CN107416869A - A kind of production line that lithium carbonate is extracted from lepidolite ore - Google Patents
A kind of production line that lithium carbonate is extracted from lepidolite ore Download PDFInfo
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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
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Abstract
The present invention relates to a kind of production line that lithium carbonate is extracted from lepidolite ore, including acidolysis pool unit (100), first sedimentation pool unit (200), second sedimentation pool unit (300), 3rd sedimentation pool unit (400), 4th sedimentation pool unit (500), 5th sedimentation pool unit (600) and the 6th sedimentation pool unit (700), so that metal ion almost eliminates in addition to lithium ion in lepidolite leachate, it is eventually adding the lithium carbonate that saturated sodium carbonate heating response can obtain high-purity, the production line energy consumption is low, requirement to equipment is low, impurity-eliminating effect is notable, it is adapted to the lithium carbonate preparation technology popularization and application using lepidolite as raw material.
Description
Technical field
The present invention relates to a kind of method and production line that lithium carbonate is extracted from lepidolite ore, belongs to the preparation of lithium battery raw material
Field.
Background technology
Lepidolite is also known as " lepidolite ", main component KLi1.5Al1.5[AlSi3O10](F,OH)2, containing Li2O is about 1.23
~5.90%, also containing other rare metals such as rubidium, caesium；Wherein Yichun City stores lepidolite ore the biggest in the world, lithia
Allowable exploitation accounts for 31%, the 8.2% of the world of the whole nation.Lepidolite is most common lithium minerals, is the important mineral for refining lithium, right
It, which carries out comprehensive development and utilization, has particularly significant economy and strategic value.
Lithium carbonate is a kind of important industrial chemicals, and with national new energy development plan, lithium electricity new energy turns into state
Family's emphasis supports one of development energy industry；And lithium carbonate develops important foundation raw material as lithium electricity new energy, it is in new energy
Importance in material also increasingly increases.
Technique of the tradition using lepidolite as raw material mainly has salt autoclaving method, basic pressure digestion method and sulfuric acid process, but these techniques
Substantial amounts of waste residue can be produced in production by, which having, (produces lithium carbonate per ton to produce more than waste residue about 30-40 tons, these " waste residues " are main
Want the mixture and substantial amounts of gypsum and a small amount of iron oxide etc. that composition is silica and aluminum oxide, the yield of lithium is low (about
60%), and severe reaction conditions, the defects of equipment heavy corrosion is easily caused, production cost is on the one hand significantly increased, constrains
The possibility of large-scale production, serious environmental pollution is on the other hand caused, and, valuable gold in lepidolite incomplete due to reacting
The leaching rate of category is not high, and utilization rate of raw materials is low, and technique added value is low.
Using ore as raw material, mainly with lepidolite, spodumene is that raw material is extracted, and current extracting method is sulfuric acid
Method or potassium sulfate and limestone calcination connection, because limestone calcination method is by the way of high-temperature calcination, temperature is typically at 1000 DEG C
Left and right, thus energy resource consumption is high, material circulation is big, and the lithium rate of recovery is low, and product cost is high, and sulfuric acid process is using the concentrated sulfuric acid and lithium cloud
Female ore deposit high-temperature roasting, carbonate sinker, same high energy consumption, and environmental pollution are influenceed greatly, if China Patent No. is ZL85101989
《Potassium sulfate method processing lepidolite produces potassium carbonate processes method》It is to carry out height after mixing potassium sulfate and lepidolite by proportioning
Temperature roasting, in 930 DEG C of temperature calcinations 2 hours, two sections of level Four extracting technologies extraction lithium carbonate products are then carried out to roasting material,
This method is still that energy waste is very big using high-temperature roasting technique, and certain pollution is also resulted in environment, also just like Chinese patent Shen
Please number be 201010001287.1《A kind of method that lithium is extracted from lepidolite》It is using lepidolite as raw material, is still using forging
Burning mode extraction process, energy waste is big, and equipment investment is big, three waste discharge, and the discharge of particularly waste gas is larger, and environment is caused
Larger pressure.
Therefore, because existing lepidolite production technology has cost height, make a low multiple use, equipment corrosion is serious.For
The comprehensive utilization of lepidolite is really realized, it is necessary to explore the new production method and production line that lithium carbonate is extracted by lepidolite.
The content of the invention
In order to overcome the not high technical deficiency of the purity for the lithium carbonate being prepared in the prior art from lepidolite, this hair
It is bright provide it is a kind of from lepidolite ore extract lithium carbonate production line, the production line by sulfuric acid reaction, low temperature sink rubidium caesium and
The functional units such as calcium hydroxide removal of impurities, sodium carbonate removal of impurities so that metal ion almost eliminates in lepidolite leachate, is eventually adding
Saturated sodium carbonate heating response is that can obtain the lithium carbonate product of high-purity, and the production line energy consumption is low, and the requirement to equipment is low, removes
Miscellaneous significant effect, it is adapted to the lithium carbonate preparation technology popularization and application using lepidolite as raw material.
The present invention is achieved through the following technical solutions above-mentioned technique effect：
A kind of production line that lithium carbonate is extracted from lepidolite ore, including following functional unit：
1) acidolysis pool unit, including closed acidolysis pond body, primary heater, the first filter and exhaust apparatus, institute
Primary heater is stated in the middle part of acidolysis pond body or bottom, first filter are arranged on the bottom of acidolysis pond body side
Portion, the exhaust apparatus are arranged on the top of acidolysis pond body；
2) the first sedimentation pool unit, including the first sedimentation pond body, the first agitator, the first condenser and the second filtering dress
Put, first agitator is arranged on the middle part or bottom of the first sedimentation pond body, and first condenser is arranged on the first sedimentation
The bottom of pond body, second filter are arranged on the bottom of the first sedimentation pond body side；
3) the second sedimentation pool unit, including the second sedimentation pond body, the second agitator, the second condenser and the 3rd filtering dress
Put, second agitator is arranged on the middle part or bottom of the second sedimentation pond body, and second condenser is arranged on the second sedimentation
The bottom of pond body, the 3rd filter are arranged on the bottom of the second sedimentation pond body side；
4) the 3rd sedimentation pool unit, including the 3rd sedimentation pond body and the 4th filter, the 4th filter are arranged on the
The bottom of three sedimentation pond body sides；
5) the 4th sedimentation pool unit, including the 4th sedimentation pond body and the 5th filter, the 5th filter are arranged on the
The bottom of four sedimentation pond body sides；
6) the 5th sedimentation pool unit, including the 5th sedimentation pond body and the 6th filter, the 6th filter are arranged on the
The bottom of five sedimentation pond body sides；
7) the 6th sedimentation pool unit, including the 6th sedimentation pond body, secondary heater, the 3rd agitator and the 7th filtering dress
Put, the secondary heater is arranged in the middle part of the 6th sedimentation pond body or bottom, the 3rd agitator are arranged on the 6th sedimentation pond body
Middle part or bottom, the 7th filter are arranged on the bottom of the 6th sedimentation pond body side；
The acidolysis pool unit, the first sedimentation pool unit, the second sedimentation pool unit, the 3rd sedimentation pool unit, the 4th sedimentation
Pool unit, the 5th sedimentation pool unit and the 6th sedimentation pool unit are sequentially connected, in addition to the filtrate (liquid of the 6th sedimentation pool unit, its
The filtrate (liquid of his each unit corresponds to the filtrate import of next unit.
Further, the concentrated sulfuric acid of the fine grain lepidolite of the mesh of 200 mesh -400 with 85% in acidolysis pond body is milled to mix,
Primary heater starts heating mixture to 150 DEG C -180 DEG C, lepidolite is fully reacted 15-20min with the concentrated sulfuric acid, has reacted
Into rear startup the first filter filtering, silica and the fluorine element of the overwhelming majority are removed, filtrate enters the first settling tank list
Member.
Further, by first settle pool unit in solution the first agitator stirring under it is per minute according to cooling rate
2.0 DEG C -2.3 DEG C of cooling, 18 DEG C to 20 DEG C are down to, are incubated 20-30min, started the second filter, be filtered to remove rubidium cesium alum,
Filtrate enters the second sedimentation pool unit.
Further, settle solution in pool unit by second and be down to 3 DEG C to 7 DEG C according to 0.5 DEG C -0.7 DEG C of cooling per minute,
Start the 3rd filter after being incubated 15-20min, be filtered to remove arcanite, filtrate enters the 3rd sedimentation pool unit.
Further, aqua calcis, regulation pH value of solution to 7- are slowly added into the solution of the 3rd sedimentation pool unit
8, start the 4th filter, be filtered to remove calcirm-fluoride, filtrate enters the 4th sedimentation pool unit.
Further, aqua calcis is added into the solution of the 4th sedimentation pool unit, regulation pH value of solution to 11-12,
Start the 5th filter, remove ferro element and aluminium element, filtrate enters the 5th sedimentation pool unit.
Further, at room temperature, saturated sodium carbonate solution is added to without precipitation into the solution of the 5th sedimentation pool unit
Generation, start the 6th filter, be filtered to remove calcium constituent, filtrate enters the 6th sedimentation pool unit.
Further, the solution of the 6th sedimentation pool unit is concentrated into lithium concentration in 25-35g/L, startup second to add
Hot device, solution is heated to add saturated sodium carbonate solution in 85 DEG C -95 DEG C backward solution, starts the 3rd agitator, stirring is anti-
Start the 7th filter after answering 20-40min, filter while hot, obtain the lithium carbonate product of high-purity.
In production line of the present invention, it can be removed in acidolysis pool unit by lepidolite and concentrated sulfuric acid heating response in lepidolite
Silica and most of fluorine ion；Under conditions of heating, hydrofluoric acid volatilization is removed.First sedimentation unit and
Arcanite and rubidium cesium alum are removed by gradient cooling in two sedimentation units, be on the one hand because arcanite, rubidium cesium alum speed of separating out not
Together, on the other hand crossing conference when cooling rate causes part lithium salts loss.By adding in calcium hydroxide in 3rd sedimentation unit
With the fluorine ion that can remove residual, it is generated calcium fluoride precipitate and remove, calcium hydroxide is continuously added, in the solution that can make
Iron ion and the metal ion such as aluminium ion remove.Sodium carbonate is added in 6th sedimentation unit and removes excessive calcium ion, so
It is the lithium carbonate product that can obtain high-purity that concentration, which adds saturated sodium carbonate solution, afterwards.
The present invention also provides a kind of method that lithium carbonate is extracted from lepidolite ore, and it specifically comprises the following steps：
1) lepidolite is milled to the mesh fine grained of 200 mesh -400 using ball milling, it is mixed with 85% concentrated sulfuric acid, is heated to
150 DEG C -180 DEG C make it fully react 15-20min, are filtered after the completion of reaction, obtain solution A；
2) solution A is down to 18 DEG C to 20 DEG C under stirring according to cooling rate 2.0 DEG C -2.3 DEG C of cooling per minute,
20-30min is incubated, is filtered to remove rubidium caesium vanadium；Solution after filtering is down to 3 DEG C to 7 according to 0.5 DEG C -0.7 DEG C of cooling per minute
DEG C, potassium vanadium is filtered to remove after being incubated 15-20min, solution B is obtained, solution B is recovered to room temperature；
3) be slowly added to aqua calcis into solution B, regulation pH value of solution to 7-8, solution filtering, to filtering after solution
In continuously add aqua calcis adjust pH value of solution to 11-12, be filtrated to get solution C.
4) saturated sodium carbonate solution is added under room temperature condition into solution to generate to without precipitation, filtering, by solution after filtering
Lithium concentration is concentrated into 25-35g/L, solution is heated to 85 DEG C -95 DEG C, saturated sodium carbonate solution is added into solution,
Filtering can obtain the lithium carbonate product of high-purity while hot after stirring reaction 20-40min.
Preferably, in the method that lithium carbonate is extracted from lepidolite ore, lepidolite fine grained and 85% concentrated sulfuric acid
Mass mixing ratio be 1:2-4, more preferably 1:3.
Preferably, in the method that lithium carbonate is extracted from lepidolite ore, step 2) concretely comprises the following steps：By solution
A is down to 19 DEG C under stirring according to cooling rate 2.1 DEG C of cooling per minute, is incubated 25min, is filtered to remove rubidium caesium vanadium；Will
Solution is down to 5 DEG C according to 0.6 DEG C of cooling per minute after filtering, is filtered to remove potassium vanadium after being incubated 18min, solution B is obtained, by solution
B recovers to room temperature.
Preferably, in the method that lithium carbonate is extracted from lepidolite ore, aqua calcis in step 3)
Concentration is 3-5mol/L.
Preferably, in the method that lithium carbonate is extracted from lepidolite ore, specifically included in the step 4) as follows
Step：Saturated sodium carbonate solution is added into solution to generate to without precipitation, be filtered to remove calcium ion and other gold under room temperature condition
Belong to ion, solution is concentrated into lithium concentration in 30g/L, 90 DEG C will be heated in solution saturated sodium carbonate is added into solution
Solution, filter while hot after stirring reaction 30min.
Preferably, in the method that lithium carbonate is extracted from lepidolite ore, filtering refers to while hot in the step 4)
The temperature of solution is between 50 DEG C -70 DEG C during filtering.
The purity of the lithium carbonate prepared according to 1- of embodiment of the present invention embodiments 5 is high, and on 99.0%, yield exists
On 82%, this shows that process purity and yield of the present invention significantly improve compared with prior art, and Comparative Examples 1 by
In the cooling rate for changing rubidium caesium and potassium metal ion therein is removed not thorough, affect final product purity.
Comparative Examples 2 then by two sections cooling is changed to one section cooling so that final lithium carbonate product include more monovalent metal from
Son, product purity and yield have declined.Comparative Examples 3 are then due to changing the depositing technology of calcium hydroxide so that part
Fluorine ion is remained in finished product lithium carbonate, and product purity and elemental lithium yield decline.In preparation technology of the present invention,
The purity highest of lithium carbonate corresponding to embodiment 3 corresponding to technique, the yield of elemental lithium also highest, implements for the present invention is optimal
Example.
The production line and method of the present invention has technique effect prominent as follows relative to prior art：
1) present invention takes " two-step method " for the fluorine element in lepidolite ore, passes through first with the volatility of hydrofluoric acid
Adding strong acid makes hydrofluoric acid therein volatilize, then introduced in step 3) of the present invention calcium hydroxide make wherein to remain fluorine ion with
The form of calcium fluoride precipitate removes, and it is more preferable compared to the technique elimination effect of the existing fluorine removal from lepidolite, so as to improve
The quality of finished product lithium carbonate.
2) present invention has found in actual process, and the time that arcanite and rubidium cesium alum separate out in temperature-fall period is different, tradition
Precipitation technique in only with one section of falling temperature method make it that the precipitation of arcanite and rubidium cesium alum is ineffective, the present invention creatively makes
With two sections of cooling precipitation techniques, and control cooling rate this key parameter so that rubidium cesium alum and arcanite successively separate out, and its is right
Potassium element and rubidium cesium element remove more thorough in solution.
3) present invention removes bivalent metal ion therein by adding aqua calcis, then passes through saturated sodium carbonate
Solution removes calcium ion therein and remaining bivalent metal ion, so that follow-up processing operation is more prone to.
4) handling process processing method of the present invention is simple, and energy consumption consumption is low, and lithium is got rid of by suitable step
Impurity element in mica, its technological feasibility is strong, and the purity for the lithium carbonate being prepared is high, is adapted to prepare carbonic acid in lepidolite
Popularization and application in the production of lithium.
Brief description of the drawings
Fig. 1 is a kind of schematic diagram for the production line that lithium carbonate is extracted from lepidolite ore of the present invention.
Embodiment
Below by way of specific embodiment further describe the present invention, but the embodiment does not limit this in any way
The scope of invention patent protection.Lepidolite used in the following embodiments of the present invention originates from Jiangxi Province's Yichun City, and it is main
Chemical composition is as shown in table 1.
The chemical constituent analysis of the lepidolite ore of the present invention of table 1
| Li2O | K2O+Na2O | Al2O3 | SiO2 | Fe2O3 | Rb2O | Cs2O | F |
| 4.0% | 8.5% | 23.0% | 53.57% | 0.19% | 1.30% | 0.20% | 4.1% |
The production line that lithium carbonate is extracted from lepidolite ore of the present invention, as shown in figure 1, including acidolysis pool unit 100, the
It is heavy that one sedimentation pool unit 200, second settles the sedimentation sedimentation pool unit the 500, the 5th of pool unit the 400, the 4th of pool unit the 300, the 3rd
Drop pool unit 600 and the 6th and settle pool unit 700, specifically, include following functional unit：
1) acidolysis pool unit, including closed acidolysis pond body, primary heater, the first filter and exhaust apparatus, institute
Primary heater is stated in the middle part of acidolysis pond body or bottom, first filter are arranged on the bottom of acidolysis pond body side
Portion, the exhaust apparatus are arranged on the top of acidolysis pond body；
2) the first sedimentation pool unit, including the first sedimentation pond body, the first agitator, the first condenser and the second filtering dress
Put, first agitator is arranged on the middle part or bottom of the first sedimentation pond body, and first condenser is arranged on the first sedimentation
The bottom of pond body, second filter are arranged on the bottom of the first sedimentation pond body side；
3) the second sedimentation pool unit, including the second sedimentation pond body, the second agitator, the second condenser and the 3rd filtering dress
Put, second agitator is arranged on the middle part or bottom of the second sedimentation pond body, and second condenser is arranged on the second sedimentation
The bottom of pond body, the 3rd filter are arranged on the bottom of the second sedimentation pond body side；
4) the 3rd sedimentation pool unit, including the 3rd sedimentation pond body and the 4th filter, the 4th filter are arranged on the
The bottom of three sedimentation pond body sides；
5) the 4th sedimentation pool unit, including the 4th sedimentation pond body and the 5th filter, the 5th filter are arranged on the
The bottom of four sedimentation pond body sides；
6) the 5th sedimentation pool unit, including the 5th sedimentation pond body and the 6th filter, the 6th filter are arranged on the
The bottom of five sedimentation pond body sides；
7) the 6th sedimentation pool unit, including the 6th sedimentation pond body, secondary heater, the 3rd agitator and the 7th filtering dress
Put, the secondary heater is arranged in the middle part of the 6th sedimentation pond body or bottom, the 3rd agitator are arranged on the 6th sedimentation pond body
Middle part or bottom, the 7th filter are arranged on the bottom of the 6th sedimentation pond body side；
The acidolysis pool unit, the first sedimentation pool unit, the second sedimentation pool unit, the 3rd sedimentation pool unit, the 4th sedimentation
Pool unit, the 5th sedimentation pool unit and the 6th sedimentation pool unit are sequentially connected, in addition to the filtrate (liquid of the 6th sedimentation pool unit, its
The filtrate (liquid of his each unit corresponds to the filtrate import of next unit.
The present invention also provides the several embodiments and reference example for the method that lithium carbonate is extracted from lepidolite ore.
The method that the present invention of embodiment 1 extracts lithium carbonate from lepidolite ore
A kind of method that lithium carbonate is extracted from lepidolite ore, it specifically comprises the following steps：
1) lepidolite is milled to 400 mesh fine graineds using ball milling, it is mixed with 85% concentrated sulfuric acid, is heated to 180 DEG C
It is fully reacted 20min, filtered after the completion of reaction, obtain solution A；The wherein quality of lepidolite fine grained and 85% concentrated sulfuric acid
Mixing ratio is 1:3.5.
2) solution A is dropped to 18 DEG C under stirring according to cooling rate 2.3 DEG C of cooling per minute, filtering, by solution
3 DEG C are down to according to 0.7 DEG C of cooling per minute, precipitation is filtrated to get solution B, and solution B is recovered to room temperature；
3) aqua calcis is slowly added into solution B, regulation pH value of solution to 8, solution filtering, continues to add into solution
Enter aqua calcis and adjust pH value of solution to 12, be filtrated to get solution C.The concentration of wherein described aqua calcis is 3mol/
L。
4) saturated sodium carbonate solution is added under room temperature condition into solution to generate to without precipitation, filtering, by solution after filtering
Lithium concentration is concentrated into 35g/L, 95 DEG C will be heated in solution saturated sodium carbonate solution, stirring reaction is added into solution
Filtering can obtain the lithium carbonate product of high-purity while hot after 40min.The present invention of embodiment 2 extracts lithium carbonate from lepidolite ore
Method
A kind of method that lithium carbonate is extracted from lepidolite ore, it specifically comprises the following steps：
1) lepidolite is milled to 200 mesh fine graineds using ball milling, it is mixed with 85% concentrated sulfuric acid, is heated to 150 DEG C
It is fully reacted 15min, filtered after the completion of reaction, obtain solution A；The wherein quality of lepidolite fine grained and 85% concentrated sulfuric acid
Mixing ratio is 1:2.5.
2) solution A is down to 20 DEG C under stirring according to cooling rate 2.0 DEG C of cooling per minute, filtering, by solution
7 DEG C are down to according to 0.5 DEG C of cooling per minute, precipitation is filtrated to get solution B, and solution B is recovered to room temperature；
3) aqua calcis is slowly added into solution B, regulation pH value of solution to 7, solution filtering, continues to add into solution
Enter aqua calcis and adjust pH value of solution to 11, be filtrated to get solution C.The concentration of wherein described aqua calcis is 5mol/
L。
4) saturated sodium carbonate solution is added under room temperature condition into solution to generate to without precipitation, filtering, by solution after filtering
Lithium concentration is concentrated into 25g/L, 85 DEG C DEG C will be heated in solution saturated sodium carbonate solution is added into solution, stirring is anti-
The lithium carbonate product that can obtain high-purity is filtered while hot after answering 20min.
The method that the present invention of embodiment 3 extracts lithium carbonate from lepidolite ore
A kind of method that lithium carbonate is extracted from lepidolite ore, it specifically comprises the following steps：
1) lepidolite is milled to 300 mesh fine graineds using ball milling, it is mixed with 85% concentrated sulfuric acid, be heated to 150 DEG C-
180 DEG C make it fully react 18min, are filtered after the completion of reaction, obtain solution A；Wherein lepidolite fine grained and 85% concentrated sulfuric acid
Mass mixing ratio be 1:3.
2) solution A is down to 19 DEG C under stirring according to cooling rate 2.1 DEG C of cooling per minute, filtering, by solution
5 DEG C are down to according to 0.6 DEG C of cooling per minute, precipitation is filtrated to get solution B, and solution B is recovered to room temperature；
3) aqua calcis is slowly added into solution B, regulation pH value of solution to 7, solution filtering, continues to add into solution
Enter aqua calcis and adjust pH value of solution to 12, be filtrated to get solution C.The concentration of wherein described aqua calcis is 4mol/
L。
4) saturated sodium carbonate solution is added under room temperature condition into solution to generate to without precipitation, filtering, by solution after filtering
Lithium concentration is concentrated into 30g/L, 90 DEG C will be heated in solution saturated sodium carbonate solution, stirring reaction is added into solution
Filtering can obtain the lithium carbonate product of high-purity while hot after 30min.
The method that the present invention of embodiment 4 extracts lithium carbonate from lepidolite ore
A kind of method that lithium carbonate is extracted from lepidolite ore, it specifically comprises the following steps：
1) lepidolite is milled to 200 mesh fine graineds using ball milling, it is mixed with 85% concentrated sulfuric acid, is heated to 180 DEG C
It is fully reacted 15min, filtered after the completion of reaction, obtain solution A；The wherein quality of lepidolite fine grained and 85% concentrated sulfuric acid
Mixing ratio is 1:4.
2) solution A is down to 18 DEG C under stirring according to cooling rate 2.3 DEG C of cooling per minute, filtering, by solution
7 DEG C are down to according to 0.7 DEG C of cooling per minute, precipitation is filtrated to get solution B, and solution B is recovered to room temperature；
3) aqua calcis is slowly added into solution B, regulation pH value of solution to 8, solution filtering, continues to add into solution
Enter aqua calcis and adjust pH value of solution to 11, be filtrated to get solution C.The concentration of wherein described aqua calcis is 3mol/
L。
4) saturated sodium carbonate solution is added under room temperature condition into solution to generate to without precipitation, filtering, by solution after filtering
Lithium concentration is concentrated into 35g/L, 85 DEG C will be heated in solution saturated sodium carbonate solution, stirring reaction is added into solution
Filtering can obtain the lithium carbonate product of high-purity while hot after 40min.
The method that the present invention of embodiment 5 extracts lithium carbonate from lepidolite ore
A kind of method that lithium carbonate is extracted from lepidolite ore, it specifically comprises the following steps：
1) lepidolite is milled to 400 mesh fine graineds using ball milling, it is mixed with 85% concentrated sulfuric acid, is heated to 150 DEG C
It is fully reacted 20min, filtered after the completion of reaction, obtain solution A；The wherein quality of lepidolite fine grained and 85% concentrated sulfuric acid
Mixing ratio is 1:2.
2) solution A is down to 20 DEG C under stirring according to cooling rate 2.0 DEG C of cooling per minute, filtered, will be molten
Liquid is down to 3 DEG C according to 0.5 DEG C of cooling per minute, and precipitation is filtrated to get solution B, and solution B is recovered to room temperature；
3) aqua calcis is slowly added into solution B, regulation pH value of solution to 7, solution filtering, continues to add into solution
Enter aqua calcis and adjust pH value of solution to 12, be filtrated to get solution C.The concentration of wherein described aqua calcis is 5mol/
L。
4) saturated sodium carbonate solution is added under room temperature condition into solution to generate to without precipitation, filtering, by solution after filtering
Lithium concentration is concentrated into 25g/L, 95 DEG C will be heated in solution saturated sodium carbonate solution, stirring reaction is added into solution
Filtering can obtain the lithium carbonate product of high-purity while hot after 20min.
A kind of method that lithium carbonate is extracted from lepidolite ore of Comparative Examples 1
Except step 2) is：Solution A is down to 19 DEG C according to cooling rate 1 DEG C of cooling per minute under stirring, filtered,
Solution is down to 5 DEG C according to 1 DEG C of cooling per minute, precipitation is filtrated to get solution B, and solution B is recovered to room temperature；Remaining is the same as implementation
Example 3.
A kind of method that lithium carbonate is extracted from lepidolite ore of Comparative Examples 2
Except step 2) is：Solution A is down to 5 DEG C according to cooling rate 2.1 DEG C of cooling per minute under stirring, separated out
Solution B is filtrated to get, solution B is recovered to room temperature；Remaining is the same as embodiment 3.
Comparative Examples 3
Except step 3) is：Aqua calcis is slowly added into solution B, regulation pH value of solution is filtrated to get solution to 12
C.The concentration of wherein described aqua calcis is 4mol/L.Remaining is the same as embodiment 3.
Comparative examples prepare lithium carbonate according to the technique described in the A embodiments 1 of CN 101955211.
Comparative examples：
Lithium carbonate is prepared using lepidolite of the present invention, preparation technology is respectively according to embodiment 1-5, comparative example
1-3 and the preparation method described in comparative examples.Contrast the lithium carbonate purity that each technique is prepared, elemental lithium yield.It is right
It is more as shown in table 2 than result.
Purity and elemental lithium the yield contrast for the lithium carbonate that table 2 is prepared using different process
As can be seen from Table 2, the purity of the lithium carbonate prepared according to 1- of embodiment of the present invention embodiments 5 is high, exists
On 99.0%, for yield on 82%, this shows that process purity and yield of the present invention are notable compared with prior art
Improve, and Comparative Examples 1 make it that metal ion removing therein is not thorough due to changing the cooling rate of rubidium cesium alum and arcanite
Bottom, affect final product purity.Two sections of coolings are then changed to one section of cooling by Comparative Examples 2 so that final lithium carbonate
Product includes more monovalent metallic ion, and product purity and yield have declined.Comparative Examples 3 are then due to changing hydrogen-oxygen
Change the depositing technology of calcium so that part fluorine ion is remained in finished product lithium carbonate, and product purity and elemental lithium yield decline.
In preparation technology of the present invention, the purity highest of the lithium carbonate corresponding to embodiment 3 corresponding to technique, the yield of elemental lithium
Also highest, it is preferred embodiment.
Finally it should be noted that：The preferred embodiment of present invention described above, is not intended to limit the invention, although
The present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still can be right
Technical scheme described in foregoing embodiments is modified, or carries out equivalent substitution to which part technical characteristic.It is all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements made etc., the protection of the present invention should be included in
Within the scope of.
Claims (8)
- A kind of 1. production line that lithium carbonate is extracted from lepidolite ore, it is characterised in that：Including following functional unit：1) acidolysis pool unit (100), including closed acidolysis pond body, primary heater, the first filter and exhaust apparatus, institute Primary heater is stated in the middle part of acidolysis pond body or bottom, first filter are arranged on the bottom of acidolysis pond body side Portion, the exhaust apparatus are arranged on the top of acidolysis pond body；2) the first sedimentation pool unit (200), including the first sedimentation pond body, the first agitator, the first condenser and the second filtering dress Put, first agitator is arranged on the middle part or bottom of the first sedimentation pond body, and first condenser is arranged on the first sedimentation The bottom of pond body, second filter are arranged on the bottom of the first sedimentation pond body side；3) the second sedimentation pool unit (300), including the second sedimentation pond body, the second agitator, the second condenser and the 3rd filtering dress Put, second agitator is arranged on the middle part or bottom of the second sedimentation pond body, and second condenser is arranged on the second sedimentation The bottom of pond body, the 3rd filter are arranged on the bottom of the second sedimentation pond body side；4) the 3rd sedimentation pool unit (400), including the 3rd sedimentation pond body and the 4th filter, the 4th filter are arranged on the The bottom of three sedimentation pond body sides；5) the 4th sedimentation pool unit (500), including the 4th sedimentation pond body and the 5th filter, the 5th filter are arranged on the The bottom of four sedimentation pond body sides；6) the 5th sedimentation pool unit (600), including the 5th sedimentation pond body and the 6th filter, the 6th filter are arranged on the The bottom of five sedimentation pond body sides；7) the 6th sedimentation pool unit (700), including the 6th sedimentation pond body, secondary heater, the 3rd agitator and the 7th filtering dress Put, the secondary heater is arranged in the middle part of the 6th sedimentation pond body or bottom, the 3rd agitator are arranged on the 6th sedimentation pond body Middle part or bottom, the 7th filter are arranged on the bottom of the 6th sedimentation pond body side；The acidolysis pool unit (100), the first sedimentation pool unit (200), the second sedimentation pool unit (300), the 3rd settling tank list First (400), the 4th sedimentation pool unit (500), the 5th sedimentation pool unit (600) and the 6th sedimentation pool unit (700) are sequentially connected, In addition to the filtrate (liquid of the 6th sedimentation pool unit (700), the filtrate (liquid of other each units corresponds to the filter of next unit Liquid import.
- 2. the production line of extraction lithium carbonate as claimed in claim 1, it is characterised in that：It is fine grain to be milled to the mesh of 200 mesh -400 Lepidolite mixes in acidolysis pond body with 85% concentrated sulfuric acid, and primary heater starts heating mixture to 150 DEG C -180 DEG C, makes Lepidolite and the concentrated sulfuric acid fully react 15-20min, start the filtering of the first filter after the completion of reaction, remove silica and The fluorine element of the overwhelming majority, filtrate enter the first sedimentation pool unit (200).
- 3. the production line of extraction lithium carbonate as claimed in claim 1 or 2, it is characterised in that：By the first sedimentation pool unit (200) In solution under the stirring of the first agitator according to cooling rate 2.0 DEG C -2.3 DEG C of cooling per minute, be down to 18 DEG C to 20 DEG C, protect Warm 20-30min, start the second filter, be filtered to remove rubidium cesium alum, filtrate enters the second sedimentation pool unit (300).
- 4. the production line of the extraction lithium carbonate as described in claim 1-3 is any, it is characterised in that：Pool unit is settled by second (300) solution is down to 3 DEG C to 7 DEG C according to 0.5 DEG C -0.7 DEG C of cooling per minute in, starts the 3rd filtering dress after being incubated 15-20min Put, be filtered to remove arcanite, filtrate enters the 3rd sedimentation pool unit (400).
- 5. the production line of the extraction lithium carbonate as described in claim 1-4 is any, it is characterised in that：To the 3rd sedimentation pool unit (400) aqua calcis is slowly added in solution, regulation pH value of solution to 7-8, starts the 4th filter, is filtered to remove fluorine Change calcium, filtrate enters the 4th sedimentation pool unit (500).
- 6. the production line of the extraction lithium carbonate as described in claim 1-5 is any, it is characterised in that：To the 4th sedimentation pool unit (500) add aqua calcis in solution, regulation pH value of solution to 11-12, start the 5th filter, remove ferro element and Aluminium element, filtrate enter the 5th sedimentation pool unit (600).
- 7. the production line of the extraction lithium carbonate as described in claim 1-6 is any, it is characterised in that：At room temperature, it is heavy to the 5th Drop and saturated sodium carbonate solution is added in the solution of pool unit (600) to without precipitation generation, start the 6th filter, be filtered to remove Calcium constituent, filtrate enter the 6th sedimentation pool unit (700).
- 8. the production line of the extraction lithium carbonate as described in claim 1-7 is any, it is characterised in that：Pool unit is settled by the 6th (700) solution is concentrated into lithium concentration in 25-35g/L, startup secondary heater, after solution is heated into 85 DEG C -95 DEG C Saturated sodium carbonate solution is added into solution, starts the 3rd agitator, starts the 7th filter after stirring reaction 20-40min, Filter while hot, obtain the lithium carbonate product of high-purity.
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