CN114959306B - Method for recycling lithium from lithium precipitation mother liquor by closed cycle method - Google Patents
Method for recycling lithium from lithium precipitation mother liquor by closed cycle method Download PDFInfo
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- CN114959306B CN114959306B CN202210674018.4A CN202210674018A CN114959306B CN 114959306 B CN114959306 B CN 114959306B CN 202210674018 A CN202210674018 A CN 202210674018A CN 114959306 B CN114959306 B CN 114959306B
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- lithium
- precipitation mother
- solution
- mother liquor
- sodium
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 63
- 238000001556 precipitation Methods 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000012452 mother liquor Substances 0.000 title claims description 15
- 238000004064 recycling Methods 0.000 title description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 44
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011780 sodium chloride Substances 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 19
- 239000010413 mother solution Substances 0.000 claims abstract description 16
- 229910001415 sodium ion Inorganic materials 0.000 claims abstract description 13
- 238000002386 leaching Methods 0.000 claims abstract description 12
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000460 chlorine Substances 0.000 claims abstract description 11
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 11
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 10
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract 2
- 230000001376 precipitating effect Effects 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000000706 filtrate Substances 0.000 description 14
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 10
- 229910052808 lithium carbonate Inorganic materials 0.000 description 10
- 239000011734 sodium Substances 0.000 description 9
- 239000012065 filter cake Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000005406 washing Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 4
- 229910001386 lithium phosphate Inorganic materials 0.000 description 4
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- -1 enamel Substances 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-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
- 239000003929 acidic solution Substances 0.000 description 1
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910052642 spodumene Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for recovering lithium from a lithium precipitation mother solution by a closed cycle method, wherein a lithium chloride solution is obtained by leaching a lithium-containing material by hydrochloric acid, the lithium chloride solution is purified and precipitated by sodium carbonate to obtain the lithium precipitation mother solution, a chlorine-containing compound is added into the lithium precipitation mother solution to separate sodium ions in the lithium precipitation mother solution in the form of sodium chloride, solid-liquid separation is carried out, the solid is sodium chloride, and the liquid returns to the leaching process of the lithium-containing material. The method has the advantages of low cost and high efficiency for recovering lithium in the lithium precipitation mother solution, and simultaneously, the concentration of lithium ions in the lithium precipitation mother solution is improved, and the recovery rate of lithium in lithium materials is greatly improved.
Description
Technical Field
The invention relates to a method for treating a lithium precipitation mother solution, in particular to a method for recovering lithium from the lithium precipitation mother solution by a closed cycle method, and belongs to the technical field of lithium extraction.
Background
Lithium carbonate (Li) 2 CO 3 ) Is one of the most common lithium salts, widely used in the glass, enamel, ceramic industries as a fluxing agent and reactant.
In addition, the development of the lithium ion battery is well-blown, the demand for lithium carbonate is increasingly tense, and the high-efficiency recycling and economic value of lithium is remarkable. Since lithium carbonate is slightly soluble in water, there are two inevitable problems involved in the production of lithium salts: 1. the direct yield of lithium is low in the process of precipitating lithium by carbonate; 2. in Li 2 CO 3 A large amount of wastewater with high Na/Li ratio is generated in the precipitation process, and the treatment process of the wastewater is complex and has high cost. In the prior art, the treatment method for the lithium precipitation mother liquor mainly adopts phosphoric acid compounds to further precipitate lithium to obtain lithium phosphate with lower solubility, the mother liquor after separating lithium phosphate is concentrated and crystallized to obtain sodium chloride, and the lithium phosphate is required to be converted into lithium carbonate in multiple steps, so that the overall lithium recovery rate is lower.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a method for recycling lithium from lithium precipitation mother liquor by a closed cycle method, which realizes that sodium ions in the lithium precipitation mother liquor are open-circuited in a sodium chloride form, and the lithium ions can circularly enter a leaching system, thereby not only solving the technical problem of low direct yield of the lithium ions in the lithium precipitation process, but also avoiding the generation of high Na/Li salt-containing wastewater.
In order to achieve the technical aim, the invention provides a method for recycling lithium from lithium precipitation mother liquor by a closed cycle method.
As a preferable scheme, the ratio of the concentration of sodium ions to the concentration of lithium ions in the lithium precipitation mother solution is higher than 15:1. The lithium precipitation mother liquor is a typical high Na/Li ratio solution.
As a preferable scheme, the chlorine-containing compound is at least one of HCl gas, chlorine gas and hydrochloric acid. The chlorine-containing compounds can be selected to achieve the purpose of selectively separating out sodium ions by regulating and controlling the concentration of chloride ions and hydrogen ions in a solution system, new metal ions are not introduced, and the liquid after precipitating the sodium ions is mainly an acidic solution containing lithium ions and can be directly used as a leaching agent for leaching lithium-containing materials.
As a preferable embodiment, the hydrochloric acid concentration is 6 to 12mol/L. If the concentration of the hydrochloric acid is too low, the lithium precipitation mother solution is excessively diluted, so that the difficulty of precipitation of sodium ions is increased.
As a preferred embodiment, the chlorine-containing compound is added in an amount to control H in the sodium chloride precipitation endpoint solution system + The concentration is more than 2mol/L, and the sodium ion concentration is less than 2mol/L. Most of sodium chloride in the system can be separated out with high selectivity by controlling the adding amount of the chlorine-containing compound, and of course, the higher the adding amount of the chlorine-containing compound is, the higher the separating amount of the sodium chloride is, so that the high-selectivity precipitation of the sodium chloride can be realized by controlling the adding amount of the chlorine-containing compound, and the high-efficiency recovery of lithium ions in the lithium precipitation mother solution is ensured. Further preferably, H in the solution system of the sodium chloride precipitation end point + The concentration is 3-6 mol/L. Further preferably, the concentration of sodium ions in the sodium chloride precipitation end point solution system is 0.5 to 1.5mol/L.
As a preferable mode, the temperature condition for precipitation of sodium chloride is 0-60 ℃. Generally, the lower the temperature is, the more favorable the precipitation of sodium chloride, but refrigeration is required under the condition of the excessively low temperature, and the equipment investment is required to be increased. Therefore, room temperature is further preferred.
As a preferred embodiment, the lithium-containing material may be selected from lithium mica, spodumene, battery material, spent lithium carbonate, lithium phosphate and the like. The leaching process of lithium material is a conventional process in the art.
Compared with the prior art, the technical scheme of the invention has the beneficial technical effects that:
according to the technical scheme, sodium precipitation is carried out on the lithium precipitation mother liquor, so that sodium ions in a high Na/Li chlorination system are separated out in a sodium chloride mode in a high selectivity mode, an open circuit of the sodium ions in the sodium chloride mode is realized, the lithium ions remain in the solution and enter the leaching system again, water-soluble lithium carbonate (the lithium carbonate is slightly soluble in water) in the lithium precipitation mother liquor can be recovered, and meanwhile, the solution is utilized to circularly leach lithium-containing materials, so that the concentration of lithium ions in the leaching solution can be increased, and the efficient recovery of lithium is facilitated.
The technical scheme of the invention has the advantages of short process flow, simplicity, practicability, high economic benefit and the like.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The following examples are intended to illustrate the present invention in further detail, but are not intended to limit the scope of the claims.
Example 1
The lithium deposition mother solution (Li is 0.2mol/L and Na is 4.5 mol/L) in the chlorination system, the solution is alkalescent, concentrated hydrochloric acid (12 mol/L) is continuously added into the lithium deposition mother solution, and the solution is stirred and mixed at room temperature until sodium chloride is separated out, and the solid and the liquid are separated, wherein the solution (Li is 0.17mol/L, na is 0.9mol/L and H is contained in the filtrate) + : about 5 mol/L), the filter cake is sodium chloride, the filter cake is washed by hydrochloric acid (1:1), and then dried, and the mass content of Li in the filter cake is 0.02%. The washing filtrate is mixed with the filtrate and reused for leaching the lithium-containing raw material.
Example 2
The lithium deposition mother solution (Li is 0.1mol/L and Na is 3.4 mol/L) in the chlorination system, the solution is alkalescent, hydrogen chloride gas is continuously introduced into the lithium deposition mother solution, and the solution is stirred and mixed at room temperature untilSeparating out a large amount of sodium chloride, and separating solid from liquid, wherein the concentration of Li is 0.14mol/L, na is 0.87mol/L and H in the filtrate + : 5.1 mol/L), the filter cake is sodium chloride, the filter cake is washed by hydrochloric acid (1:1), and then dried, and the mass content of Li in the filter cake is 0.02%. The washing filtrate is mixed with the filtrate and reused for leaching the lithium-containing raw material.
Example 3
The mixed filtrate in the embodiment 1, lithium manganate, hydrogen peroxide and a proper amount of distilled water are adopted for reaction, the end point pH=2, almost no filter residue exists, sodium hydroxide is adopted for adjusting the pH=11 of the solution, the filter cake is filtered and separated, washing water enters the filtrate, the filtrate is adjusted to be neutral, sodium carbonate is added for precipitating lithium, impurities are washed, the battery grade lithium carbonate is obtained, the filtrate and the washing water are mixed, the filtrate can be evaporated properly when the concentration is lower, and then Na is carried out in the case 1 or 2 + Is an open circuit of (c).
Example 4
The mixed filtrate in the example 1, waste lithium carbonate and a proper amount of distilled water are adopted for reaction, the end point pH=5, insoluble filter residues are filtered, impurities are removed step by step according to the requirement, the purified lithium chloride and sodium chloride mixed solution is obtained, sodium carbonate is added for lithium precipitation operation, impurities are washed, battery grade lithium carbonate is obtained, the filtrate and washing water are mixed, the filtrate can be evaporated properly when the concentration is lower, and then Na is carried out in the case 1 or 2 + Is an open circuit of (c).
Claims (2)
1. A method for recovering lithium from lithium precipitation mother liquor by a closed cycle method comprises the steps of leaching a lithium-containing material by hydrochloric acid to obtain a lithium chloride solution, purifying the lithium chloride solution and precipitating lithium by sodium carbonate to obtain the lithium precipitation mother liquor, and is characterized in that: adding chlorine-containing compounds into the lithium precipitation mother liquor to separate out sodium ions in the lithium precipitation mother liquor in a sodium chloride form, carrying out solid-liquid separation, wherein the solid is sodium chloride, and returning the liquid to the leaching process of the lithium-containing materials; the addition amount of the chlorine-containing compound is used for controlling H in a solution system of a sodium chloride precipitation end point + The concentration is more than 2mol/L, and the sodium ion concentration is less than 2 mol/L;
the ratio of the concentration of sodium ions to the concentration of lithium ions in the lithium precipitation mother solution is higher than 15:1;
the temperature condition for precipitation of sodium chloride is 0-60 ℃.
2. The method for recovering lithium from lithium precipitation mother liquor by a closed cycle method according to claim 1, wherein: the chlorine-containing compound is at least one of HCl gas, chlorine and hydrochloric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210674018.4A CN114959306B (en) | 2022-06-15 | 2022-06-15 | Method for recycling lithium from lithium precipitation mother liquor by closed cycle method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202210674018.4A CN114959306B (en) | 2022-06-15 | 2022-06-15 | Method for recycling lithium from lithium precipitation mother liquor by closed cycle method |
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| Publication Number | Publication Date |
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| CN114959306A CN114959306A (en) | 2022-08-30 |
| CN114959306B true CN114959306B (en) | 2023-11-03 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011168858A (en) * | 2010-02-22 | 2011-09-01 | Eco-System Recycling Co Ltd | Method for producing high concentration lithium solution from lithium-containing liquid, and method for producing lithium carbonate |
| CN105347364A (en) * | 2015-10-30 | 2016-02-24 | 华陆工程科技有限责任公司 | Method for closed-loop recycling of lithium precipitation mother liquor in lithium carbonate production |
| WO2019150403A1 (en) * | 2018-01-30 | 2019-08-08 | Cobat, Consorzio Nazionale Raccolta E Riciclo | Hydrometallurgical process for the treatment of lithium batteries and recovery of the metals contained therein |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6921522B2 (en) * | 1998-07-16 | 2005-07-26 | Chemetall Foote Corporation | Production of lithium compounds directly from lithium containing brines |
| US7390466B2 (en) * | 1999-07-14 | 2008-06-24 | Chemetall Foote Corporation | Production of lithium compounds directly from lithium containing brines |
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2022
- 2022-06-15 CN CN202210674018.4A patent/CN114959306B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011168858A (en) * | 2010-02-22 | 2011-09-01 | Eco-System Recycling Co Ltd | Method for producing high concentration lithium solution from lithium-containing liquid, and method for producing lithium carbonate |
| CN105347364A (en) * | 2015-10-30 | 2016-02-24 | 华陆工程科技有限责任公司 | Method for closed-loop recycling of lithium precipitation mother liquor in lithium carbonate production |
| WO2019150403A1 (en) * | 2018-01-30 | 2019-08-08 | Cobat, Consorzio Nazionale Raccolta E Riciclo | Hydrometallurgical process for the treatment of lithium batteries and recovery of the metals contained therein |
Non-Patent Citations (1)
| Title |
|---|
| 沉锂母液净化处理工艺;顾中苏;龙剑平;谭丽岭;;盐科学与化工(08);全文 * |
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