CN110526265A - A kind of process for producing lithium carbonate with sulfuric acid process processing lepidolite - Google Patents
A kind of process for producing lithium carbonate with sulfuric acid process processing lepidolite Download PDFInfo
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- CN110526265A CN110526265A CN201910957847.1A CN201910957847A CN110526265A CN 110526265 A CN110526265 A CN 110526265A CN 201910957847 A CN201910957847 A CN 201910957847A CN 110526265 A CN110526265 A CN 110526265A
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- Prior art keywords
- sulfuric acid
- added
- lepidolite
- solution
- lithium carbonate
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 37
- 229910052629 lepidolite Inorganic materials 0.000 title claims abstract description 30
- 230000008569 process Effects 0.000 title claims abstract description 28
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 title claims abstract description 22
- 229910052808 lithium carbonate Inorganic materials 0.000 title claims abstract description 22
- 238000012545 processing Methods 0.000 title claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 230000020477 pH reduction Effects 0.000 claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 7
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 10
- 239000012141 concentrate Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000012452 mother liquor Substances 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000004913 activation Effects 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 235000015424 sodium Nutrition 0.000 claims description 5
- 239000001569 carbon dioxide Substances 0.000 claims description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229910052701 rubidium Inorganic materials 0.000 claims description 4
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 229910052792 caesium Inorganic materials 0.000 claims description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims 1
- 230000008020 evaporation Effects 0.000 claims 1
- 238000002386 leaching Methods 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 3
- 239000011707 mineral Substances 0.000 abstract description 3
- 239000003463 adsorbent Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000000505 pernicious effect Effects 0.000 abstract description 2
- 238000001238 wet grinding Methods 0.000 abstract description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 8
- 229910052744 lithium Inorganic materials 0.000 description 8
- 239000000706 filtrate Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 229910003002 lithium salt Inorganic materials 0.000 description 3
- 159000000002 lithium salts Chemical class 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- VHUJINUACVEASK-UHFFFAOYSA-J aluminum;cesium;disulfate;dodecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.[Al+3].[Cs+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VHUJINUACVEASK-UHFFFAOYSA-J 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241001131796 Botaurus stellaris Species 0.000 description 1
- KOPBYBDAPCDYFK-UHFFFAOYSA-N Cs2O Inorganic materials [O-2].[Cs+].[Cs+] KOPBYBDAPCDYFK-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- VQLYBLABXAHUDN-UHFFFAOYSA-N bis(4-fluorophenyl)-methyl-(1,2,4-triazol-1-ylmethyl)silane;methyl n-(1h-benzimidazol-2-yl)carbamate Chemical compound C1=CC=C2NC(NC(=O)OC)=NC2=C1.C=1C=C(F)C=CC=1[Si](C=1C=CC(F)=CC=1)(C)CN1C=NC=N1 VQLYBLABXAHUDN-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- AKUNKIJLSDQFLS-UHFFFAOYSA-M dicesium;hydroxide Chemical compound [OH-].[Cs+].[Cs+] AKUNKIJLSDQFLS-UHFFFAOYSA-M 0.000 description 1
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910001953 rubidium(I) oxide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001180 sulfating effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to mineral extractive technique fields, and in particular to a kind of process that lithium carbonate is produced with sulfuric acid process processing lepidolite.Method of the invention it has been found that passing through grinding for a long time by that polyethylene glycol progress wet grinding is added in lepidolite, can promote lepidolite to be modified, avoid high-temperature burning process in the prior art, can save mass energy, be conducive to environmental protection first；Fines after grinding uses ultrasonic wave added sulfuric acid leaching, shortens acidification extraction time, and material acidification is abundant.By the way that active carbon is added in leachate, active carbon has strong adsorption capacity, is added as adsorbent, can fail absorbed gaseous impurity produced by adsorption reaction, reduce the discharge of pernicious gas.
Description
Technical field
The present invention relates to mineral extractive technique fields, and in particular to a kind of to produce lithium carbonate with sulfuric acid process processing lepidolite
Process.
Background technique
Lithium is a kind of important mineral resources, and increasingly important role is played in development of human civilization.Currently, all kinds of
With annual 10% increasing rate, and in all lithium salts, the purposes of lithium carbonate is the most extensive for the consumption of lithium salts, and dosage is also most
Greatly.It is not only a kind of raw material that the industries such as ceramics, metallurgy, the energy, medicine largely use, and synthesizes the centre of other lithium salts
Raw material, therefore, the technology of preparing for studying lithium carbonate are of great significance.
The preparation process of lithium carbonate is broadly divided into ore and extracts and salt lake bittern extraction two major classes.Domestic production carbonic acid at present
Based on lithium is extracted with ore, yield accounts for about 70% or more of lithium carbonate production, lepidolite as one kind containing lithium ore,
It is often used in extracting lithium carbonate, and during lepidolite extracts lithium carbonate, there are the high temperature of calcination activation temperature, it usually needs
Reach 1000 DEG C~1200 DEG C or so, and contain a large amount of potassium and sodium in lepidolite, post-processing purifying process is complicated.
The Chinese patent literature of Publication No. CN107089673A discloses a kind of two sections of conversions of lithium ore and produces lithium carbonate
Method, after lithium ore powder is mixed with the concentrated sulfuric acid first, first under the conditions of 150~400 DEG C carry out low temperature sulfating roasting, so
Clinker is carried out to medium temperature reduction roasting at 550~900 DEG C afterwards, the method can reduce the maturing temperature of lithium ore to a certain degree,
But still remain the long defect of transformation time.
Summary of the invention
For the above-mentioned shortcoming of the prior art, carbonic acid is produced with sulfuric acid process processing lepidolite the invention proposes a kind of
The process of lithium carries out grinding activation to addition polyethylene glycol in lepidolite first, then uses ultrasonic wave added sulfuric acid leaching,
Lepidolite can be activated by needing not move through high-temperature calcination, and can significantly shorten the time that acidification is leached.
A kind of process for producing lithium carbonate with sulfuric acid process processing lepidolite of the present invention, comprising the following steps:
(1) grinding activation: the lepidolite of coarse crushing is taken, size controlling is in 80 mesh hereinafter, 2~3.5 times of lepidolite matter are added
2.5%~5% polyethylene glycol of above-mentioned slurry weight is added in slurry after slurrying by the water slurrying of amount, then by above-mentioned object
Material carries out the ultra-fine fine grinding of wet type and obtains finer abrasive a in 8~10 hours；
(2) ultrasonic wave acidification is leached: sulfuric acid solution being added into finer abrasive a, finer abrasive and sulfuric acid solution press quality 1:(3
~5) ratio is uniformly mixed, and is leached under conditions of ultrasonic wave, and setting ultrasonic power is 100W~150W, ultrasonic frequency
For 20KHz~28KHz, temperature is 70~100 DEG C, and extraction time is 10min~15min, and leachate b is collected by filtration；
(3) alkalization removal of impurities: NaOH solution is added into leachate b, pH value of solution is adjusted to 10~12, then again into solution
A small amount of active carbon is added, is stirred to react 10~30min and cleans, is filtered to obtain removal of impurities liquid c after the reaction was completed；
(4) it neutralizes concentration: dense H is added into removal of impurities liquid c2SO4, solution ph is adjusted to 6~7, is then evaporated solution dense
It is reduced to the 45%~55% of original solution volume, cooled to room temperature obtains concentrate d；
(5) secondary removal of impurities: concentrate d is refrigerated to -10 DEG C~10 DEG C precipitated sodiums, potassium, rubidium, cesium alums, is separated by filtration to obtain
Mother liquor e；
(6) sinker: being heated to 96 DEG C~100 DEG C for mother liquor e under stiring, be passed through carbon dioxide sinker reaction 60min~
100min generates white precipitate；The separation white precipitate, lithium carbonate obtained by drying.
Preferably, the concentration of step (2) described sulfuric acid is 35wt%~55wt%.
Preferably, the concentration of NaOH solution is 15wt%~25wt% in step (3).
Preferably, the additional amount of step (3) active carbon is 0.2 ‰~the 0.8 ‰ of solution quality.
Preferably, the drying condition of step (6) is dried in vacuo under the conditions of 70 DEG C~80 DEG C.
Compared with prior art, the invention has the advantages that method of the invention passes through first to poly- second is added in lepidolite
Glycol carries out wet grinding, it has been found that lepidolite can be promoted to be modified by grinding for a long time, avoids existing
Technology high temperature calcination process, can save mass energy, be conducive to environmental protection；Fines after grinding is soaked using ultrasonic wave added sulfuric acid
Out, acidification extraction time is shortened, and material acidification is abundant.By the way that active carbon is added in leachate, active carbon has strong
Adsorption capacity, be added as adsorbent, absorbed gaseous impurity can be failed produced by adsorption reaction, reduce pernicious gas
Discharge.
Specific embodiment
The invention discloses a kind of process that lithium carbonate is produced with sulfuric acid process processing lepidolite, those skilled in the art
Present disclosure can be used for reference, realization of process parameters is suitably modified.In particular, it should be pointed out that all similar substitutions and modifications pair
It is it will be apparent that they are considered as being included in the present invention for those skilled in the art.Method and application of the invention is
Through being described by preferred embodiment, related personnel obviously can not depart from the content of present invention, in spirit and scope to this
Methods and applications described in text are modified or appropriate changes and combinations, carry out implementation and application the technology of the present invention.
It is common commercially available product in supplementary material according to the present invention if not specified, can be bought and be obtained by market.
The present invention uses Yichuan Ta Nb tailings lepidolite, physicochemical property are as follows: appearance white；With glassy lustre or
Pearly luster；Flakey, relative density 2.8-2.9.The main component of chemical composition is as follows in lithium cloud:
| Li2O | K2O | Na2O | Al2O3 | SiO2 | Fe2O3 | Rb2O | Cs2O | F |
| 4.1% | 8.2% | 0.9% | 23.2% | 53.7% | 0.2% | 1.3% | 0.24% | 4.1% |
Embodiment 1:
Grinding activation: the lepidolite (size controlling is below 80 mesh) of 200g coarse crushing is weighed, 2 times of lepidolite quality are added
Water slurrying, the slurry after slurrying is added to 2.5% polyethylene glycol of above-mentioned slurry weight, then by above-mentioned material carry out exist
The ultra-fine fine grinding of wet type is carried out in ball mill obtains finer abrasive a within 8 hours；
Ultrasonic wave acidification is leached: the sulfuric acid solution that concentration is 35wt%, finer abrasive and sulfuric acid solution being added into finer abrasive a
It is uniformly mixed in quality 1:5 ratio, is leached under conditions of ultrasonic wave, setting ultrasonic power is 100W~150W, ultrasound
Wave frequency rate is 20KHz~28KHz, and temperature is 70 DEG C, extraction time 10min, be filtered to obtain after the completion of leaching residue and
Filtrate；Residue is washed with a small amount to be discarded afterwards twice, is merged water lotion and is obtained leachate b into filtrate；
Alkalization removal of impurities: the NaOH solution of 15wt% being added into leachate b, pH value of solution is adjusted to 10~12, then past again
0.2 ‰ active carbon of solution quality is added in solution, is stirred to react 10~30min and cleans, carried out after the reaction was completed
Filter obtains removal of impurities liquid c；
It neutralizes concentration: the H of 98wt% being added into removal of impurities liquid c2SO4, solution ph is adjusted to 6~7, then steams solution
Hair is concentrated into the 45%~55% of original solution volume, and cooled to room temperature obtains concentrate d；
Secondary removal of impurities: being refrigerated to -10 DEG C of precipitated sodiums, potassium, rubidium, cesium alum for concentrate d, is separated by filtration to obtain mother liquor e；
Sinker: being heated to 96 DEG C~100 DEG C for mother liquor e under stiring, is passed through the reaction of carbon dioxide sinker with 2 atmospheric pressure
60min~100min generates white precipitate；White precipitate described in end of reaction, filtering or centrifuge separation, reusable heat water is repeatedly
After washing, vacuum drying is under the conditions of 70 DEG C~80 DEG C up to lithium carbonate, product purity 99.94%.
Embodiment 2:
Grinding activation: the lepidolite (size controlling is below 80 mesh) of 200g coarse crushing is weighed, 3.5 times of lepidolite matter are added
5% polyethylene glycol of above-mentioned slurry weight is added, then by above-mentioned material in ball milling in slurry after slurrying by the water slurrying of amount
The ultra-fine fine grinding of wet type is carried out in machine obtains finer abrasive a within 10 hours；
Ultrasonic wave acidification is leached: the sulfuric acid solution that concentration is 55wt%, finer abrasive and sulfuric acid solution being added into finer abrasive a
It is uniformly mixed in quality 1:3 ratio, is leached under conditions of ultrasonic wave, setting ultrasonic power is 100W~150W, ultrasound
Wave frequency rate is 20KHz~28KHz, and temperature is 100 DEG C, extraction time 15min, be filtered to obtain after the completion of leaching residue and
Filtrate；Residue is washed with a small amount to be discarded afterwards twice, is merged water lotion and is obtained leachate b into filtrate；
Alkalization removal of impurities: the NaOH solution of 25wt% being added into leachate b, pH value of solution is adjusted to 10~12, then past again
0.8 ‰ active carbon of solution quality is added in solution, is stirred to react 10~30min and cleans, carried out after the reaction was completed
Filter obtains removal of impurities liquid c；
It neutralizes concentration: the H of 98wt% being added into removal of impurities liquid c2SO4, solution ph is adjusted to 6~7, then steams solution
Hair is concentrated into the 45%~55% of original solution volume, and cooled to room temperature obtains concentrate d；
Secondary removal of impurities: being refrigerated to -10 DEG C of precipitated sodiums, potassium, rubidium, cesium alum for concentrate d, is separated by filtration to obtain mother liquor e；
Sinker: being heated to 96 DEG C~100 DEG C for mother liquor e under stiring, is passed through the reaction of carbon dioxide sinker with 2 atmospheric pressure
60min~100min generates white precipitate；White precipitate described in end of reaction, filtering or centrifuge separation, reusable heat water is repeatedly
After washing, vacuum drying is under the conditions of 70 DEG C~80 DEG C up to lithium carbonate, product purity 99.95%.
The above case study on implementation is the present invention to be specifically described for example, technical staff belonging to the present invention can be with
Various concrete cases are modified or supplemented.
Claims (5)
1. a kind of process for producing lithium carbonate with sulfuric acid process processing lepidolite, which comprises the following steps:
(1) grinding activation: the lepidolite of coarse crushing is taken, size controlling is in 80 mesh hereinafter, 2~3.5 times of lepidolite quality are added
2.5%~5% polyethylene glycol of above-mentioned slurry weight is added in slurry after slurrying by water slurrying, then by above-mentioned material into
The ultra-fine fine grinding of row wet type obtains finer abrasive a in 8~10 hours；
(2) ultrasonic wave acidification is leached: sulfuric acid solution being added into finer abrasive a, finer abrasive and sulfuric acid solution press quality 1:(3~5)
Ratio is uniformly mixed, and is leached under conditions of ultrasonic wave, and setting ultrasonic power is 100W~150W, and ultrasonic frequency is
20KHz~28KHz, temperature are 70~100 DEG C, and extraction time is 10min~15min, and leachate b is collected by filtration；
(3) alkalization removal of impurities: NaOH solution is added into leachate b, pH value of solution is adjusted to 10~12, is then added again into solution
A small amount of active carbon, is stirred to react 10~30min and cleans, and is filtered to obtain removal of impurities liquid c after the reaction was completed；
(4) it neutralizes concentration: dense H is added into removal of impurities liquid c2SO4, solution ph is adjusted to 6~7, then by solution be concentrated by evaporation to
The 45%~55% of original solution volume, cooled to room temperature obtain concentrate d；
(5) secondary removal of impurities: concentrate d is refrigerated to -10 DEG C~10 DEG C precipitated sodiums, potassium, rubidium, cesium alums, is separated by filtration to obtain mother liquor
e；
(6) sinker: being heated to 96 DEG C~100 DEG C for mother liquor e under stiring, be passed through carbon dioxide sinker reaction 60min~
100min generates white precipitate；The separation white precipitate, lithium carbonate obtained by drying.
2. a kind of process for producing lithium carbonate with sulfuric acid process processing lepidolite according to claim 1, which is characterized in that
The concentration of step (2) described sulfuric acid is 35wt%~55wt%.
3. a kind of process for producing lithium carbonate with sulfuric acid process processing lepidolite according to claim 1, which is characterized in that
The concentration of NaOH solution is 15wt%~25wt% in step (3).
4. a kind of process for producing lithium carbonate with sulfuric acid process processing lepidolite according to claim 1, which is characterized in that
The additional amount of step (3) active carbon is 0.2 ‰~the 0.8 ‰ of solution quality.
5. a kind of process for producing lithium carbonate with sulfuric acid process processing lepidolite according to claim 1, which is characterized in that
The drying condition of step (6) is dried in vacuo under the conditions of 70 DEG C~80 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112645363A (en) * | 2020-12-31 | 2021-04-13 | 江西南氏锂电新材料有限公司 | Method for preparing battery-grade lithium carbonate by taking lepidolite as raw material |
| CN113955776A (en) * | 2021-12-02 | 2022-01-21 | 江苏容汇通用锂业股份有限公司 | Preparation method of lithium carbonate |
| CN116986836A (en) * | 2023-08-04 | 2023-11-03 | 江西永兴特钢新能源科技有限公司 | Lepidolite slag impurity removal modification method |
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| CN101955211A (en) * | 2010-10-29 | 2011-01-26 | 江西本源新材料科技有限公司 | Method for extracting lithium carbonate from lepidolite |
| CN102107888A (en) * | 2011-03-28 | 2011-06-29 | 江西本源新材料科技有限公司 | Method for preparing potassium sulphate |
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