CN106636673A - A kind of method adopting extraction method to extract lithium from salt lake brine - Google Patents
A kind of method adopting extraction method to extract lithium from salt lake brine Download PDFInfo
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- CN106636673A CN106636673A CN201611206853.6A CN201611206853A CN106636673A CN 106636673 A CN106636673 A CN 106636673A CN 201611206853 A CN201611206853 A CN 201611206853A CN 106636673 A CN106636673 A CN 106636673A
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- salt lake
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- 238000000605 extraction Methods 0.000 title claims abstract description 109
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 82
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000012267 brine Substances 0.000 title abstract description 7
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 title abstract description 7
- 230000007935 neutral effect Effects 0.000 claims abstract description 25
- 239000000284 extract Substances 0.000 claims abstract description 24
- AFCIMSXHQSIHQW-UHFFFAOYSA-N [O].[P] Chemical compound [O].[P] AFCIMSXHQSIHQW-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229940126062 Compound A Drugs 0.000 claims abstract description 21
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000011069 regeneration method Methods 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 230000008929 regeneration Effects 0.000 claims abstract description 15
- 239000003085 diluting agent Substances 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 7
- 230000005588 protonation Effects 0.000 claims abstract description 4
- 239000012074 organic phase Substances 0.000 claims description 80
- 239000012071 phase Substances 0.000 claims description 73
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 42
- 241001131796 Botaurus stellaris Species 0.000 claims description 38
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 17
- 239000011777 magnesium Substances 0.000 claims description 17
- 239000003607 modifier Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 13
- 230000007704 transition Effects 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 239000003350 kerosene Substances 0.000 claims description 11
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- -1 phosphorus oxygen class compound Chemical class 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 6
- BBMCTIGTTCKYKF-UHFFFAOYSA-N 1-heptanol Chemical compound CCCCCCCO BBMCTIGTTCKYKF-UHFFFAOYSA-N 0.000 claims description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 6
- SJWFXCIHNDVPSH-UHFFFAOYSA-N octan-2-ol Chemical compound CCCCCCC(C)O SJWFXCIHNDVPSH-UHFFFAOYSA-N 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910001514 alkali metal chloride Inorganic materials 0.000 claims description 5
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 150000003141 primary amines Chemical class 0.000 claims description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 2
- 101100037762 Caenorhabditis elegans rnh-2 gene Proteins 0.000 claims description 2
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 claims description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- NNBFNNNWANBMTI-UHFFFAOYSA-M brilliant green Chemical compound OS([O-])(=O)=O.C1=CC(N(CC)CC)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](CC)CC)C=C1 NNBFNNNWANBMTI-UHFFFAOYSA-M 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 150000003335 secondary amines Chemical class 0.000 claims description 2
- 241000894007 species Species 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
- 230000003750 conditioning effect Effects 0.000 claims 1
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 abstract description 4
- GCICAPWZNUIIDV-UHFFFAOYSA-N lithium magnesium Chemical compound [Li].[Mg] GCICAPWZNUIIDV-UHFFFAOYSA-N 0.000 abstract description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 abstract description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000005191 phase separation Methods 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 239000003513 alkali Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 238000005660 chlorination reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- YEVQZPWSVWZAOB-UHFFFAOYSA-N 2-(bromomethyl)-1-iodo-4-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=C(I)C(CBr)=C1 YEVQZPWSVWZAOB-UHFFFAOYSA-N 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000008439 repair process Effects 0.000 description 3
- FOGVNFMUZXDMTR-UHFFFAOYSA-N [Mg].Cl Chemical compound [Mg].Cl FOGVNFMUZXDMTR-UHFFFAOYSA-N 0.000 description 2
- 229910001617 alkaline earth metal chloride Inorganic materials 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- YKGBNAGNNUEZQC-UHFFFAOYSA-N 6-methyl-n,n-bis(6-methylheptyl)heptan-1-amine Chemical compound CC(C)CCCCCN(CCCCCC(C)C)CCCCCC(C)C YKGBNAGNNUEZQC-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 101000686983 Xenopus laevis 26S proteasome regulatory subunit 6A-B Proteins 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 description 1
- 235000013923 monosodium glutamate Nutrition 0.000 description 1
- 239000004223 monosodium glutamate Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/40—Mixtures
- C22B3/409—Mixtures at least one compound being an organo-metallic compound
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/007—Contaminated open waterways, rivers, lakes or ponds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
本发明涉及一种采用萃取法从盐湖卤水中提取锂的方法，该方法适用于从高镁锂比盐湖卤水和盐田含锂浓缩老卤中制取碳酸锂和氯化锂的生产过程。该方法采用共萃剂FeCl3、萃取剂和稀释剂进行锂的萃取，所述萃取剂为中性磷氧类化合物A和相调节剂B的混合物，其中所述相调节剂B为萃取反应过程中可与中性磷氧类化合物A发生质子化反应的有机化合物，所述萃取剂萃锂后的萃合物组成为xLiFeCl4·yHCl·aA·bB，该萃合物易溶于稀释剂，萃取体系具有良好的分相性能和反萃、再生性能，进一步优化了萃取法提锂的工艺。本发明方法对设备要求低、所用有机化合物价廉易得、适于工业应用。
The invention relates to a method for extracting lithium from salt lake brine by an extraction method, which is suitable for the production process of producing lithium carbonate and lithium chloride from salt lake brine with a high magnesium-lithium ratio and lithium-containing concentrated old brine in salt fields. The method uses a co-extractant FeCl 3 , an extractant and a diluent to extract lithium, and the extractant is a mixture of a neutral phosphorus-oxygen compound A and a phase regulator B, wherein the phase regulator B is an extraction reaction process An organic compound that can undergo a protonation reaction with the neutral phosphorus-oxygen compound A. The composition of the extract after the extraction of lithium by the extractant is xLiFeCl 4 yHCl aA bB, the extract is easily soluble in the diluent, The extraction system has good phase separation performance, stripping and regeneration performance, and further optimizes the process of extracting lithium by extraction. The method of the invention has low equipment requirements, the organic compound used is cheap and easy to obtain, and is suitable for industrial application.
Description
Technical field
The present invention relates to chemical technology field, more particularly to a kind of employing extraction extracts the side of lithium from salt lake bittern
Method.
Background technology
Lithium has various excellent properties, is referred to as " energy metal of 21st century ", " industrial monosodium glutamate ", " space of tomorrow
Boat alloy ", strategic position is notable.Salt lake bittern is the valuable source of lithium, and China has abundant salt lake bittern lithium resource, its storage
Amount is at the forefront in the world.The bittern that now foreign countries have produced carries lithium and is all only limitted to containing the relatively low bittern of magnesium density, and Mg/Li ratio value is less than
6:1, and for separation in so-called " high Mg/Li ratio " bittern of high concentration magnesium, low concentration lithium is contained in such as China Caidamu Basin salt lake
Lithium is extracted, is generally acknowledged worldwide technological puzzle.
Solvent extraction technology is the effective technology of the various metals of separation and Extraction from solution, in carrying for low concentration intentional metal
Take aspect to be widely used, with separative efficiency is high, technique and equipment is simple, operation serialization, be easily achieved automatically control etc. it is excellent
Point, researcher extracts separating Li from salt lake brine with high magnesium-lithium ratio and has carried out substantial amounts of research to solvent extraction technology, it is proposed that
Some extraction systems and technique, wherein with FeCl3Make common extraction agent, tributyl phosphate makees the closest industry of system of extractant should
With.The Chinese invention patent 87103431 of Qinghai Yanhu Inst., Chinese Academy of Sciences's application in 1987 is proposed uses FeCl3It is total to
Extraction agent, the system and technique of the kerosin extraction lithium of single extractant tributyl phosphate, technology has carried out big bavin denier salt lake
The pilot-plant test of lithium is extracted in bittern.But, the system middle and high concentration tributyl phosphate exist it is strong to extraction equipment corrosivity,
Easily greatly, in acid medium the deficiencies such as degraded in the water-soluble loss of organic phase, it is difficult to large-scale industrial application there is.Chinese section in 2012
Institute's Qinghai Salt Lake is studied apllied Chinese invention patent 201210055323.1 and is proposed with alkali metal chloride, alkaline earth gold
Category chloride or its mixture replace the full alkali phase inversion of full acid in the extraction process of Chinese invention patent 87103431, to reduce soda acid
The corrosion of expense and reduction to equipment, the Chinese invention patent of Qinghai Yanhu Inst., Chinese Academy of Sciences's application in 2012
201210164150.7 propose with the extraction system that the mixture of amide-type and neutral phosphorus oxygen class compound is extractant, the extraction
The system of taking compares single extractant tributyl phosphate and can reduce the corrosion to equipment, document " N523-TBP- sulfonated kerosene extractor bodies
System extracts the technical study of lithium from Saturated with Magnesium chloride bittern " (Shi Dong etc., salt lake research, 2013,21 (2)：52-57) report in detail
The mixture of the new acid amides kind of extractants N523 in road and neutral phosphorus oxygen kind of extractants TBP is the extraction system of extractant, is adopted
The new extraction system of " 20%N523-30%TBP-50% sulfonated kerosenes ", have studied adverse current cascade extraction, washing, back extraction, phase inversion
Deng the technological parameter of workshop section, it is determined that extraction process flow, the experiment of whole process extraction process is completed, for lithium concentration about 2g/
L, Mg/Li ratio about 55:1 Qinghai salt lake carries old halogen after potassium, and the extraction system is Jing after 8 grades of whole process extractions, and lithium extraction yield is reachable
To more than 96%, extraction split-phase is fast, without three-phase and emulsion.The phase inversion regenerative process of the extraction system organic phase is that hydrochloric acid is anti-
Empty load organic phases after extraction neutralize the acid in organic phase after shaking up with quantitative NaOH, then contact with raffinate and will enter
The iron of water phase extracts into organic phase, makes HFeCl4It is converted into NaFeCl4、Mg(FeCl4)2, make the ability of extractant recovery extraction lithium complete
Into phase inversion process, necessary precise control adds the amount of alkali during phase inversion, and caustic dosage is too low, can have a strong impact on regeneration organic phase lithium
Extracting power, caustic dosage is too high, and excessive alkali can not completely be neutralized by the acid in bittern in load organic phases, can be had a strong impact on
Split-phase effect, to industrial control level very high requirement is proposed.On the whole, existing salt lake bittern extraction carries lithium side
Method still has that technological process is complicated, extraction agent price is high, extraction equipment requirement for anticorrosion is high and invests big, overall production cost
It is high.
The content of the invention
The purpose of the present invention is for the deficiencies in the prior art, there is provided a kind of corrosivity and technique stream that can be reduced to equipment
Journey is simply controllable, it is easy to the method that lithium is extracted from salt lake bittern of Project Realization.
The present invention provides a kind of method that employing extraction extracts lithium from salt lake bittern, and it adopts common extraction agent FeCl3, extraction
Take agent and diluent carries out the extraction of lithium, the extractant is the mixture of neutral phosphorus oxygen class compound A and phase modifier B, institute
Phase modifier B is stated for protonation reaction can occur with neutral phosphorus oxygen class compound A during extractive reaction organic compound, institute
State the extracted species after extractant extraction lithium and consist of xLiFeCl4YHClaAbB, Jing back extractions-regenerated after extractant extraction lithium
Journey can return to extraction and carry lithium.
Described employing extraction extracts the method for lithium from salt lake bittern and specifically includes following step：
1) blank organic phase is prepared：Dilution dilution agent will be used after neutral phosphorus oxygen class compound A and phase modifier B mixing,
It is 10%～40% to control neutral phosphorus oxygen class compound ratio in blank organic phase；
2) prepared by load organic phases：Organic phase load titanium tetrachloride complex compound and hydrochloric acid：By above-mentioned blank organic phase and bag
Solution containing 0.1～1mol/l ferric trichlorides and 0.1～1mol/l hydrochloric acid is according to volume ratio 1:1 is mixed, and is stood after vibration
Split-phase obtains the load organic phases of load iron and acid；
3) load organic phases transition：Load organic phases are mixed with alkali-metal chloride solution, split-phase are stood after vibration,
Complete load organic phases transition；
4) extraction section：Load organic phases after transition are mixed with bittern containing lithium, split-phase is stood after vibration, measured respectively point
Organic phase and water phase Li after phase+、Mg2+、Na+And K+Concentration calculates the separation of Li/Mg, Li/Na and Li/K, it is known that Li+Proceed to
To in organic phase, and Mg2+、Na+And K+In being transferred to water phase.Wherein Li in bittern+With LiFeCl4Complex form is present；
5) washing section：Mixed with organic using water, split-phase is stood after vibration, repeatedly, by the Mg in organic phase2 +、Na+And K+In being transferred to water phase；
Described employing extraction extracts the method for lithium from salt lake bittern can also include that stripping section and organic phase regenerate,
Wherein stripping section comprises the steps：The organic phase of extraction lithium is taken, 1-6mol/l hydrochloric acid is added thereto to, it is quiet after vibrating 10 minutes
Put split-phase, H+With HFeCl4Complex form extracts into organic phase, and the Li in organic phase+It is counter enter water phase, wherein emerald green area's lithium is organic
20 are preferably with the volume ratio of hydrochloric acid：1.
Described organic phase regeneration comprises the steps：The organic phase after hydrochloric acid back extraction is taken, the chlorination of 3～6mol/l is added
Magnesium solution, vibration stands split-phase after 10 minutes, obtains final product regeneration organic phase, and regeneration organic phase can return to carry out extraction to carry lithium.
Above-mentioned employing extraction is extracted in the method for lithium from salt lake bittern, described described neutral phosphorus oxygen class compound A
For tributyl phosphate TBP, trioctyl phosphate TOP one or two.The phase modifier B is can to carry after itself or extraction hydrochloric acid
Protogenic organic compound, it is preferable that the phase modifier B be high-carbon alcohol compound, aminated compounds in one kind or
Its combination.It is highly preferred that the high-carbon alcohol compound is C6-C12 alcohol, more preferably described high-carbon alcohol compound is secondary
Octanol, isooctanol, n-octyl alcohol, one or more of n-heptanol.The aminated compounds is primary amine RNH2, secondary amine R2NH, tertiary amine R3N
In one or more.
Above-mentioned employing extraction is extracted in the method for lithium from salt lake bittern, the neutral phosphorus oxygen class compound A with mutually adjust
Contents (percentage by volume V%) of the agent B in extractant and diluent mixture is saved between 30% to 80%, wherein described
Contents of the neutral phosphorus oxygen class compound A in extractant and diluent mixture is 10%～40%.
Wherein, the neutral phosphorus oxygen class compound A and the scope of the relative volume ratio of two kinds of extractants of phase modifier B are 1:
30 to 30:1.
Wherein, the diluent is aliphatic hydrocarbon or aromatic hydrocarbon.Preferably, the diluent is sulfonated kerosene.
The method that above-mentioned employing extraction extracts lithium from salt lake bittern, it also includes the stripping process, wherein back extraction
During using 1～6mol/l hydrochloric acid back extraction.
The regenerative process is, with organic after alkali or alkaline earth metal chloride brine hydrochloric acid back extraction, to make HFeCl4Turn
Turn to NaFeCl4、Mg(FeCl4)2Deng the ability for making extractant recover extraction lithium.Compared to prior art, the acquirement of the present invention
Following unforeseeable technique effect：
1) by introducing the phase modifier B that protonation reaction can occur with neutral phosphorus oxygen class compound A in extraction system,
Split-phase effect of the neutral phosphorus oxygen class compound extraction titanium tetrachloride complex compound in sulfonated kerosene diluent, split-phase can be significantly improved
Speed is fast, and extraction system to be extracted and possess a range of acidity self-adjusting ability after a certain amount of hydrochloric acid, is conducive to control extraction
The hydrolysis of iron in whole process, cyclic process is smooth.
2) extraction system proposed by the present invention further optimizes the extraction of extraction-back extraction-regeneration and proposes lithium technological process,
Reduce the consumption of neutral phosphorus oxygen class compound, alkali or alkaline earth metal chloride salting liquid used in organic phase regenerative process and not
Need to use alkali, so that solubility and chemistry drop in corrosivity, the water of neutral phosphorus oxygen class compound in existing extraction process
Solution effect is significantly alleviated, while whole process does not use alkali, reduces the corrosion of extraction process expense and reduction to equipment.This
Inventive method is low for equipment requirements, organic compound used is cheap and easy to get, be suitable to commercial Application.
Description of the drawings
Fig. 1 is the schematic flow sheet that the embodiment of the present invention extracts lithium using extraction from salt lake bittern.
Specific embodiment
The present invention is described in detail below by way of concrete and infinite embodiment, so that advantages and features of the invention energy
It is easier to be readily appreciated by one skilled in the art.
Fig. 1 is the schematic flow sheet that the embodiment of the present invention extracts lithium using extraction from salt lake bittern.Can be seen by Fig. 1
Go out, the flow process of described extraction lithium includes：Preparing blank organic phase -- organic phase load titanium tetrachloride complex compound and hydrochloric acid -- has
Machine mutually makes the transition --- extraction section-extraction section washing is extracted to obtain, it is described
Following examples adopt technique as shown in Figure 1.
The composition of table 1 certain salt lake brine with high magnesium-lithium ratio
| Composition | Li+ | Mg2+ | Na+ | K+ | Cl- | B2O3 |
| Content (g/l) | 0.5～5 | 80～130 | 0～3 | 0～3 | ≥200 | 0～3 |
Embodiment 1
Neutral phosphorus oxygen class compound A selects tributyl phosphate TBP, phase modifier B to select aminated compounds tri-iso-octylamine
N235 and high-carbon alcohol compound sec-octyl alcohol, diluent constitutes extractant from sulfonated kerosene, and tributyl phosphate TBP is in extractant
In account for volume ratio 10%～40%.
0.1～6mol/l hydrochloric acid solutions of 1 part of extractant and 1 part of ferric trichloride 0.1～3mol/l of concentration are vibrated into 10 points
Split-phase is stood after clock, the load organic phases of load iron and acid are obtained；By 1 part of above-mentioned load organic phases and 4 parts of 3～6mol/l chlorinations
Calcium solution stands split-phase after vibrating 10 minutes, completes load organic phases transition；By the load organic phases and 1 after 1 part of above-mentioned transition
Certain salt lake (Mg/Li=100 of bittern containing lithium of composition shown in part table 1:1 mass ratio) vibration extracted within 10 minutes, vibration terminates
After stand split-phase, organic phase and water phase Li after split-phase are measured respectively+、Mg2+、Na+And K+Concentration, thus calculates the extraction yield of lithium
For 78.56%, Li+、Mg2+、Na+And K+Distribution ratio is respectively 3.265,0.0085,0.0837,0.0425, Li/Mg, Li/Na and
The separation of Li/K is respectively 384.1,39.0,76.8.
Embodiment 2
Neutral phosphorus oxygen class compound A selects trioctyl phosphate TOP, phase modifier B from aminated compounds primary amine N1923 and
High-carbon alcohol compound n-heptanol, diluent constitutes extractant from sulfonated kerosene, and trioctyl phosphate TOP accounts for body in extractant
Product ratio 10%～40%.
By 1 part of extractant and 1 part of ferric trichloride 0.1～1mol/l of concentration, the saturation chlorination of 0.1～1mol/l of concentration of hydrochloric acid
Magnesium solution stands split-phase after vibrating 10 minutes, obtain the load organic phases of load iron and acid；By 1 part of above-mentioned load organic phases and 6
3～6mol/l of part magnesium chloride solutions stand split-phase after vibrating 10 minutes, complete load organic phases transition；After 2 parts of above-mentioned transition
Load organic phases and composition shown in 1 part of table 1 certain salt lake (Mg/Li=50 of bittern containing lithium:1 mass ratio) vibration carry out within 10 minutes
Extraction, vibration stands split-phase after terminating, and organic phase and water phase Li after split-phase are measured respectively+、Mg2+、Na+And K+Concentration, thus calculates
The extraction yield for going out lithium is 90.45%, Li+、Mg2+、Na+And K+Distribution ratio is respectively 4.536,0.0096,0.0987,0.0479,
The separation of Li/Mg, Li/Na and Li/K is respectively 472.5,45.96,94.7.
Embodiment 3
Neutral phosphorus oxygen class compound A selects tributyl phosphate TBP, phase modifier B from aminated compounds primary amine N1923 and
High-carbon alcohol compound sec-octyl alcohol, diluent constitutes extractant from sulfonated kerosene, and tributyl phosphate TBP accounts for body in extractant
Product ratio 10%～40%.
By 1 part of extractant and 1 part of ferric trichloride 0.1～1mol/l of concentration, the saturation chlorination of 0.1～1mol/l of concentration of hydrochloric acid
Magnesium solution stands split-phase after vibrating 10 minutes, obtain the load organic phases of load iron and acid；By 1 part of above-mentioned load organic phases and 6
3～6mol/l of part magnesium chloride solutions stand split-phase after vibrating 10 minutes, complete load organic phases transition；After 2 parts of above-mentioned transition
Load organic phases and composition shown in 1 part of table 1 certain salt lake (Mg/Li=50 of bittern containing lithium:1 mass ratio) carry out three stage countercurrent extractions
Take, balance back loading organic phase Li+、Mg2+、Na+And K+Concentration (g/l) is respectively 1.287,0.203,0.075,0.008；By 30
The above-mentioned extraction lithium organic phase of part is washed with the aqueous solution of 1 part of chlorination 0.1～3mol/l of lithium concentration, 0.1～3mol/l of concentration of hydrochloric acid
Wash, back loading organic phase Li is balanced after washing+、Mg2+、Na+And K+Concentration (g/l) is respectively 1.178,0.002,0.018,
0.002。
Embodiment 4
Neutral phosphorus oxygen class compound A selects tributyl phosphate TBP, phase modifier B from aminated compounds primary amine N1923 and
High-carbon alcohol compound sec-octyl alcohol, diluent constitutes extractant from sulfonated kerosene, and tributyl phosphate TBP accounts for body in extractant
Product ratio 10%～40%.
The extraction system of suitable commercial Application, does not require nothing more than and has good extraction ability and selectivity to object ion,
And to have good back extraction performance, organic phase to be easy to regeneration and permanent stable circulation, " 10%～40%TBP- is enumerated for this
The sulfonated kerosene of-0%～30% sec-octyl alcohol of 0%～30% primary amine N1923-30%～80% " extraction system " extraction-back extraction-again
Life " carries the example of lithium from salt lake bittern.
Organic extractant phase proposes lithium operation with embodiment 3, and Jing after extraction carries lithium, organic phase Li concentration is 1.287g/l, raffinate
Water phase Fe concentration≤1mg/l；The organic phase of 20 parts of extraction lithiums is taken, 1 part of 6mol/l hydrochloric acid (comparing O/A=20), vibration 10 is added
Minute carries out back extraction, and vibration stands split-phase, organic phase Li after split-phase is measured respectively after terminating+Concentration is 0.034g/l, water phase Li+
Concentration is 25.12g/l, and the back extraction ratio of lithium is 97.6%, strip aqueous Fe concentration≤30mg/l；Take having after 1 part of hydrochloric acid back extraction
Machine phase, adds the magnesium chloride solution of 6 parts of 3～6mol/l, vibration to carry out within 10 minutes organic phase regeneration, and vibration stands after terminating and divides
Phase, measures water phase Fe concentration≤1mg/l, and the organic phase after regeneration returns extraction and carries lithium, Jing after extraction carries lithium, organic phase Li concentration
For 1.284g/l.
From back extraction and organic phase regeneration cycle data, " 10%～40%TBP-10%～30% sec-octyl alcohol -30%～
80% sulfonated kerosene " extraction system back extraction ratio is high, and organic phase regeneration is easy, and organic extractant phase capacity is substantially unattenuated after regeneration,
It is high using the rich lithium strip liquor lithium concentration for comparing acquisition after back extraction greatly, facilitate views with conventional method and obtain lithium chloride or lithium carbonate
Product.
Claims (9)
1. a kind of method that employing extraction extracts lithium from salt lake bittern, it adopts common extraction agent FeCl3, extractant and diluent
Carry out the extraction of lithium, it is characterised in that the extractant is the mixture of neutral phosphorus oxygen class compound A and phase modifier B, wherein
The phase modifier B is the organic compound that protonation reaction can occur during extractive reaction with neutral phosphorus oxygen class compound A,
Extracted species after the extractant extraction lithium consists of xLiFeCl4YHClaAbB, Jing back extractions-regeneration after extractant extraction lithium
Process can return to extraction and carry lithium.
2. the method that employing extraction according to claim 1 extracts lithium from salt lake bittern, it is characterised in that described
The method that lithium is extracted from salt lake bittern using extraction specifically includes following step：
1) blank organic phase is prepared：, using dilution dilution agent, will control after neutral phosphorus oxygen class compound A and phase modifier B mixing
Neutral phosphorus oxygen class compound ratio in blank organic phase is 10%～40%；
2) prepared by load organic phases：Organic phase load titanium tetrachloride complex compound and hydrochloric acid：By above-mentioned blank organic phase and comprising 0.1
The solution of～1mol/l ferric trichlorides and 0.1～1mol/l hydrochloric acid is according to volume ratio 1:1 is mixed, and split-phase is stood after vibration and is obtained
Obtain the load organic phases of load iron and acid；
3) load organic phases transition：Load organic phases are mixed with alkali-metal chloride solution, split-phase is stood after vibration, completed
Load organic phases make the transition；
4) extraction section：Load organic phases after transition are mixed with bittern containing lithium, split-phase is stood after vibration, measured respectively after split-phase
Organic phase and water phase Li+、Mg2+、Na+And K+Concentration calculates the separation of Li/Mg, Li/Na and Li/K, it is known that Li+It has been transferred to
In machine phase, and Mg2+、Na+And K+In being transferred to water phase.Wherein Li in bittern+With LiFeCl4Complex form is present；
5) washing section：Mixed with organic using water, split-phase is stood after vibration, repeatedly, by the Mg in organic phase2+、Na+
And K+In being transferred to water phase.
3. the method that employing extraction according to claim 1 extracts lithium from salt lake bittern, it is characterised in that in described
Property phosphorus oxygen class compound A be tbp or the pungent fat of tricresyl phosphate one or two.
4. the method that employing extraction according to claim 1 extracts lithium from salt lake bittern, it is characterised in that the phase
To carry protogenic organic compound after itself or extraction hydrochloric acid, the phase modifier B is high-carbon alcohols chemical combination to conditioning agent B
One kind or its combination in thing, aminated compounds, wherein described high-carbon alcohol compound is C6-C12 alcohol, preferably Zhong Xin
One kind or its combination in alcohol, isooctanol, n-octyl alcohol, n-heptanol；The aminated compounds is primary amine RNH2, secondary amine R2NH, uncle
One kind or its combination in amine R3N.
5. the method that employing extraction according to claim 1 extracts lithium from salt lake bittern, it is characterised in that in described
The total content of property phosphorus oxygen class compound A and phase modifier B in organic phase between 30% to 80%, wherein the neutral phosphor oxygen
Class compound A is 1 with the scope of the relative volume ratio of two kinds of extractants of phase modifier B:30 to 30:1, it is preferable that in described
Property contents of the phosphorus oxygen class compound A in extractant and diluent mixture be 10%～40%.
6. the method that employing extraction according to claim 1 extracts lithium from salt lake bittern, it is characterised in that described dilute
Agent is released for aliphatic hydrocarbon or aromatic hydrocarbon, preferably sulfonated kerosene.
7. the method that employing extraction according to claim 1 extracts lithium from salt lake bittern, it is characterised in that described common
Load capacity of the extraction agent ferric trichloride in organic phase is 0.05mol/l to 1mol/l.
8. the method that employing extraction according to claim 1 extracts lithium from salt lake bittern, it is characterised in that it is also wrapped
Stripping section and organic phase regeneration are included, wherein stripping section comprises the steps：The organic phase of extraction lithium is taken, 1- is added thereto to
6mol/l hydrochloric acid, vibration stands split-phase, H after 10 minutes+With HFeCl4Complex form extracts into organic phase, and the Li in organic phase+
It is counter enter water phase, wherein the emerald green organic phase of area's lithium is preferably 20 with the volume ratio of hydrochloric acid：1；Described organic phase regeneration includes following
Step：The organic phase after hydrochloric acid back extraction is taken, adds the magnesium chloride solution of 3～6mol/l, vibration to stand split-phase after 10 minutes, obtain final product
Regeneration organic phase, regeneration organic phase can return to carry out extraction to carry lithium.
9. the method that employing extraction according to claim 2 extracts lithium from salt lake bittern, it is characterised in that described
Back extraction system include 10%～40% tributyl phosphate, 0%～30% primary amine N1923,0%～30% sec-octyl alcohol, 30%～
80% sulfonated kerosene.
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