CN103290217B - Technology for extracting lithium by processing lithium ores through high-pressure steaming process - Google Patents
Technology for extracting lithium by processing lithium ores through high-pressure steaming process Download PDFInfo
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Abstract
The invention discloses a technology for extracting lithium by processing lithium ores through a high-pressure steaming process. The technology comprises the following steps: mixing lithium ore powder with a powdery solid strong alkali for 20-40min to uniformity, directly letting in high-pressure steam, and carrying out dissolving and reacting of the powdery solid strong alkali and the lithium ores through utilizing water in the high-pressure water at a high temperature under a high pressure to completely generate soluble substances. In the invention, the strong alkali in the above reaction materials dissolves through absorbing water molecules in the water steam, so the application amount of the strong alkali can be substantially reduced, and the cost is saved. Lithium, sodium, potassium, rubidium and cesium ions in the lithium ores can be completely dissolved in a solution, so the lithium extraction is convenient, and the lithium yield is high. Fluorine in the lithium ores does not form strong-corrosion hydrofluoric acid corroding apparatuses. Reaction byproducts comprising an alumina sol and a silica sol can be directly sold, so the lithium extraction reaction cost is correspondingly reduced.
Description
Technical field
The present invention relates to a kind of high pressure steam process process lithium ore and put forward lithium technique, belong to field of metallurgy.
Background technology
There is abundant lithium resource in China, the triphane of Koktokay, northwestern Sichuan and the lithionite etc. of Yichuan, all has abundant lithium resource to treat in utilization.The current lithium industrial expansion of China mainly carries lithium from triphane and lithionite, main method comprises: 1, sulfatizing roasting method potassium sulfate roasting method is that first German Wadmen proposes, Frankfort Metallurgical Factory is developed further, is widely used in lithium ore and carries lithium production Quilonum Retard.But this method sylvite consumption is very large and very strict to maturing temperature requirement.The feature that China's Guangzhou Research Institute of Nonferrous Metals is high according to potassium content in Yichun lithia mica, have studied sulphate process roasting one or two sections of leaching novel techniques, novel process has roasting and adds materials few, roasting time and extraction time short, leach liquor lithium concentration is high, steam output is little, energy consumption is low, sylvite can the advantage such as recycle, but there is ring formation in kiln, the aluminium in lithionite, the elements such as silicon can not the deficiency such as Appropriate application.2, sulfuric acid process sulfuric acid process process lithionite is the first roasting under 150-300 DEG C of condition by lithionite concentrate and the vitriol oil, and product of roasting carries out re-baking in 800 DEG C again, makes the lithium in lithionite be converted to water-soluble Lithium Sulphate.The advantage of sulfuric acid process is that logistics capacity is little, material does not need fine grinding after lithionite and roasting, and solid liquid phase easily mixes, and leach simple, the rate of recovery of lithium, potassium is high, and leach liquor lithium concentration is high, steam output is little.When shortcoming is roasting, the vitriol oil is decomposed to form acid mist, pollutes air, needs equipment acid-resistant anti-corrosion.Because the vitriol oil destroys the structure of lithionite, causing part aluminium stripping in lithionite, except needing to consume sodium hydroxide in a large number during aluminium, and making material filtering performance become very poor due to the existence of alumine hydroxide colloid, spent acid is difficult to reclaim simultaneously, does not possess competitive edge economically.3, lime burning method lime burning method be exactly lithionite concentrate and Wingdale is levigate respectively after, roasting in kilns is being turned round than material coal dust after mixing in mechanical slot etc. by metering, maturing temperature controls at 940-1050 DEG C, after roasting completes, leach at normal temperatures with water, the alkali metal in lithionite is all present in leach liquor with hydroxide form.Present method advantage is that technical process is simple, and need not consume valuable industrial chemicals, leaching product is lithium hydroxide, can be directly used in production Quilonum Retard.Shortcoming is that logistics capacity is large, and the quantity of slag is large especially, energy consumption is high, and the rate of recovery of lithium is relatively low, and because economic benefit is not remarkable, this production technique is abroad eliminated already.4, sodium-chlor, sodium sulfate pressure cooking method lithionite concentrate are at about 900 DEG C, water vapor defluorinate roasting is passed in rotary kiln, then boil 3h with sodium-chlor or sodium sulfate 240 DEG C of pressures, the solubility rate of Lithium Oxide 98min can reach more than 95%, and leach liquor entered the concentrated rear available soda ash sinker of purification.Because sodium-chlor and sodium sulfate can be water-soluble and a large amount of reprocessing cycle uses, therefore this technique has that logistics capacity is little, pressure boils that the rear quantity of slag is little, pressure boils that rear material filtering performance is good, filtered liquid lithium concentration is high, washing times is few, low power consumption and other advantages.But the method requires very high to equipment anticorrosion, particularly sodium-chlor pressure cooking method is more serious to equipment corrosion.5, alkali solution technique lithionite and highly basic react under liquid environment, make the lithium in lithionite, sodium, potassium, rubidium, caesium enter in solution, after lithionite powder is molten by alkali, and dilution, then through ion-exchange, capture the positively charged ion in system.Its advantage is: the lithium 100% in lithionite can be allowed to enter (lithionite reaction filter residue returns the molten operation of alkali, realizes complete alkali molten) in solution.Because be react under alkaline liquid environment, the fluorine in lithionite can not generate the hydrofluoric acid of deep-etching.Byproduct is the aluminium silicon sol having extensive use, greatly can be reduced the cost proposing lithium reaction by the direct marketing of aluminium silicon sol.Shortcoming is that the water absorbability of lithium ore powder is strong, and in order to keep the high density of highly basic, must add excessive strong base solution and could maintain to react and carry out under liquid environment, its consequence is exactly that highly basic is excessive more, and cost increase, the process of follow-up alkali collection operation is loaded down with trivial details.
Along with the progress of science and technology, the application of compound in scientific domain of lithium and lithium is more and more wide, and particularly in lithium ion battery, lithium has irreplaceable effect.China's lithium resource enriches, and utilizes new technologies and methods novel method to develop lithium ore and not only can create obvious economic benefit, reduce the dependence to external Quilonum Retard, also prevent the idle waste of resource simultaneously.
Summary of the invention
The present invention is directed to above problem, propose a kind of high pressure steam process process lithium ore and put forward lithium processing method.The present invention proposes the method utilizing high pressure steam process process lithium ore first, with lithium ore powder and powdery solid highly basic for raw material, utilize the water molecules dissolved solids highly basic in high pressure steam, high local concentrations is produced around lithium ore, when High Temperature High Pressure, dissolving limit, solid alkali limit is reacted, until reach lithium ore powder to be converted into soluble substance completely.The method can reduce the highly basic addition in reaction largely, reduces reaction cost, simplifies the difficulty that excess base is reclaimed in aftertreatment, meanwhile, in this production technique, jellyfish liquid recycles, and produces without waste water and gas, byproduct is fully utilized, can environmental requirement be realized.
Technical scheme of the present invention is: a kind of high pressure steam process process lithium ore puies forward lithium technique, lithium ore powder and the mixing of powdery solid highly basic 20-40 minute are to after evenly, directly pass into high pressure steam, utilize the moisture in high pressure steam, dissolving limit, powdery solid highly basic limit in reactant is reacted, under the condition of High Temperature High Pressure, react with lithium ore and generate complete soluble substance.
High pressure steam process process lithium ore puies forward lithium technique, the steps include: 1. will be crushed to lithium ore powder, the powdery solid highly basic lithium ore powder by weight of more than 100 orders: the ratio of highly basic=1:0.5 ~ 5 mixes, put in reactor, start stirring, adopt straight-through method to pass into high pressure steam, utilize the moisture in high pressure steam to participate in reaction, make lithium ore powder and highly basic high-temperature high-voltage reaction 2 ~ 8 hours under the effect of water vapor, cooling, discharging; 2. reaction product is diluted with water to mass percent concentration 0.1% ~ 25%, carries out ion-exchange, the positively charged ion in acquisition system, comprise sodium ion, potassium ion, lithium ion, cesium ion and rubidium ion with Zeo-karb to the material after dilution; Remaining aluminium silicon sol by anionite-exchange resin, then adds a small amount of sodium hydroxide and makees stablizer, regulates PH=8 ~ 10, crystallization, concentrated, obtains the direct marketing of aluminium silicon sol finished product; 3. adsorb cationic ion exchange resin first with water cleaning, then used the diluted acid drip washing of 2% ~ 10%, finally use pure water drip washing to elutant in neutral; 4. elutant is first concentrated to Li+ concentration is 20 ~ 50g/L, is then that the wt% sodium carbonate of 40% ~ 70% reacts 40 ~ 100 minutes at 80 DEG C ~ 100 DEG C temperature with concentration, obtains Quilonum Retard precipitation, filters, washing, dry, obtained standard compliant technical grade Quilonum Retard.
Highly basic comprises sodium hydroxide, potassium hydroxide.Lithium ore comprises lithionite, triphane.The temperature of high pressure steam is 100 ~ 374 DEG C, and pressure is 0.1 ~ 22MPa.
The invention has the advantages that: 1, the water molecules that highly basic in reaction mass absorbs in water vapour dissolves, high local concentrations can be formed around lithium ore, due to the level of response of lithium ore and highly basic and speed and alkali concn, temperature, pressure is directly related, alkali concn is larger, react faster, also more complete, like this, lithium ore reacts with high density highly basic at high temperature under high pressure and generates soluble substance, along with the continuous dissolving of highly basic, reaction is constantly carried out, therefore, the method overcome the deficiency of " method of extracting lithium by processing lepidolite through alkali dissolution process ", the usage quantity of highly basic can be greatly reduced, save cost." method of extracting lithium by processing lepidolite through alkali dissolution process " lithium ore powder and strong base solution is reacted, because the water absorbability of lithium ore powder is strong, in order to keep the high density of highly basic, must add excessive strong base solution could maintain reaction carry out under liquid environment, its consequence is exactly that highly basic is excessive more, cost increase, the process of follow-up alkali collection operation is loaded down with trivial details.2, this technique can allow the lithium in lithium ore, sodium, potassium, rubidium, cesium ion dissolve completely and enter in solution, and make to carry lithium more convenient, yield is higher.3, this technique is owing to being react under alkaline environment, and the fluorine in lithium ore can not generate the hydrofluoric acid of severe corrosive.4, byproduct of reaction aluminium silicon sol can direct marketing, correspondingly reduces the cost proposing lithium reaction.
Accompanying drawing explanation
Fig. 1 represents that the high pressure steam process process lithium ore that the present invention relates to carries lithium process flow diagram.
Embodiment
High pressure steam process process lithium ore puies forward lithium Technology, it is characterized in that: carry out according to the following steps:
1. the lithium ore powder crushed, powdery solid highly basic are mixed in proportion, put in reactor, start strong stirring, straight-through method is adopted to pass into high pressure steam, the moisture in high pressure steam is utilized to participate in reaction, make lithium ore powder and highly basic high-temperature high-voltage reaction under the effect of water vapor, cooling, discharging.
2. reaction product dilute with water, carries out ion-exchange, the positively charged ion in acquisition system with Zeo-karb to the material after dilution, comprises sodium ion, potassium ion, lithium ion, cesium ion and rubidium ion; Remaining aluminium silicon sol by anionite-exchange resin, then adds a small amount of sodium hydroxide and makees stablizer, regulates PH, crystallization, concentrated, obtains the direct marketing of aluminium silicon sol finished product;
3. adsorb cationic ion exchange resin first with water cleaning, then used diluted acid drip washing, finally use pure water drip washing to elutant in neutral;
4. elutant first concentrates, and then reacts with sodium carbonate, obtains Quilonum Retard precipitation, filters, washing, dry, obtained standard compliant technical grade Quilonum Retard.
Below in conjunction with embodiment, the present invention is described in further detail.
The lithionite that the embodiment of the present invention is selected picks up from Yichuan lepidolite ore, and its main chemical compositions is as following table (wt%)
Yichun lithia mica composition detection data
| Composition | Li 2O | Na 2O | K 2O | Rb 2P | Cs 2O | Al 2O 3 | SiO 2 | F | Burn vector |
| Content, % | 4.26 | 1.31 | 8.10 | 1.35 | 0.27 | 22.60 | 52.70 | 5.24 | 3.63 |
Embodiment 1:
(1) 100 object lithionite powder, powdery solid highly basic will be crushed to by weight lithionite powder: the ratio of highly basic=1:0.5 mixes, put in reactor, start strong stirring, adopt straight-through method to pass into high pressure steam, high pressure steam temperature is 100 DEG C, and pressure is 0.1MPa, the moisture in high pressure steam is utilized to participate in reaction, make lithium ore powder and highly basic high-temperature high-voltage reaction 2 hours under the effect of water vapor, cooling, discharging;
(2) reaction product is diluted with water to mass percent concentration 0.1%, carries out ion-exchange, the positively charged ion in acquisition system, comprise sodium ion, potassium ion, lithium ion, cesium ion and rubidium ion with Zeo-karb to the material after dilution; Remaining aluminium silicon sol by anionite-exchange resin, then adds a small amount of sodium hydroxide and makees stablizer, regulates PH=8, crystallization, concentrated, obtains the direct marketing of aluminium silicon sol finished product;
(3) adsorb cationic ion exchange resin first with water cleaning, then used the diluted acid drip washing of 2%, finally use pure water drip washing to elutant in neutral;
(4) elutant is first concentrated to Li+ concentration to 20g/L,
(5) mother liquor after (4) step being concentrated, add concentration be 40% sodium carbonate react 40 minutes at 80 DEG C of temperature;
(6) by reacted for (5) step material filtered while hot, obtain Quilonum Retard crude product, then through washing, dry, obtained standard compliant technical grade Quilonum Retard, the solution after filtration goes to put forward caesium, rubidium operation, washes lithium water and returns preparation sodium carbonate solution.
Embodiment 2:
(1) 700 object lithionite powder, powdery solid highly basic will be crushed to by weight lithionite powder: the ratio of highly basic=1:5 mixes, put in reactor, start strong stirring, adopt straight-through method to pass into high pressure steam, high pressure steam temperature is 180 DEG C, and pressure is 1MPa, the moisture in high pressure steam is utilized to participate in reaction, make lithium ore powder and highly basic high-temperature high-voltage reaction 8 hours under the effect of water vapor, cooling, discharging;
(2) reaction product is diluted with water to mass percent concentration 0.1%, carries out ion-exchange, the positively charged ion in acquisition system, comprise sodium ion, potassium ion, lithium ion, cesium ion and rubidium ion with Zeo-karb to the material after dilution; Remaining aluminium silicon sol by anionite-exchange resin, then adds a small amount of sodium hydroxide and makees stablizer, regulates PH=10, crystallization, concentrated, obtains the direct marketing of aluminium silicon sol finished product;
(3) adsorb cationic ion exchange resin first with water cleaning, then used the diluted acid drip washing of 5%, finally use pure water drip washing to elutant in neutral;
(4) elutant is first concentrated to Li+ concentration to 40g/L,
(5) mother liquor after (4) step being concentrated, add concentration be 50% sodium carbonate react 80 minutes at 90 DEG C of temperature;
(6) by reacted for (5) step material filtered while hot, obtain Quilonum Retard crude product, then through washing, dry, obtained standard compliant technical grade Quilonum Retard, the solution after filtration goes to put forward caesium, rubidium operation, washes lithium water and returns preparation sodium carbonate solution.
Embodiment 3:
(1) 500 object lithionite powder, powdery solid highly basic will be crushed to by weight lithionite powder: the ratio of highly basic=1:3 mixes, put in reactor, start strong stirring, adopt straight-through method to pass into high pressure steam, high pressure steam temperature is 250 DEG C, and pressure is 4MPa, the moisture in high pressure steam is utilized to participate in reaction, make lithium ore powder and highly basic high-temperature high-voltage reaction 5 hours under the effect of water vapor, cooling, discharging;
(2) reaction product is diluted with water to mass percent concentration 1%, carries out ion-exchange, the positively charged ion in acquisition system, comprise sodium ion, potassium ion, lithium ion, cesium ion and rubidium ion with Zeo-karb to the material after dilution; Remaining aluminium silicon sol by anionite-exchange resin, then adds a small amount of sodium hydroxide and makees stablizer, regulates PH=8, crystallization, concentrated, obtains the direct marketing of aluminium silicon sol finished product;
(3) adsorb cationic ion exchange resin first with water cleaning, then used the diluted acid drip washing of 5%, finally use pure water drip washing to elutant in neutral;
(4) elutant is first concentrated to Li+ concentration to 50g/L,
(5) mother liquor after (4) step being concentrated, add concentration be 50% sodium carbonate react 60 minutes at 80 DEG C of temperature;
(6) by reacted for (5) step material filtered while hot, obtain Quilonum Retard crude product, then through washing, dry, obtained standard compliant technical grade Quilonum Retard, the solution after filtration goes to put forward caesium, rubidium operation, washes lithium water and returns preparation sodium carbonate solution.
Embodiment 4:
(1) 200 object lithionite powder, powdery solid highly basic will be crushed to by weight lithionite powder: the ratio of highly basic=1:1.5 mixes, put in reactor, start strong stirring, adopt straight-through method to pass into high pressure steam, high pressure steam temperature is 280 DEG C, and pressure is 6.4MPa, the moisture in high pressure steam is utilized to participate in reaction, make lithium ore powder and highly basic high-temperature high-voltage reaction 3 hours under the effect of water vapor, cooling, discharging;
(2) reaction product is diluted with water to mass percent concentration 12%, carries out ion-exchange, the positively charged ion in acquisition system, comprise sodium ion, potassium ion, lithium ion, cesium ion and rubidium ion with Zeo-karb to the material after dilution; Remaining aluminium silicon sol by anionite-exchange resin, then adds a small amount of sodium hydroxide and makees stablizer, regulates PH=8, crystallization, concentrated, obtains the direct marketing of aluminium silicon sol finished product;
(3) adsorb cationic ion exchange resin first with water cleaning, then used the diluted acid drip washing of 2%, finally use pure water drip washing to elutant in neutral;
(4) elutant is first concentrated to Li+ concentration to 30g/L,
(5) mother liquor after (4) step being concentrated, add concentration be 60% sodium carbonate react 50 minutes at 90 DEG C of temperature;
(6) by reacted for (5) step material filtered while hot, obtain Quilonum Retard crude product, then through washing, dry, obtained standard compliant technical grade Quilonum Retard, the solution after filtration goes to put forward caesium, rubidium operation, washes lithium water and returns preparation sodium carbonate solution.
Embodiment 5:
(1) 200 object lithionite powder, powdery solid highly basic will be crushed to by weight lithionite powder: the ratio of highly basic=1:1.5 mixes, put in reactor, start strong stirring, adopt straight-through method to pass into high pressure steam, high pressure steam temperature is 310 DEG C, and pressure is 9.8MPa, the moisture in high pressure steam is utilized to participate in reaction, make lithium ore powder and highly basic high-temperature high-voltage reaction 3 hours under the effect of water vapor, cooling, discharging;
(2) reaction product is diluted with water to mass percent concentration 12%, carries out ion-exchange, the positively charged ion in acquisition system, comprise sodium ion, potassium ion, lithium ion, cesium ion and rubidium ion with Zeo-karb to the material after dilution; Remaining aluminium silicon sol by anionite-exchange resin, then adds a small amount of sodium hydroxide and makees stablizer, regulates PH=8, crystallization, concentrated, obtains the direct marketing of aluminium silicon sol finished product;
(3) adsorb cationic ion exchange resin first with water cleaning, then used the diluted acid drip washing of 2%, finally use pure water drip washing to elutant in neutral;
(4) elutant is first concentrated to Li+ concentration to 30g/L,
(5) mother liquor after (4) step being concentrated, add concentration be 60% sodium carbonate react 50 minutes at 90 DEG C of temperature;
(6) by reacted for (5) step material filtered while hot, obtain Quilonum Retard crude product, then through washing, dry, obtained standard compliant technical grade Quilonum Retard, the solution after filtration goes to put forward caesium, rubidium operation, washes lithium water and returns preparation sodium carbonate solution.
Claims (2)
1. a high pressure steam process process lithium ore puies forward lithium technique, it is characterized in that: lithium ore powder and the mixing of powdery solid highly basic 20-40 minute are to after evenly, directly passing into temperature is 100 ~ 374 DEG C, pressure is the high pressure steam of 0.1 ~ 22MPa, utilize the moisture in high pressure steam, dissolving limit, powdery solid highly basic limit in reactant is reacted, under the condition of High Temperature High Pressure, reacts with lithium ore and generate complete soluble substance.
2. high pressure steam process process lithium ore puies forward lithium technique according to claim 1, the steps include:
1. lithium ore powder, the powdery solid highly basic lithium ore powder by weight of more than 100 orders will be crushed to: the ratio of highly basic=1:0.5 ~ 5 mixes, put in reactor, start stirring, straight-through method is adopted to pass into high pressure steam, the moisture in high pressure steam is utilized to participate in reaction, make lithium ore powder and highly basic high-temperature high-voltage reaction 2 ~ 8 hours under the effect of water vapor, cooling, discharging; 2. reaction product is diluted with water to mass percent concentration 0.1% ~ 25%, carries out ion-exchange, the positively charged ion in acquisition system, comprise sodium ion, potassium ion, lithium ion, cesium ion and rubidium ion with Zeo-karb to the material after dilution; Remaining aluminium silicon sol by anionite-exchange resin, then adds a small amount of sodium hydroxide and makees stablizer, regulates pH=8 ~ 10, crystallization, concentrated, obtains the direct marketing of aluminium silicon sol finished product; 3. adsorb cationic ion exchange resin first with water cleaning, then used the diluted acid drip washing of 2% ~ 10%, finally use pure water drip washing to elutant in neutral; 4. elutant is first concentrated to Li+ concentration is 20 ~ 50g/L, is then that the wt% sodium carbonate of 40% ~ 70% reacts 40 ~ 100 minutes at 80 DEG C ~ 100 DEG C temperature with concentration, obtains Quilonum Retard precipitation, filters, washing, dry, obtained standard compliant technical grade Quilonum Retard.
3. high pressure steam process process lithium ore puies forward lithium technique according to claim 2, it is characterized in that: highly basic comprises sodium hydroxide, potassium hydroxide.
4. high pressure steam process process lithium ore puies forward lithium technique according to claim 2, it is characterized in that: lithium ore comprises lithionite, triphane.
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| WO2018023159A1 (en) * | 2016-08-02 | 2018-02-08 | Lithium Australia Nl | Caustic digestion process |
| CN109487096A (en) * | 2017-09-09 | 2019-03-19 | 鲁婷 | High pressure steam process processing lithium ore proposes lithium technique |
| CN108645995B (en) * | 2018-04-28 | 2021-02-26 | 宜春市金地锂业有限公司 | Device and method for detecting ore quality after lepidolite mineral separation |
| JP7225681B2 (en) * | 2018-10-26 | 2023-02-21 | 住友金属鉱山株式会社 | Lithium leaching method and lithium recovery method |
| CN109321748B (en) * | 2018-11-12 | 2020-07-17 | 北京科技大学 | Method for extracting lithium and rubidium from lepidolite ore and by-producing zeolite or kaliophilite |
| CN111847488A (en) * | 2020-08-03 | 2020-10-30 | 柴肖芳 | Process for extracting lithium from lepidolite |
| CN115488085A (en) * | 2022-08-11 | 2022-12-20 | 中核龙原科技有限公司 | Method for cleaning residual sodium metal |
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| CN101948124B (en) * | 2010-09-09 | 2012-09-19 | 江西赣锋锂业股份有限公司 | Method for extracting lithium salt from spodumene |
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