CN106430260B - A kind of lepidolite prepares the preparation method of high-purity lithium carbonate - Google Patents
A kind of lepidolite prepares the preparation method of high-purity lithium carbonate Download PDFInfo
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- CN106430260B CN106430260B CN201611148616.9A CN201611148616A CN106430260B CN 106430260 B CN106430260 B CN 106430260B CN 201611148616 A CN201611148616 A CN 201611148616A CN 106430260 B CN106430260 B CN 106430260B
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- Prior art keywords
- chamber
- calcification
- lithium carbonate
- mouth
- lepidolite
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- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 title claims abstract description 32
- 229910052808 lithium carbonate Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910052629 lepidolite Inorganic materials 0.000 title claims abstract description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 230000002308 calcification Effects 0.000 claims abstract description 25
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 13
- 238000000605 extraction Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 235000007926 Craterellus fallax Nutrition 0.000 description 1
- 240000007175 Datura inoxia Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- YNQRWVCLAIUHHI-UHFFFAOYSA-L dilithium;oxalate Chemical compound [Li+].[Li+].[O-]C(=O)C([O-])=O YNQRWVCLAIUHHI-UHFFFAOYSA-L 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- GBPZIFLFRULNBM-UHFFFAOYSA-N lithium;oxalic acid Chemical class [Li].OC(=O)C(O)=O GBPZIFLFRULNBM-UHFFFAOYSA-N 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses the preparation facilities that a kind of lepidolite prepares high-purity lithium carbonate, including body and ammonia tank, control panel is provided with the outer surface of the body, and its upper end is connected with feeding mouth, the lower end of the control panel is mounted with discharging opening, the right-hand member of the feeding mouth is provided with pipeline, the front end of the body is mounted with aspiration pump, the lower end of the ammonia tank is connected with base, the inside of the body is provided with calcification chamber, the positioned inside of the calcification chamber has auger, the lower end of the belt pulley is provided with motor, the lower end of the calcification chamber is connected with the mouth that drops, the lower end of the mouth that drops is provided with extraction chamber, heating tube is installed between the extraction chamber and calcification chamber, and its positioned inside has agitating roller.The preparation facilities that the lepidolite prepares high-purity lithium carbonate carries out preparing lithium carbonate using lepidolite, can not only economize on resources, while can propose the lithium carbonate of high-purity, effectively protection equipment.
Description
Technical field
The present invention relates to chemical technology field, specially a kind of lepidolite prepares the preparation method of high-purity lithium carbonate.
Background technology
Lithium carbonate, a kind of inorganic compound, chemical formula Li2CO3 is colourless monoclinic system crystal body or white powder,
Density 2.11g/cm3, is dissolved in diluted acid.Water is slightly soluble in, solubility is big compared with hot water in cold water.Insoluble in alcohol and acetone, can use
In potting porcelain, medicine, catalyst etc..Conventional lithium ion battery raw material, because the primary raw material for producing lithium carbonate is salt lake halogen
Water (ore method is because cost height is in global production capacity very little), therefore the enterprise of large-scale production lithium carbonate must possess lithium resource storage
The salt lake resources right to mine compared with horn of plenty is measured, this causes the sector to possess higher resource barrier；On the other hand, due to global salt
Lake overwhelming majority resource is all the low lithium type of high magnesium, and the technological difficulty of purification ＆ isolation lithium carbonate is very from the low lithium of high magnesium old halogen
Greatly, the global lithium carbonate market concentration is very high at present.Before several mega projects in China are gone into operation, the main production capacity in the whole world is concentrated
In tri- hands of SQM, FMC and Chemetal l；Data is shown, although lithium carbonate product is in the presence of certain resource and art wall
Build, but China possess can the salt lake of extraction value or many, technology Salt Lake Group Company in addition to CITIC Guoan, Tibetan Mining also faces
Break through, the barrier of industry just gradually weakens.
Existing lithium carbonate manufacture method substantially has electrolysis, crystallisation, the precipitation method, and what industry was conventional at present prepares high-purity
The method purity of lithium carbonate can only 99.9% level, the preparation method pair with the lithium carbonate of higher purity, examination can only be rested on
The problem of testing the stage, while precipitation method absorptivity is relatively low, purity is not high, and crude product separately needs to handle, and cumbersome, equipment is fragile.
The content of the invention
It is an object of the invention to provide the preparation method that a kind of lepidolite prepares high-purity lithium carbonate, to solve the above-mentioned back of the body
Itd is proposed in scape technology the preparation pure Lithium Carbonate that industry is conventional at present method purity can only 99.9% level, pair with it is more high-purity
The preparation method of the lithium carbonate of degree, the problem of experimental stage can only be rested on, while precipitation method absorptivity is relatively low, purity is not high,
Crude product separately needs to handle, and cumbersome, equipment is fragile.
To achieve the above object, the present invention provides the preparation that a kind of lepidolite of following technical scheme prepares high-purity lithium carbonate
Method, including body and ammonia tank, control panel is provided with the outer surface of the body, and its upper end is connected with feeding mouth,
The lower end of the control panel is mounted with discharging opening, and the right-hand member of the feeding mouth is provided with pipeline, the front end placement of the body
Have an aspiration pump, and its outer surface or that be provided with and be connected with base into agent mouth, the lower end of the ammonia tank, the body
Inside is provided with calcification chamber, and the positioned inside of the calcification chamber has auger, and its left end is connected with belt pulley, the belt
The lower end of wheel is provided with motor, and the lower end of the calcification chamber is connected with the mouth that drops, and the lower end of the mouth that drops is provided with extraction
Chamber, heating tube is installed between the extraction chamber and calcification chamber, and its positioned inside has agitating roller.
Preferably, temperature sensor is installed between the extraction chamber and calcification chamber.
Preferably, the agitating roller is provided with two groups altogether.
Preferably, the auger and calcification chamber are detachable connecting device.
Preferably, it is described enter agent mouth be provided with two groups.
Compared with prior art, the beneficial effects of the invention are as follows：The lepidolite prepares the preparation method of high-purity lithium carbonate
Change traditional preparation method, carry out preparing lithium carbonate using lepidolite, can not only economize on resources, while can propose high-purity
The lithium carbonate of degree；Using aspiration pump, the oxygen of internal body is extracted out, prevents from, when injecting ammonia, causing internal ammonia impure,
Influence the purity of lithium carbonate；Increase temperature sensor, because the mechanical movement of internal body can produce substantial amounts of heat, heat mistake
Height can not only influence the purification of lithium carbonate, while can also damage inner body, in the presence of temperature sensor can be observed effectively
The temperature in portion, while to manually being radiated to it, effectively protection equipment.
Brief description of the drawings
Fig. 1 is schematic structural view of the invention；
Fig. 2 is organism internal structure schematic diagram of the present invention.
In figure：1st, body, 2, control panel, 3, feeding mouth, 4, pipeline, 5, aspiration pump, 6, discharging opening, 7, enter agent mouth, 8,
Base, 9, ammonia tank, 10, calcification chamber, 11, auger, 12, belt pulley, 13, motor, 14, temperature sensor, 15, heating tube,
16th, drop mouth, and 17, extraction chamber, 18, agitating roller.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not made
Embodiment, belong to the scope of protection of the invention.
Fig. 1-2 is referred to, the present invention provides a kind of technical scheme：A kind of lepidolite prepares the preparation side of high-purity lithium carbonate
Method, including body 1, control panel 2, feeding mouth 3, pipeline 4, aspiration pump 5, discharging opening 6, enter agent mouth 7, base 8, ammonia tank 9, calcium
Change chamber 10, auger 11, belt pulley 12, motor 13, temperature sensor 14, heating tube 15, the mouth 16 that drops, extraction chamber 17 and stir
Roller 18 is mixed, control panel 2 is provided with the outer surface of body 1, and its upper end is connected with feeding mouth 3, the lower end peace of control panel 2
Discharging opening 6 is equipped with, the right-hand member of feeding mouth 3 is provided with pipeline 4, and the front end of body 1 is mounted with aspiration pump 5, and its outer surface is still
That is provided with into agent mouth 7, is entered agent mouth 7 and is provided with two groups, the lower end of ammonia tank 9 is connected with base 8, the inside installation of body 1
There is calcification chamber 10, the positioned inside of calcification chamber 10 has auger 11, and its left end is connected with belt pulley 12, auger 11 and calcification
Chamber 10 is detachable connecting device, and the lower end of belt pulley 12 is provided with motor 13, and the lower end of calcification chamber 10, which is connected with, drops
Mouth 16, the lower end for the mouth 16 that drops are provided with extraction chamber 17, extract and be provided with TEMP between chamber 17 and calcification chamber 10
Device 14, the temperature of inside can be effectively observed, while to manually being radiated to it, effectively protection equipment, extracts chamber 17
Heating tube 15 is installed between calcification chamber 10, and its positioned inside has agitating roller 18, agitating roller 18 is provided with two groups altogether, side
Just repair and change.
Operation principle：, it is necessary to whole device before the preparation method of high-purity lithium carbonate is prepared using the lepidolite
Structure simply understood, claim a certain amount of lepidolite to insert calcification chamber 10, by its internal a certain amount of water, using full
With lithium oxalate solution, carry out decalcification processing, while calcification chamber 10 is rotated, internal auger 11 by saturated oxalic acid lithium solution,
Lepidolite and water are stirred, and allow it to be sufficiently mixed, and stand two hours, and filtering is evaporated to saturation, and by dropping, mouth 16 enters
Chamber 16 is extracted, medicament is added and is extracted, depth is gone out other impurities, and stirs two hours using agitating roller 17, is stood
Filtering, aspiration pump 5 extract the oxygen extracted in chamber 16 out, inject ammonia using ammonia tank 9, and heating tube 15 is heated, and obtain
To the lithium carbonate of high-purity, when internal temperature is too high, temperature sensor 14 transfers data to control panel 2, passes through control
Panel 2 stops heating, and is radiated.
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art,
It can still modify to the technical scheme described in foregoing embodiments, or which part technical characteristic is carried out etc.
With replacing, within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., this should be included in
Within the protection domain of invention.
Claims (3)
1. a kind of lepidolite prepares the preparation facilities of high-purity lithium carbonate, including body（1）And ammonia tank（9）, it is characterised in that：
The body（1）Outer surface on be provided with control panel（2）, and its upper end is connected with feeding mouth（3）, the control panel
（2）Lower end be mounted with discharging opening（6）, the feeding mouth（3）Right-hand member be provided with pipeline（4）, the body（1）Front end peace
It is equipped with aspiration pump（5）, and its outer surface is provided with into agent mouth（7）, the ammonia tank（9）Lower end be connected with base（8）, it is described
Body（1）Inside calcification chamber is installed（10）, the calcification chamber（10）Positioned inside have auger（11）, and its left end
It is connected with belt pulley（12）, the belt pulley（12）Lower end be provided with motor（13）, the calcification chamber（10）Lower end connect
It is connected to the mouth that drops（16）, the mouth that drops（16）Lower end be provided with extraction chamber（17）, the extraction chamber（17）With calcification
Chamber（10）Between heating tube is installed（15）, and its positioned inside has agitating roller（18）；
The extraction chamber（17）With calcification chamber（10）Between temperature sensor is installed（14）；
The agitating roller（18）Two groups are provided with altogether.
2. a kind of lepidolite according to claim 1 prepares the preparation facilities of high-purity lithium carbonate, it is characterised in that：It is described
Auger（11）With calcification chamber（10）For detachable connecting device.
3. a kind of lepidolite according to claim 1 prepares the preparation facilities of high-purity lithium carbonate, it is characterised in that：It is described
Enter agent mouth（7）It is provided with two groups.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611148616.9A CN106430260B (en) | 2016-12-13 | 2016-12-13 | A kind of lepidolite prepares the preparation method of high-purity lithium carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611148616.9A CN106430260B (en) | 2016-12-13 | 2016-12-13 | A kind of lepidolite prepares the preparation method of high-purity lithium carbonate |
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| Publication Number | Publication Date |
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| CN106430260A CN106430260A (en) | 2017-02-22 |
| CN106430260B true CN106430260B (en) | 2017-11-24 |
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Family Cites Families (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2470861C2 (en) * | 2008-04-22 | 2012-12-27 | Роквуд Литиэм Инк. | Method of producing high-purity lithium hydroxide and hydrochloric acid |
| JP5138640B2 (en) * | 2009-07-06 | 2013-02-06 | Ｊｘ日鉱日石金属株式会社 | Method for producing lithium carbonate from recovered lithium ion secondary battery |
| CN102408120B (en) * | 2010-09-20 | 2014-01-01 | 华东理工大学 | A method for preparing high-purity lithium carbonate ultrafine powder |
| KR101047984B1 (en) * | 2010-11-17 | 2011-07-13 | 한국지질자원연구원 | Process for producing high purity lithium carbonate in brine |
| CN102009989B (en) * | 2010-12-31 | 2012-07-18 | 重庆昆瑜锂业有限公司 | Method for preparing high-purity lithium carbonate by utilizing digestive solution generated in lithium production |
| AU2011236094B2 (en) * | 2011-01-20 | 2012-11-29 | Rockwood Lithium Inc. | Production of high purity lithium compounds directly from lithium containing brines |
| CN102173438A (en) * | 2011-01-25 | 2011-09-07 | 宜春学院 | Method for producing gypsum as byproduct in preparation of lithium carbonate by using lepidolite from tantalum-niobium tailings |
| CN102583453B (en) * | 2011-08-31 | 2013-10-16 | 四川长和华锂科技有限公司 | Industrial method for producing battery-grade lithium carbonate or high-purity lithium carbonate |
| CN102432045B (en) * | 2011-09-26 | 2013-02-13 | 江苏海龙锂业科技有限公司 | Preparation method of ultra-high purity lithium carbonate |
| CN102531002B (en) * | 2011-12-23 | 2013-08-14 | 四川天齐锂业股份有限公司 | Method for purifying lithium carbonate |
| CN102557084A (en) * | 2012-01-18 | 2012-07-11 | 黄三贵 | Method for preparing high-purity lithium carbonate from lithium chloride stock solution |
| JP5406955B2 (en) * | 2012-03-22 | 2014-02-05 | 日鉄鉱業株式会社 | Method for producing lithium carbonate |
| CN102963914B (en) * | 2012-11-27 | 2014-08-20 | 西藏金浩投资有限公司 | Method for preparing high-purity lithium carbonate from salt lake brine |
| CN103539169A (en) * | 2013-10-24 | 2014-01-29 | 中国地质科学院郑州矿产综合利用研究所 | Method for preparing battery-grade lithium carbonate or high-purity lithium carbonate by using industrial-grade lithium carbonate |
| CN203728593U (en) * | 2014-01-10 | 2014-07-23 | 朱彬元 | Multifunctional integrated industrial device for preparing high-purity lithium carbonate |
| CN105329921A (en) * | 2015-12-08 | 2016-02-17 | 汕头市泛世矿业有限公司 | Three-in-one preparing technology for high-purity lithium carbonate |
| CN106082285B (en) * | 2016-06-23 | 2019-01-11 | 湖南中大技术创业孵化器有限公司 | The method of lithium salts is extracted from salt lake brine with high magnesium-lithium ratio |
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