, so that be obtained can be former as lithium carbonate
The sodium carbonate seminal fluid of material.
To sodium carbonate semen sample, the carbonate content in sodium carbonate seminal fluid, the sodium carbonate obtained by the present embodiment are determined
The concentration of seminal fluid is 5.12mol/L.
To contain in lithium concentrate input reactor, be 1.4 according to the mol ratio of sodium carbonate and lithium：2, the present embodiment is made
Standby sodium carbonate seminal fluid is added in reactor, hybrid reaction, and in the course of reaction of reaction solution, the stir speed (S.S.) of reaction solution sets
It is set to 60r/min, reaction temperature is 40 DEG C, persistently terminates reaction after 30min altogether.This step generates lithium carbonate in a kettle.
Precipitation.
Step S3 postorder treatment process：
Material in step S2 reactors is transferred in crystallization kettle, material is heated, with the increase of temperature of charge, knot
Crystalline solid in brilliant kettle gradually increases, after material is warming up to 85 DEG C, to the material in crystallization kettle by the way of centrifugation
Separated.
The solid material isolated using filtering and washing is carried out without ion desalted water, is then inputted pneumatic conveying drying first
It is dried in tower, then makes to be dried in its input fluid bed again, Two stage dryer temperature is disposed as 115 DEG C.Last thing
Material is exported from fluid bed, and natural cooling obtains final product the final product lithium carbonate product prepared by the present embodiment.
The liquid material isolated is played back to salt pan after its pH is adjusted into 6.0 using hydrochloric acid.
In the lithium carbonate product that the present embodiment is produced, the content of lithium carbonate is 99.34%, and impurity content is as follows：Na2O
Mass fraction be 0.081%, Fe2O3Mass fraction for 0.0004%, CaO mass fraction be 0.0437%, SO4 2-Matter
Amount fraction is 0.011, Cl-Mass fraction be 0.04%, H2The mass fraction of O is 0.099%, the quality point of hydrochloric acid insoluble substance
Number is 0.0214% for the mass fraction of 0.001%, MgO.It is computed, yield 80% of the present embodiment to lithium carbonate.
Example IV
Each step in the present embodiment is identical with embodiment three, and simply in the present embodiment, sodium carbonate material is used not
It is the accessory substance washing soda crystal during urea method production biruea, but soda ash solution, therefore omit to accessory substance
Process step a2~the c2 of washing soda, directly makes soda ash solution and the hybrid reaction of concentrate containing lithium.
In the lithium carbonate product that the present embodiment is produced, the mass fraction of lithium carbonate is 99.15%, and impurity content is as follows：
Na2The mass fraction of O is 0.1047%, Fe2O3Mass fraction for 0, CaO mass fraction be 0.0307, SO4 2-Quality point
Number is 0.0018, Cl-Mass fraction be 0.1027%, H2The mass fraction of O is 0.08%, the mass fraction of hydrochloric acid insoluble substance
The mass fraction for being 0.042%, MgO is 0.0331%.
Embodiment five
Step S1 removal of impurities enrichment process：
Step a1：By in salt lake bittern adsorption-desorption device of the feeding equipped with lithium adsorbent so that salt lake bittern is passed through successively
Absorption, drip washing and desorption manipulation are crossed, lithium desorption liquid is obtained.Lithium concentration in the lithium desorption liquid is 0.5g/L, and magnesium ion is dense
It is 1.0g/L to spend, and Na ion concentration is 0.4g/L, and chlorine ion concentration is 3.3g/L.
Step b1：Make above-mentioned lithium desorption liquid by calcium and magnesium polymeric adsorbent, so as to remove the magnesium ion in lithium desorption liquid so that
The magnesium ion concentration of lithium desorption liquid is 0.015mg/L, obtains removal of impurities liquid.
Step c1：Removal of impurities liquid is realized using reverse osmosis concentration method concentrating, obtain one section of lithium concentrate, one section of lithium concentration
Lithium concentration in liquid is 4.5g/L, and afterwards, continuation uses evaporating and concentrating process to one section of lithium concentrate, so as to obtain this implementation
Concentrate containing lithium in example, the lithium concentration for containing lithium concentrate is 23g/L.
Step S2 carbonization sinker operations：
Washing soda is processed first, process step is as follows：
Step a2：The accessory substance washing soda that urea method is produced during biruea is placed in dissolving tank, is used
Steam-heated mode causes that washing soda crystal all dissolves, and forms sodium carbonate liquor, during heating, controls molten
Temperature of charge in solution groove is 35 DEG C.
Step b2：The sodium carbonate liquor in step a2 is set to realize removal of impurities by millipore filter, filter pressure is set as
0.08MPa, to remove the cotton-shaped crystal of the magnesium hydroxide in sodium carbonate liquor and mechanical admixture, so that be obtained can be former as lithium carbonate
The sodium carbonate seminal fluid of material.
To sodium carbonate semen sample, the carbonate content in sodium carbonate seminal fluid, the sodium carbonate obtained by the present embodiment are determined
The concentration of seminal fluid is 5.21mol/L.
To contain in lithium concentrate input reactor, be 1.6 according to the mol ratio of sodium carbonate and lithium：2, the present embodiment is made
Standby sodium carbonate seminal fluid is added in reactor, hybrid reaction, and in the course of reaction of reaction solution, the stir speed (S.S.) of reaction solution sets
It is set to 45r/min, reaction temperature is 35 DEG C, persistently terminates reaction after 30min altogether.This step generates lithium carbonate in a kettle.
Precipitation.
Step S3 postorder treatment process：
Material in step S2 reactors is transferred in crystallization kettle, material is heated, with the increase of temperature of charge, knot
Crystalline solid in brilliant kettle gradually increases, after material is warming up to 80 DEG C, to the material in crystallization kettle by the way of centrifugation
Separated.
The solid material isolated using filtering and washing is carried out without ion desalted water, is then inputted pneumatic conveying drying first
It is dried in tower, then makes to be dried in its input fluid bed again, Two stage dryer temperature is disposed as 120 DEG C.Last thing
Material is exported from fluid bed, and natural cooling obtains final product the final product lithium carbonate product prepared by the present embodiment.
The liquid material isolated is played back to salt pan after its pH is adjusted into 6.5 using hydrochloric acid.
In the lithium carbonate product that the present embodiment is produced, the content of lithium carbonate is 99.26%, and impurity content is as follows：Na2O
Mass fraction be 0.0618%, Fe2O3Mass fraction for 0.0004%, CaO mass fraction be 0.0821%, SO4 2-'s
Mass fraction is 0, Cl-Mass fraction be 0.014%, H2The mass fraction of O is 0.04%, the mass fraction of hydrochloric acid insoluble substance
The mass fraction for being 0.003%, MgO is 0.0193%.It is computed, yield 77% of the present embodiment to lithium carbonate.
Embodiment six
Each step in the present embodiment is identical with embodiment five, and simply in the present embodiment, sodium carbonate material is used not
It is the accessory substance washing soda crystal during urea method production biruea, but soda ash solution, therefore omit to accessory substance
Process step a2~the c2 of washing soda, directly makes soda ash solution and the hybrid reaction of concentrate containing lithium.
In the lithium carbonate product that the present embodiment is produced, the mass fraction of lithium carbonate is 99.22%, and impurity content is as follows：
Na2The mass fraction of O is 0.0788%, Fe2O3Mass fraction for 0, CaO mass fraction be 0.0339, SO4 2-Quality point
Number is 0.0081, Cl-Mass fraction be 0.0680%, H2The mass fraction of O is 0.07%, the mass fraction of hydrochloric acid insoluble substance
The mass fraction for being 0.039%, MgO is 0.0399%.
Table 1 lists the mass fraction (%) of each composition of product lithium carbonate in one~embodiment of embodiment six.
Table 1
In table 1, embodiment one, embodiment three, embodiment five are using the preparation technology institute of lithium carbonate of the present invention
The lithium carbonate product for preparing, embodiment two, example IV and embodiment six are as sodium carbonate material using soda ash solution
Preparation-obtained lithium carbonate product.Lithium carbonate purity in each lithium carbonate product in table 1 is contrasted, it is known that, using this
Carbonic acid lithium content in the preparation-obtained product of preparation technology of the described lithium carbonate of invention is apparently higher than using soda ash solution
As the carbonic acid lithium content in the preparation-obtained product of sodium carbonate material.Therefore, contrast and can draw by above-mentioned experimental result,
Quality using the lithium carbonate product obtained by the preparation technology of lithium carbonate of the present invention is higher.
Why there is the effect above, be using right in accessory substance washing soda crystal, the present invention with raw material of the invention
The process step and reaction treatment step of washing soda are relevant.First, due to using soda ash solution as sodium carbonate thing
Expect to prepare during lithium carbonate, soda ash is in production, although the magnesium chloride to being brought into from raw material sodium chloride is processed, but residual
The micro magnesium chloride deposited can form the form of magnesium bicarbonate, and through the calcination process during soda manufacture after, be converted into carbonic acid
The form of magnesium is present, and when soda ash solution to be applied the preparation section in lithium carbonate, the magnesium carbonate that it contains will enter carbonic acid
In lithium finished product, and it is converted into the form of magnesia in later stage treatment process and exists.And use lithium carbonate of the present invention
Preparation technology when, accessory substance washing soda crystal is first processed, then just carried out as sodium carbonate material
Utilize, due to producing the process of biruea in urea method, magnesium ion is present in the form of magnesium hydroxide, and the present invention is to by-product
In the processing procedure of thing washing soda, removal of impurities is carried out to it using millipore filter, so as to remove washing soda crystal
A large amount of magnesium hydroxides in the sodium carbonate liquor of formation.Second, soda ash in process of production from raw material sodium chloride bring into it is micro
Silicon compound can be partially converted into the sodium metasilicate hydrotrope, so that can enter in final product lithium carbonate product, and the present invention is used
Sodium carbonate material be the accessory substance washing soda existed in Crystallization during urea method production biruea, it is to avoid silicon
The presence of element compound.3rd, during production, raw material sodium chloride can bring micro sodium sulphate into soda ash, so as to lead
There is the presence of sulfate radical in the lithium carbonate product that ultimately forms of cause, and the by-product in crystal form presence that the present invention is directly used
Thing washing soda, so that being substantially free of sulfate radical in raw material.Drawn based on above-mentioned analysis and embodiment result, this
The preparation technology of the described lithium carbonate of invention can prepare high-quality lithium carbonate product, and be significantly higher than industrial lithium carbonate matter
The national standard of amount, the utilization beneficial to the later stage to lithium carbonate.
It should be noted that above-described embodiment the present invention will be described rather than limiting the invention, and this
Art personnel can design alternative embodiment without departing from the scope of the appended claims.In claim
In, any reference symbol being located between bracket should not be configured to limitations on claims.Word "comprising" is not excluded for depositing
In element or step not listed in the claims.
Claims (10)
1. a kind of preparation technology of lithium carbonate, it is characterised in that comprise the following steps：
Step S1 removal of impurities enrichment process：
After salt lake bittern removal of impurities is concentrated, concentrate containing lithium is formed；
Step S2 carbonization sinker operations：
Reaction solution is formed to addition sodium carbonate material in the concentrate containing lithium, during reaction original state, carbon in the reaction solution
Sour sodium is 1.2~1.6 with the mol ratio of lithium：2, it is reacted after, in the reaction solution generate lithium carbonate precipitation,
Wherein, the sodium carbonate material is the accessory substance washing soda crystal during urea method production biruea；
Step S3 postorder treatment process：
The lithium carbonate precipitation is isolated, final product lithium carbonate product is obtained after scrubbed, drying.
2. the preparation technology of lithium carbonate according to claim 1, it is characterised in that the step S1 removal of impurities enrichment process bag
Include following steps：
Step a1：By in salt lake bittern adsorption-desorption device of the feeding equipped with lithium adsorbent, by absorption, drip washing and de-
Attached operation, is obtained lithium desorption liquid；
Step b1：Magnesium ion in the lithium desorption liquid is removed by cationic ion-exchange resin, removal of impurities liquid is obtained；
Step c1：The removal of impurities liquid is realized to concentrate using reverse osmosis concentration operation and evaporation and concentration operation, is formed containing lithium concentration
Liquid.
3. the preparation technology of lithium carbonate according to claim 1 and 2, it is characterised in that concentrated containing lithium described in step S1
The lithium concentration of liquid is 20~25g/L.
4. the preparation technology of lithium carbonate according to claim 1, it is characterised in that in the step S2 carbonizations sinker operation
Sodium carbonate material be that, through the sodium carbonate seminal fluid after treatment, the treatment process of the sodium carbonate material comprises the following steps：
Step a2：By the sodium carbonate material be urea method production biruea during accessory substance washing soda be placed on it is molten
In solution groove, dissolve it by heating complete, sodium carbonate liquor is obtained；
Step b2：The sodium carbonate liquor is set to realize removal of impurities by millipore filter, filter pressure is 0.05~0.1MPa, is obtained
Sodium carbonate seminal fluid.
5. the preparation technology of lithium carbonate according to claim 4, it is characterised in that sodium carbonate liquor described in step a2
Heating-up temperature is 30~40 DEG C.
6. the preparation technology of lithium carbonate according to claim 1, it is characterised in that in step S2 carbonization sinker operations, institute
Reaction solution stir speed (S.S.) during the course of the reaction is stated for 30~60r/min, reaction temperature is 30~40 DEG C, and the reaction time continues 20
~40min.
7. the preparation technology of lithium carbonate according to claim 1, it is characterised in that in step S2 carbonization sinker operations, instead
When answering original state, sodium carbonate and the mol ratio of lithium are 1.4 in the reaction solution：2.
8. lithium carbonate preparation section according to claim 1, it is characterised in that described in step S3 postorder treatment process
Separate mode is crystallized to heat up, and the crystal solution temperature in the intensification crystallization mode rises to 75~85 DEG C.
9. lithium carbonate preparation section according to claim 8, it is characterised in that the liquid that the intensification crystallization mode is isolated
After body uses hydrochloric acid to be neutralized to pH for 5.5~6.5, it is set to be played back to salt pan.
10. lithium carbonate preparation section according to claim 1, it is characterised in that the institute in step S3 subsequent treatment operations
Mode of washing is stated for filtering and washing, the drying mode is that pneumatic conveying drying and fluidized drying merge utilization.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500318A (en) * | 2017-09-26 | 2017-12-22 | 马海军 | The method that lithium carbonate is extracted from aluminum oxide factory sodium aluminate solution |
| CN108217701A (en) * | 2018-04-11 | 2018-06-29 | 宜春市鼎鑫高能科技有限公司 | A kind of lithium carbonate process units |
| CN111470521A (en) * | 2020-05-25 | 2020-07-31 | 中国地质科学院矿产资源研究所 | Method for extracting lithium from solar cell |
| US11524901B2 (en) * | 2019-03-22 | 2022-12-13 | Beijing University Of Chemical Technology | Method for efficiently separating magnesium and lithium from salt lake brine and simultaneously preparing high-purity magnesium oxide and battery-grade lithium carbonate |
| WO2023051728A1 (en) * | 2021-09-30 | 2023-04-06 | 比亚迪股份有限公司 | Method for recovering lithium from lithium-containing solution |
Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1106358A (en) * | 1994-02-04 | 1995-08-09 | 地质矿产部西藏自治区中心实验室 | Method for extracting lithium salt from brine |
| CN1335262A (en) * | 2001-09-07 | 2002-02-13 | 中信国安锂业科技有限责任公司 | Lithium carbonate preparing process from salt lake bittern with high Mg/Li ratio |
| CN101007642A (en) * | 2007-01-10 | 2007-08-01 | 青海省地质调查院 | Preparation method of lithium carbonate by using brine of oil field |
| CN101691239A (en) * | 2009-09-30 | 2010-04-07 | 达州市恒成能源（集团）有限责任公司 | Comprehensive utilization method for bittern |
| CN102275956A (en) * | 2011-07-21 | 2011-12-14 | 清华大学 | Method for extracting lithium carbonate from salt lake brine with high magnesium/lithium ratio |
| CN102432046A (en) * | 2011-09-26 | 2012-05-02 | 江苏海龙锂业科技有限公司 | Utilization method of chloride type salt lake brine |
| CN102774860A (en) * | 2012-08-22 | 2012-11-14 | 东莞市广华化工有限公司 | Method for preparing lithium carbonate by brine |
| CN102976367A (en) * | 2012-12-20 | 2013-03-20 | 青海锂业有限公司 | Method for preparing battery-level lithium carbonate by using salt lake brine |
| CN102992358A (en) * | 2012-02-24 | 2013-03-27 | 中国科学院青海盐湖研究所 | Method for extracting lithium salt from lithium brine |
| CN103449481A (en) * | 2012-05-29 | 2013-12-18 | 日铁矿业株式会社 | Preparation method of lithium carbonate |
| CN103708508A (en) * | 2014-01-17 | 2014-04-09 | 长沙有色冶金设计研究院有限公司 | Method for producing cell-grade lithium carbonate from lithium concentrate |
| CN103898341A (en) * | 2014-03-06 | 2014-07-02 | 中国科学院青海盐湖研究所 | Method for separating and extracting lithium from lithium sulfate coarse ore |
| CN104030324A (en) * | 2014-06-06 | 2014-09-10 | 无锡市崇安区科技创业服务中心 | Method for extracting lithium carbonate from salt lake brine |
| CN105036159A (en) * | 2015-07-23 | 2015-11-11 | 韦海棉 | Method for preparing lithium carbonate with high-lithium salt lake bittern |
| CN105152191A (en) * | 2015-10-28 | 2015-12-16 | 中国科学院青海盐湖研究所 | Method for preparing lithium carbonate through salt lake brine with high ratio of magnesium to lithium |
| CN106241841A (en) * | 2016-08-29 | 2016-12-21 | 江苏海普功能材料有限公司 | A kind of salt lake bittern prepares the method for lithium carbonate |
-
2017
- 2017-01-17 CN CN201710041119.7A patent/CN106745102B/en active Active
Patent Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1106358A (en) * | 1994-02-04 | 1995-08-09 | 地质矿产部西藏自治区中心实验室 | Method for extracting lithium salt from brine |
| CN1335262A (en) * | 2001-09-07 | 2002-02-13 | 中信国安锂业科技有限责任公司 | Lithium carbonate preparing process from salt lake bittern with high Mg/Li ratio |
| CN101007642A (en) * | 2007-01-10 | 2007-08-01 | 青海省地质调查院 | Preparation method of lithium carbonate by using brine of oil field |
| CN101691239A (en) * | 2009-09-30 | 2010-04-07 | 达州市恒成能源（集团）有限责任公司 | Comprehensive utilization method for bittern |
| CN102275956A (en) * | 2011-07-21 | 2011-12-14 | 清华大学 | Method for extracting lithium carbonate from salt lake brine with high magnesium/lithium ratio |
| CN102432046A (en) * | 2011-09-26 | 2012-05-02 | 江苏海龙锂业科技有限公司 | Utilization method of chloride type salt lake brine |
| CN102992358A (en) * | 2012-02-24 | 2013-03-27 | 中国科学院青海盐湖研究所 | Method for extracting lithium salt from lithium brine |
| CN103449481A (en) * | 2012-05-29 | 2013-12-18 | 日铁矿业株式会社 | Preparation method of lithium carbonate |
| CN102774860A (en) * | 2012-08-22 | 2012-11-14 | 东莞市广华化工有限公司 | Method for preparing lithium carbonate by brine |
| CN102976367A (en) * | 2012-12-20 | 2013-03-20 | 青海锂业有限公司 | Method for preparing battery-level lithium carbonate by using salt lake brine |
| CN103708508A (en) * | 2014-01-17 | 2014-04-09 | 长沙有色冶金设计研究院有限公司 | Method for producing cell-grade lithium carbonate from lithium concentrate |
| CN103898341A (en) * | 2014-03-06 | 2014-07-02 | 中国科学院青海盐湖研究所 | Method for separating and extracting lithium from lithium sulfate coarse ore |
| CN104030324A (en) * | 2014-06-06 | 2014-09-10 | 无锡市崇安区科技创业服务中心 | Method for extracting lithium carbonate from salt lake brine |
| CN105036159A (en) * | 2015-07-23 | 2015-11-11 | 韦海棉 | Method for preparing lithium carbonate with high-lithium salt lake bittern |
| CN105152191A (en) * | 2015-10-28 | 2015-12-16 | 中国科学院青海盐湖研究所 | Method for preparing lithium carbonate through salt lake brine with high ratio of magnesium to lithium |
| CN106241841A (en) * | 2016-08-29 | 2016-12-21 | 江苏海普功能材料有限公司 | A kind of salt lake bittern prepares the method for lithium carbonate |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500318A (en) * | 2017-09-26 | 2017-12-22 | 马海军 | The method that lithium carbonate is extracted from aluminum oxide factory sodium aluminate solution |
| CN108217701A (en) * | 2018-04-11 | 2018-06-29 | 宜春市鼎鑫高能科技有限公司 | A kind of lithium carbonate process units |
| US11524901B2 (en) * | 2019-03-22 | 2022-12-13 | Beijing University Of Chemical Technology | Method for efficiently separating magnesium and lithium from salt lake brine and simultaneously preparing high-purity magnesium oxide and battery-grade lithium carbonate |
| CN111470521A (en) * | 2020-05-25 | 2020-07-31 | 中国地质科学院矿产资源研究所 | Method for extracting lithium from solar cell |
| WO2023051728A1 (en) * | 2021-09-30 | 2023-04-06 | 比亚迪股份有限公司 | Method for recovering lithium from lithium-containing solution |
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