CN102337399B - Method for extracting lithium by processing lepidolite through alkali dissolution process - Google Patents
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Abstract
The invention discloses a method for extracting lithium by processing lepidolite through an alkali dissolution process, which comprises the following steps of: enabling the lepidolite to react with alkali in a liquid environment so as to enable the lithium, sodium, potassium, rubidium and cesium in the lepidolite to enter a solution, diluting lepidolite powder after alkali dissolution, and further performing ion exchange to acquire cations in a system. By adopting the method, 100% of the lithium in the lepidolite can enter the solution, reaction filter slag of the lepidolite returns to the alkali dissolution process step, and the complete alkali dissolution is realized. As sodium ions, potassium ions, lithium ions, cesium ions and rubidium ions in the lepidolite are obtained through ion exchange, and the interference of silicon, aluminum, fluorine and other elements in the system is removed, the lithium ions, the cesium ions and the rubidium ions in the lepidolite are easier to be extracted. According to the method, as the reaction is performed in the alkaline liquid environment, the fluorine in the lepidolite can not generate highly-corrosive hydrofluoric acid capable of corroding equipment. A byproduct generated by the method is aluminum silicon sol with a wide range of applications, and the direct selling of the aluminum silicon sol can greatly lower the cost of lithium extraction reaction.
Description
Technical field
The present invention relates to a kind of alkali solution technique and handle the method that lithionite is carried lithium, especially a kind of alkali solution technique is handled the method that lithionite is carried lithium.
Background technology
Make a general survey of both at home and abroad is that the method for raw material production lithium salts has tens kinds approximately with the lithionite; But these methods basically all are enrichment ore and various alkali; Salt or their mixture be fusion or sintering together, further handles sinter with diverse ways then, produces lithium salts.Summary is got up, and roughly has following several kinds:
1) vitriolate of tartar method: by a certain percentage, with lithionite and vitriolate of tartar sintering together at high temperature, at this moment the lithium in the mineral is just replaced by potassium, and reaction result makes lithium change water-soluble Lithium Sulphate into.The aluminium of former mineral, compositions such as silicon generate new silicate minerals with potassium, sodium respectively.For reaction is thoroughly carried out, temperature is not less than 1000 ℃, carries out sintering at 1100 ℃ usually, passes through ball milling, leaching, purification, evaporation then, and deposition makes Quilonum Retard.This method exists the vitriolate of tartar consumption excessive, and cost is higher, the problem that energy consumption is bigger.
2) chloride process: chloride process is exactly with the mixture sintering of triphane with lime carbonate and ammonium chloride.Sintering divides two stages, originally under 250 ℃, brings up to 750 ℃ then.At this moment mineral decompose, and generate lithium chloride, and the solution behind the water extraction can use volatile salt (and bicarbonate of ammonia) that lithium and calcium are precipitated out from solution.The carbonate of gained is used lime treatment again.This reaction corrodibility is stronger, reclaim ammonia.
3) limestone-based process: lithionite is that the roasting of raw material is with a lithionite and two parts of Wingdale mixing calcination, forms mixture after abrasive dust, and Lithium Hydroxide MonoHydrate is leached in entry, and its calcination temperature is between 800 ℃-900 ℃.But the limestone sintering method is big because of the streams flux, energy consumption is high, the lithium recovery is low, product cost is high, is difficult to expand the scale of production.
4) pressurized boiling process for preparing lithium carbonate with lithium mica ore and mixed base (Dianfeng Lithium Industry Co., Ltd., application number/patent No.: 200810127821).This production technique through the high-temperature roasting defluorinate, levigate, press ooze exchange, removal of impurities, concentrate, freezing sodium, carbonization sinker, spinning, the back washing dryings etc. analysed obtain the product Quilonum Retard.This method has advantages such as the lithium yield is higher, recrement is capable of using, sodium salt is capable of circulation, but also exists energy consumption higher generally, and high-temperature roasting defluorinate equipment corrosion is big, and the recrement comprehensive utilization benefit is low.
5) Hao Hai lithium in Jiangxi can Science and Technology Ltd.'s employing Yichuan lithionite ore be a raw material; After the special activation of milling; Sulfuric acid (100～130 ℃) under normal pressure about with 50% leaches reaction, after analyse alum, sinker reaction, realizes extracting Quilonum Retard after the precipitate and separate.Mainly there is acidleach temperature corrosive equipment in this method, and the recrement comprehensive utilization benefit is low.
Consider the production technique of tradition and said extracted lithium salts, its production unit very easily corrodes, and (needing roasting) energy consumption is big, and production process is polluted big; According to the calculation of price of present raw material and product, produce the cost of lithium salts with lithionite and produce the cost of lithium salts, and lose money much larger than bittern and triphane.Have only the employing additive method, and consider comprehensive utilization, just can make lithionite is that raw material production lithium salts technology is achieved.
Summary of the invention
The object of the present invention is to provide a kind of alkali solution technique to handle the method that lithionite is carried lithium; With lithionite powder and strong base solution is raw material; Under the situation of certain temperature and pressure; Reach the dissolving fully of lithionite powder, and utilize the positively charged ion in the method abstraction reaction thing of IX, reach the purpose of efficiently carrying lithium.
Technical scheme of the present invention is: a kind of alkali solution technique is handled the method that lithionite is carried lithium; Lithionite and highly basic react under liquid environment; Lithium, sodium, potassium, rubidium, caesium in the lithionite are got in the solution, after the lithionite powder dissolves through alkali, dilution; Pass through IX again, capture the positively charged ion in the system.
Alkali solution technique is handled the method that lithionite is carried lithium; Its step: the strong base solution that 1. will be crushed to the above lithionite powder, 25%～50% (wt%) of 100 orders is put in the reactor drum by weight the ratio of lithionite powder: strong base solution=1:3～8; Start stirring; Under 100～250 ℃, 6～10 atmospheric situation, reacted 2～8 hours, cooling is filtered; 2. reaction solution is diluted with water to weight ratio 2%～15%, with Zeo-karb the material after diluting is carried out IX, and the positively charged ion in the acquisition system comprises sodium ion, potassium ion, lithium ion, cesium ion and rubidium ion; Remaining aluminium silicon sol adds small amounts of sodium hydroxide again and makees stablizer through anionite-exchange resin, regulates pH=8～10, and crystallization, concentrated obtains the direct marketing of aluminium silicon sol finished product; 3. adsorbed the at first water cleaning of cationic ion exchange resin, used 2%～10% diluted acid drip washing again, be neutral with pure water drip washing to elutant at last; 4. elutant is concentrated to Li earlier
+Concentration is 20～50g/L, and the yellow soda ash with 40%～70% (wt%) reacted 40～100 minutes under 80 ℃～100 ℃ temperature then, obtains the Quilonum Retard deposition, filter, and washing, oven dry makes standard compliant technical grade Quilonum Retard.
Highly basic comprises sodium hydroxide, Pottasium Hydroxide.The Zeo-karb that carries out IX comprises: strongly acidic cationic exchange resin and weakly acidic cation-exchange resin; The anionite-exchange resin that carries out IX comprises strongly basic anion exchange resin and weakly basic anion exchange resin.The diluted acid that cationic ion exchange resin has been adsorbed in drip washing comprises: sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, oxalic acid.Solution after lithionite powder alkali dissolves obtains the aluminium silicon sol through IX.
The invention has the advantages that: present method can let the lithium 100% in the lithionite get in the solution, and lithionite reaction filter residue returns alkali and dissolves operation, realizes that complete alkali dissolves.Because wherein sodium ion, potassium ion, lithium ion, cesium ion and rubidium ion are to obtain through IX, the interference of having removed elements such as silicon, aluminium, fluorine in the system makes wherein lithium ion, cesium ion, rubidium ion be extracted more easily.Present method is because be reaction under the alkaline liq environment, and the fluorine in the lithionite can not generate the hydrofluoric acid etching apparatus of deep-etching.The sub product of present method is the aluminium silicon sol that extensive use is arranged, and the direct marketing through the aluminium silicon sol can reduce the cost of proposing the lithium reaction greatly.
Description of drawings
Fig. 1 handles the method process flow sheet that lithionite is carried lithium for alkali solution technique of the present invention.
Embodiment
Below in conjunction with embodiment the present invention is done further detailed description.
The lithionite that the embodiment of the invention is selected for use picks up from lithionite ore deposit, Yichuan, its main chemical compositions such as following table (wt%)
Table 1 Yichun lithia mica composition detection data
| Form | Li 2O | Na 2O | K 2O | Rb 2P | Cs 2O | Al 2O 3 | SiO 2 | F | Vector burns |
| Content | 4.26 | 1.31 | 8.10 | 1.35 | 0.27 | 22.60 | 52.70 | 5.24 | 3.63 |
Embodiment 1:
The strong base solution that (1) will be crushed to 700 purpose lithionite powder, 50% (wt%) is put in the voltage-resistant reactor by weight the ratio of lithionite powder: strong base solution=1:8; Start stirring; Reaction is 8 hours under 250 ℃, 10 atmospheric situation, and cooling is filtered.In the solid Returning reactor after the filtration, continue reaction next time.
(2) to be diluted with water to concentration be 2% (wt%) to reaction solution, carries out IX, the positively charged ion in the acquisition system with the material of weakly acidic cation-exchange resin after to dilution.Remaining aluminium silicon sol is removed the fluorion in the solution through weakly basic anion exchange resin, adds small amounts of sodium hydroxide again and makees stablizer, regulates pH=8, through crystallization, concentrated, obtains the direct marketing of aluminium silicon sol finished product again.
(3) adsorbed cationic ion exchange resin at first water clean, using concentration again is 3% dilute sulphuric acid drip washing, is neutrality with pure water drip washing to elutant at last.
(4) concentrate: elutant is concentrated to Li earlier
+Concentration is 40g/L;
(5) sinker: (4) are gone on foot the mother liquor after concentrating, and the yellow soda ash that adds 50% (wt%) concentration carries out sinker reaction 60 minutes under 95 ℃ of temperature;
(6) separate: with the reacted material filtered while hot of (5) step sinker, obtain the Quilonum Retard bullion, carry out drying after the drip washing with pure water, obtain the technical grade lithium carbonate product, the solution after the filtration goes to put forward caesium, rubidium operation, washes lithium water and returns preparing sodium carbonate solution.
Embodiment 2:
The strong base solution that (1) will be crushed to 100 purpose lithionite powder, 25% (wt%) is put in the voltage-resistant reactor by weight the ratio of lithionite powder: strong base solution=1:3; Start stirring; Reaction is 2 hours under 100 ℃, 6 atmospheric situation, and cooling is filtered.In the solid Returning reactor after the filtration, continue reaction next time.
(2) to be diluted with water to concentration be 5% (wt%) to reaction solution, carries out IX, the positively charged ion in the acquisition system with the material of weakly acidic cation-exchange resin after to dilution.Remaining aluminium silicon sol is removed the fluorion in the solution through weakly basic anion exchange resin, adds small amounts of sodium hydroxide again and makees stablizer, regulates pH=8, through crystallization, concentrated, obtains the direct marketing of aluminium silicon sol finished product again.
(3) adsorbed cationic ion exchange resin at first water clean, using concentration again is 3% dilute sulphuric acid drip washing, is neutrality with pure water drip washing to elutant at last.
(4) elutant is concentrated to Li earlier
+Concentration is 20g/L;
(5) mother liquor after will concentrating, the yellow soda ash that adds 40% (wt%) concentration carries out sinker reaction 40 minutes under 80 ℃ of temperature;
(6) with the reacted material filtered while hot of sinker, obtain the Quilonum Retard bullion, carry out drying after the drip washing with pure water, obtain the technical grade lithium carbonate product, the solution after the filtration goes to put forward caesium, rubidium operation, washes lithium water and returns preparing sodium carbonate solution.
Embodiment 3:
The strong base solution that (1) will be crushed to 200 purpose lithionite powder, 35% (wt%) is put in the voltage-resistant reactor by weight the ratio of lithionite powder: strong base solution=1:6; Start stirring; Reaction is 6 hours under 190 ℃, 8 atmospheric situation, and cooling is filtered.In the solid Returning reactor after the filtration, continue reaction next time.
(2) to be diluted with water to concentration be 10% (wt%) to reaction solution, carries out IX, the positively charged ion in the acquisition system with the material of strongly acidic cationic exchange resin after to dilution.Remaining aluminium silicon sol is removed the fluorion in the solution through weakly basic anion exchange resin, adds small amounts of sodium hydroxide again and makees stablizer, regulates pH=8, through crystallization, concentrated, obtains the direct marketing of aluminium silicon sol finished product again.
(3) adsorbed cationic ion exchange resin at first water clean, using concentration again is 5% dilute sulphuric acid drip washing, is neutrality with pure water drip washing to elutant at last.
(4) elutant is concentrated to Li earlier
+Concentration is 50g/L;
(5) mother liquor after will concentrating, the yellow soda ash that adds 60% (wt%) concentration carries out sinker reaction 100 minutes under 90 ℃ of temperature;
(6) with the reacted material filtered while hot of sinker, obtain the Quilonum Retard bullion, carry out drying after the drip washing with pure water, obtain the technical grade lithium carbonate product, the solution after the filtration goes to put forward caesium, rubidium operation, washes lithium water and returns preparing sodium carbonate solution.
Embodiment 4:
The strong base solution that (1) will be crushed to 500 purpose lithionite powder, 40% (wt%) is put in the voltage-resistant reactor by weight the ratio of lithionite powder: strong base solution=1:5; Start stirring; Reaction is 4 hours under 150 ℃, 8 atmospheric situation, and cooling is filtered.In the solid Returning reactor after the filtration, continue reaction next time.
(2) to be diluted with water to concentration be 15% (wt%) to reaction solution, carries out IX, the positively charged ion in the acquisition system with the material of strongly acidic cationic exchange resin after to dilution.Remaining aluminium silicon sol is removed the fluorion in the solution through strongly basic anion exchange resin, adds small amounts of sodium hydroxide again and makees stablizer, regulates pH=9, through crystallization, concentrated, obtains the direct marketing of aluminium silicon sol finished product again.
(3) adsorbed cationic ion exchange resin at first water clean, using concentration again is 5% dilute sulphuric acid drip washing, is neutrality with pure water drip washing to elutant at last.
(4) elutant is concentrated to Li earlier
+Concentration is 45g/L;
(5) mother liquor after will concentrating, the yellow soda ash that adds 70% (wt%) concentration carries out sinker reaction 50 minutes under 90 ℃ of temperature;
(6) with the reacted material filtered while hot of sinker, obtain the Quilonum Retard bullion, carry out drying after the drip washing with pure water, obtain the technical grade lithium carbonate product, the solution after the filtration goes to put forward caesium, rubidium operation, washes lithium water and returns preparing sodium carbonate solution.
Claims (4)
1. an alkali solution technique is handled the method that lithionite is carried lithium, its step:
1. will be crushed to 100 orders above lithionite powder, concentration and be 25%～50% wt% strong base solution puts in the reactor drum by weight the ratio of lithionite powder: strong base solution=1:3～8; Start stirring; Under 100～250 ℃, 6～10 atmospheric situation, reacted 2～8 hours; Cooling is filtered;
2. reaction solution is diluted with water to weight ratio 2%～15%, with Zeo-karb the material after diluting is carried out IX, and the positively charged ion in the acquisition system comprises sodium ion, potassium ion, lithium ion, cesium ion and rubidium ion; Remaining aluminium silicon sol adds small amounts of sodium hydroxide again and makees stablizer through anionite-exchange resin, regulates pH=8～10, and crystallization, concentrated obtains the direct marketing of aluminium silicon sol finished product;
3. adsorbed the at first water cleaning of cationic ion exchange resin, used 2%～10% diluted acid drip washing again, be neutral with pure water drip washing to elutant at last;
4. elutant is concentrated to Li earlier
+Concentration is 20～50g/L, is that 40%～70% wt% yellow soda ash reacted 40～100 minutes under 80 ℃～100 ℃ temperature with concentration then, obtains the Quilonum Retard deposition, filter, and washing, oven dry makes standard compliant technical grade Quilonum Retard.
2. handle the method that lithionite is carried lithium according to the said alkali solution technique of claim 1, it is characterized in that: highly basic comprises sodium hydroxide, Pottasium Hydroxide.
3. handle the method that lithionite is carried lithium according to the said alkali solution technique of claim 1, it is characterized in that: the Zeo-karb that carries out IX comprises: strongly acidic cationic exchange resin and weakly acidic cation-exchange resin; The anionite-exchange resin that carries out IX comprises strongly basic anion exchange resin and weakly basic anion exchange resin.
4. handle the method that lithionite is carried lithium according to the said alkali solution technique of claim 1, it is characterized in that: the diluted acid that cationic ion exchange resin has been adsorbed in drip washing comprises: sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, oxalic acid.
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| CN104140116A (en) * | 2014-06-06 | 2014-11-12 | 江西江锂新材料科技有限公司 | Method for preparing lithium hydroxide monohydrate by adopting method for autoclaving lepidolite with potassium sulfate |
| CN104876225A (en) * | 2015-05-12 | 2015-09-02 | 云南云天化股份有限公司 | Method for separating residual fluorine from by-product silica gel prepared in process of producing fluoride salt from fluorosilicic acid |
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| CN108118143B (en) * | 2017-12-27 | 2021-10-01 | 中南大学 | Method for preparing lithium carbonate by extracting lithium from lepidolite through two-stage chlorination roasting-alkali liquor leaching method |
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| CN108996532B (en) * | 2018-09-12 | 2020-07-24 | 江西海汇龙洲锂业有限公司 | Method for recovering rubidium, cesium, aluminum and potassium from mixed vanadium of by-products of lithium extraction from lepidolite |
| CN111019407B (en) * | 2019-12-16 | 2021-06-15 | 江西省科学院应用化学研究所 | Method for preparing electrolytic aluminum carbon anode antioxidant coating by treating lepidolite lithium extraction mother liquor through alkali dissolution method and product |
| CN118545938A (en) * | 2024-04-17 | 2024-08-27 | 华筑绿建(北京)科技有限公司 | Solidified lepidolite slag cementing material and preparation method and application thereof |
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| CN1029112C (en) * | 1992-06-23 | 1995-06-28 | 中南工业大学 | Pressurized boiling process for preparing lithium carbonate with lithium mica ore and mixed base |
| CN100439245C (en) * | 2006-03-15 | 2008-12-03 | 周明辉 | Preparation method of acid swellable mica |
| CN100503849C (en) * | 2006-11-24 | 2009-06-24 | 江西赣锋锂业股份有限公司 | Method for producing refined lithium sulfate solution used in lepidolite lithium-extracting technique by sulfuric acid process |
| CN101302018B (en) * | 2008-07-02 | 2010-08-11 | 江西赣锋锂业股份有限公司 | Method for preparing lithium carbonate by extracting lithium from lepidolite |
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