CN102502721A - Method for preparing lithium carbonate through extracting lithium from lithium ore - Google Patents
Method for preparing lithium carbonate through extracting lithium from lithium ore Download PDFInfo
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- CN102502721A CN102502721A CN2011103616219A CN201110361621A CN102502721A CN 102502721 A CN102502721 A CN 102502721A CN 2011103616219 A CN2011103616219 A CN 2011103616219A CN 201110361621 A CN201110361621 A CN 201110361621A CN 102502721 A CN102502721 A CN 102502721A
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- quilonum retard
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Abstract
The invention relates to a method for preparing lithium carbonate through extracting lithium from lithium ore. The method comprises the following steps: 1, reacting the lithium ore with fluosilicic acid; 2, filtering; 3, carrying out a fluorine removal reaction; 4, adding water, and dissolving; 5, carrying out a neutralization reaction; and 6, carbonizing to precipitate lithium. The method which allows high energy consumption processes of high temperature roasting and pressurization reacting of the lithium ore in traditional technologies to be not needed and is a method for extracting lithium from the lithium ore through a low temperature process has the characteristics of simple process, low energy consumption and high extraction rate, and makes the comprehensive utilization rate of byproducts be high and the production cost be substantially reduced.
Description
Technical field
The present invention relates to lithium ore comprehensive development and utilization technical field, relate in particular to a kind of low temperature wet method that adopts and from the lithium ore, put forward the method that lithium prepares Quilonum Retard.
Background technology
Lithium is a kind of important strategic property resource material, is the indispensable important raw and processed materials of modern high technology product.The main raw material that extracts lithium is triphane, lithionite, lithium sanidine and salt lake brine.According to different raw materials, the extraction of lithium is divided into from lithium ore and salt lake brine extracts two kinds of methods.
The method that present ore is carried lithium has:
(1) lime sinter process.This method is that lithium ore and Wingdale are prepared burden by 1: 3 (mass ratio), goes out 850-950 ℃ of following high-temperature roasting, ball milling, water logging, obtains containing LiO
2The LiOH solution of 3～4g/l, through sedimentation, filtration, purification, removal of impurities, evaporation, crystallization, drying obtains Lithium Hydroxide MonoHydrate again.This is present main industrial process, and this method raw material is easy to get, cheap, wide material sources, and production technique is simple; But the Wingdale proportioning is high; Need in rotary kiln, decompose a large amount of Wingdales, energy consumption is high, and mass flow is big; Equipment capacity low (the design production capacity of 2.07 * 45 meters rotary kilns of Φ is 800 tons/year), the quantity of slag big (42 tons of slag/ton products), the recovery low (about 67%).
(2) sulphate process.This method is that the lithium ore is mixed high-temperature roasting, ball milling, leaching, purification, evaporation, deposition system Quilonum Retard with auxiliary materials such as vitriolate of tartar.Though this method is superior to lime sinter process, but still there is following problem: the one, the vitriolate of tartar consumption is big, and the cost of vitriolate of tartar is 4～5 times of Wingdale, causes production cost higher; The 2nd, because the adding of vitriolate of tartar descends the furnace charge fusing point, partial melting and sintering very easily appear, the leaching yield of lithium is reduced greatly.
(3) chlorinating roasting.This method is lithium and other alkali metal and the chlorizating agent generation chlorination reaction that under maturing temperature, makes in the lithium ore, generates the corresponding chlorinated thing, from these muriates, extracts various alkali metal cpd products then respectively.Technical process mainly comprises batching system ball, chloridizing roasting, diafiltration stripping, solution purification, condensing crystal, crystallisation by cooling, Quilonum Retard deposition and washing and drying etc.
(4) basic pressure digestion method.This method is with behind the lithium grinde ore, directly adds the water adding calcium hydroxide and in autoclave, presses and boil, and pressing and boiling temperature is 240～260 ℃, and pressure is 2.8Mpa, reacts 4 hours, and the rate of decomposition of lithium ore can reach 95%.But this method calcium hydroxide consumption is big, and energy-saving effect is not remarkable, press temperature, pressure when boiling all very high, and the cost of high pressure leaching plant is also very high.
Through the literature search of prior art is found, because the importance of lithium, it is very active at present ore to be proposed the research of lithium.Like Huang Jifen; People such as Tang Xianliu disclose a kind of technology of pressurized boiling process for preparing lithium carbonate with lithium mica ore and mixed base in patent CN1067028; Be concentrate to be fed water vapor carry out roasting; To bake then material allocate into mixed base (like quicklime, yellow soda ash or sodium hydroxide) grind size mixing, solution purification, evaporation concentration, carbonating carry lithium, the mixed base recycling use, potassium, rubidium, caesium comprehensively reclaim.
Xu Longquan; The bright method that waits the people in patent CN1267636, to disclose a kind of sulfuric acid process to produce battery-level lithium carbonate of great-grandfather is that make the transition roasting, acidizing fired, leaching, purifying treatment, concentration, sinker processing, cleaning, drying treatment, pulverizing, packaged for processing of lithium concentrate formed.Characteristics such as this method has constant product quality, and production technique is simple, makes full use of resource, and cost is low.The suitable raw-material production application of lithium ion battery.
Zhong Hui, Xu Hui disclose a kind of lithium system Li that from lithionite, extracts in patent CN1827527
2CO
3Method, its basic working procedure is: the lithionite ore deposit is added CaF, CaSO
4, Na
2SO
4After carrying out modification by calcination under the certain temperature, ball milling, leaching, filtration add Na with leach liquor again Deng auxiliary material
2CO
3Deposition Li
+, form Li
2CO
3Deposition is filtered the solid that obtains and is Li through washing, drying
2CO
3Product, filtrated stock return and are circulated in deposition Li
+Process, this filtrated stock is separated out K through crystallisation by cooling after 2 circulations
2SO
4, Na
2SO
4Mixing salt returns this mixing salt part and does the baking mixed recycle of auxiliary material and lithionite ore deposit, and another part can be used as the raw material of potassium sulfate making.
Can find out that what at present both at home and abroad carry that the method for lithium adopts from ore all is roasting at high temperature, leaches crystalline technology then, all has the characteristics of energy consumption height, complex process.
Summary of the invention
To the deficiency of prior art, the present invention aims to provide a kind of method of from the lithium ore deposit, extracting lithium, and it is simple that this method has technology, do not need pyroreaction, and energy consumption is low, and the extraction yield of lithium is high, greatly reduces production cost.
The technical scheme that the present invention adopts is:
A kind ofly from the lithium ore, put forward the method that lithium prepares Quilonum Retard, it is characterized in that, said method comprising the steps of:
(1) lithium ore and silicofluoric acid reaction: the lithium ore powder after will pulverizing is put into reaction kettle, by ratio=1 of quality (g) and volume (ml): 1～1: 10 ratio adding silicofluoric acid, heated and stirred was reacted 1.0-3.0 hour;
(2) filter: step (1) gained reaction product is filtered, the gained solid is joined in the defluorination reactor drum;
(3) defluorination reaction: in the defluorination reactor drum, add sulfuric acid and carry out the defluorination reaction, above-mentioned solid reactant and vitriolic mass ratio are 1: 0.1-1: 0.8, and the reaction times is 0.5-4 hour;
(4) be dissolved in water: step (3) gained reaction product is filtered, and the gained solid joins in the dissolution kettle, adds entry in 1: 1～1: 5 ratio of mass ratio, is heated to boiling, stirring and dissolving 2-30 minute;
(5) neutralization reaction: step (4) gained reaction product is filtered, and gained filtrating is sent into neutralization tank, adds ammoniacal liquor and regulates pH value to 4～10;
(6) carbonization sinker: step (5) gained reaction product is filtered, in gained filtrating, add the soluble carbon hydrochlorate, stirring reaction 2-20 minute; Ageing 0.5-2 hour then, filter, the gained solid product is thick Quilonum Retard; Thick Quilonum Retard back washing is dry, promptly get the product Quilonum Retard.
Preferably, the granularity of the lithium ore powder in the step (1) is 80～200 orders.
Preferably, the mass percent concentration of the silicofluoric acid in the step (1) is 10%～50%.
Preferably, the temperature of reaction in the step (1) is 90 ℃-140 ℃.
Preferably, the vitriolic mass percent concentration in the step (3) is 50%-98%.
Preferably, the mass percent concentration of the used ammoniacal liquor of step (4) is 5%～30%.
Preferably, the soluble carbon hydrochlorate is a volatile salt described in the step (6).
Preferably, the mass ratio of filtrating and soluble carbon hydrochlorate is 3: 0.02～3: 1 in the step (6).
The present invention overcome on the traditional technology with the high-temperature roasting of lithium ore; High energy consumption technologies such as compressive reaction; It is a kind of method that adopts the low temperature wet method from the lithium ore, to extract lithium; Have the advantages that technology is simple, energy consumption is low, extraction yield is high, and the sub product comprehensive utilization ratio is high, greatly reduces production cost.
Description of drawings
Fig. 1 is the synoptic diagram that from the lithium ore deposit, extracts the method for lithium of the present invention.
Embodiment
Embodiment 1
(1) will be crushed to 80～200 purpose triphane powder 1000g and put into reaction kettle, adding 1000ml mass percent concentration is 50% silicofluoric acid, is heated to 90 ℃, reacts 1 hour;
(2) reaction product of step (1) is filtered, filter the gained solid and join in the defluorination reactor drum;
(3) in the defluorination reactor drum, adding mass percent concentration is that 50% sulfuric acid carries out the defluorination reaction, and solid reactant and vitriolic mass ratio be 1: 0.8, and the reaction times is 4 hours;
(4) step (3) gained reaction product is filtered, the gained solid joins in the dissolution kettle, adds entry in 1: 1 ratio of mass ratio, is heated to boiling, stirring and dissolving 30 minutes;
(5) step (4) gained reaction product is filtered with pressure filter, gained filtrating is sent into neutralization tank, and the adding mass percent concentration is 5% ammoniacal liquor adjusting pH value to 4;
(6) step (5) gained reaction product is filtered, in gained filtrating, add volatile salt, and the mass ratio of filtrating and volatile salt is 3: 1; Stirring reaction 20 minutes; Ageing is 0.5 hour then, filters with pressure filter, and the gained solid product is thick Quilonum Retard; Thick Quilonum Retard back washing is dry, promptly get the product Quilonum Retard.
Embodiment 2
(1) will be crushed to 80～200 purpose lithionite powder 1000g and put into reaction kettle, adding 10000ml mass percent concentration is 10% silicofluoric acid, is heated to 120 ℃, reacts 3 hours;
(2) reaction product of step (1) is filtered, filter the gained solid and join in the defluorination reactor drum;
(3) in the defluorination reactor drum, adding mass percent concentration is that 98% sulfuric acid carries out the defluorination reaction, and solid reactant and vitriolic mass ratio be 1: 0.1, and the reaction times is 0.5 hour;
(4) step (3) gained reaction product is filtered, the gained solid joins in the dissolution kettle, adds entry in 1: 5 ratio of mass ratio, is heated to boiling, stirring and dissolving 2 minutes;
(5) step (4) gained reaction product is filtered with pressure filter, gained filtrating is sent into neutralization tank, and the adding mass percent concentration is 30% ammoniacal liquor adjusting pH value to 6;
(6) step (5) gained reaction product is filtered, in gained filtrating, add volatile salt, and the mass ratio of filtrating and yellow soda ash is 3: 0.02; Stirring reaction 2 minutes; Ageing is 2 hours then, filters with pressure filter, and the gained solid product is thick Quilonum Retard; Thick Quilonum Retard back washing is dry, promptly get the product Quilonum Retard.
Embodiment 3
(1) will be crushed to 80～200 purpose lithium Feldspar Powder 1000g and put into reaction kettle, adding 3000ml mass percent concentration is 40% silicofluoric acid, is heated to 100 ℃, reacts 1.5 hours;
(2) reaction product of step (1) is filtered, filter the gained solid and join in the defluorination reactor drum;
(3) in the defluorination reactor drum, adding mass percent concentration is that 65% sulfuric acid carries out the defluorination reaction, and solid reactant and vitriolic mass ratio be 1: 0.6, and the reaction times is 2 hours;
(4) step (3) gained reaction product is filtered, the gained solid joins in the dissolution kettle, adds entry in 1: 2 ratio of mass ratio, is heated to boiling, stirring and dissolving 20 minutes;
(5) step (4) gained reaction product is filtered with pressure filter, gained filtrating is sent into neutralization tank, and the adding mass percent concentration is 15% ammoniacal liquor adjusting pH value to 8;
(6) step (5) gained reaction product is filtered, in gained filtrating, add volatile salt, and the mass ratio of filtrating and volatile salt is 3: 0.1; Stirring reaction 10 minutes; Ageing is 1 hour then, filters with pressure filter, and the gained solid product is thick Quilonum Retard; Thick Quilonum Retard back washing is dry, promptly get the product Quilonum Retard.
Embodiment 4
(1) will be crushed to 80～200 purpose triphane powder 1000g and put into reaction kettle, adding 5000ml mass percent concentration is 30% silicofluoric acid, is heated to 140 ℃, reacts 2 hours;
(2) reaction product of step (1) is filtered, filter the gained solid and join in the defluorination reactor drum;
(3) in the defluorination reactor drum, adding mass percent concentration is that 70% sulfuric acid carries out the defluorination reaction, and solid reactant and vitriolic mass ratio be 1: 0.4, and the reaction times is 2 hours;
(4) step (3) gained reaction product is filtered, the gained solid joins in the dissolution kettle, adds entry in 1: 3 ratio of mass ratio, is heated to boiling, stirring and dissolving 10 minutes;
(5) step (4) gained reaction product is filtered with pressure filter, gained filtrating is sent into neutralization tank, and the adding mass percent concentration is 25% ammoniacal liquor adjusting pH value to 10;
(6) step (5) gained reaction product is filtered, in gained filtrating, add yellow soda ash, and the mass ratio of filtrating and volatile salt is 3: 0.5; Stirring reaction 15 minutes; Ageing is 1.5 hours then, filters with pressure filter, and the gained solid product is thick Quilonum Retard; Thick Quilonum Retard back washing is dry, promptly get the product Quilonum Retard.
Embodiment 1～5 gained Quilonum Retard is detected, and the mass percentage content of each composition is seen table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Li 2C O3 | 99.51 | 99.57 | 99.61 | 99.67 |
| Na + | 0.025 | 0.020 | 0.023 | 0.031 |
| K + | 0.001 | 0.002 | 0.002 | 0.003 |
| Fe 3+ | 0.002 | 0.002 | 0.001 | 0.002 |
| Ca 2+ | 0.005 | 0.004 | 0.006 | 0.005 |
| Mg 2+ | 0.002 | 0.001 | 0.001 | 0.002 |
| S0 4 2- | 0.04 | 0.05 | 0.06 | 0.07 |
| Cl - | 0.005 | 0.006 | 0.004 | 0.008 |
Can find out that from table 1 purity of Quilonum Retard according to the invention is all more than 99.5%.
Claims (8)
1. from the lithium ore, put forward the method that lithium prepares Quilonum Retard for one kind, it is characterized in that, said method comprising the steps of:
(1) lithium ore and silicofluoric acid reaction: the lithium ore powder after will pulverizing is put into reaction kettle, by ratio=1 of quality (g) and volume (ml): 1～1: 10 ratio adding silicofluoric acid, heated and stirred was reacted 1.0-3.0 hour;
(2) filter: step (1) gained reaction product is filtered, the gained solid is joined in the defluorination reactor drum;
(3) defluorination reaction: in the defluorination reactor drum, add sulfuric acid and carry out the defluorination reaction, above-mentioned solid reactant and vitriolic mass ratio are 1: 0.1-1: 0.8, and the reaction times is 0.5-4 hour;
(4) be dissolved in water: step (3) gained reaction product is filtered, and the gained solid joins in the dissolution kettle, adds entry in 1: 1～1: 5 ratio of mass ratio, is heated to boiling, stirring and dissolving 2-30 minute;
(5) neutralization reaction: step (4) gained reaction product is filtered, and gained filtrating is sent into neutralization tank, adds ammoniacal liquor and regulates pH value to 4～10;
(6) carbonization sinker: step (5) gained reaction product is filtered, in gained filtrating, add the soluble carbon hydrochlorate, stirring reaction 2-20 minute; Ageing 0.5-2 hour then, filter, the gained solid product is thick Quilonum Retard; Thick Quilonum Retard back washing is dry, promptly get the product Quilonum Retard.
2. as claimed in claim 1ly from the lithium ore, put forward the method that lithium prepares Quilonum Retard, it is characterized in that the granularity of the lithium ore powder in the step (1) is 80～200 orders.
3. as claimed in claim 1ly from the lithium ore, put forward the method that lithium prepares Quilonum Retard, it is characterized in that the mass percent concentration of the silicofluoric acid in the step (1) is 10%～50%.
4. as claimed in claim 1ly from the lithium ore, put forward the method that lithium prepares Quilonum Retard, it is characterized in that the temperature of reaction in the step (1) is 90 ℃-140 ℃.
5. as claimed in claim 1ly from the lithium ore, put forward the method that lithium prepares Quilonum Retard, it is characterized in that the vitriolic mass percent concentration in the step (3) is 50%-98%.
6. as claimed in claim 1ly from the lithium ore, put forward the method that lithium prepares Quilonum Retard, it is characterized in that the mass percent concentration of the used ammoniacal liquor of step (4) is 5%～30%.
7. as claimed in claim 1ly from the lithium ore, put forward the method that lithium prepares Quilonum Retard, it is characterized in that the soluble carbon hydrochlorate is a volatile salt described in the step (6).
8. as claimed in claim 1ly from the lithium ore, put forward the method that lithium prepares Quilonum Retard, it is characterized in that filtrating is 3: 0.02～3: 1 with the mass ratio of soluble carbon hydrochlorate in the step (6).
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495880A (en) * | 2014-12-29 | 2015-04-08 | 宜春市科远化工有限公司 | Method for preparing lithium chloride and byproducts of lithium chloride from lepidolite |
| CN104591232A (en) * | 2014-12-29 | 2015-05-06 | 宜春市科远化工有限公司 | Method for extracting lithium carbonate from Yichun tantalum niobium tailings lithium mica and obtaining by-product |
| CN105152188A (en) * | 2015-08-06 | 2015-12-16 | 昊青薪材（北京）技术有限公司 | Method for preparing lithium carbonate and potassium sulfate by using zinnwaldite |
| CN106044804A (en) * | 2016-05-26 | 2016-10-26 | 四川思达能环保科技有限公司 | Novel process for producing lithium salt by aid of sulfuric acid methods |
| WO2017096646A1 (en) * | 2015-12-08 | 2017-06-15 | 范兵 | Three-in-one preparation process for high-purity lithium carbonate |
| CN107344725A (en) * | 2017-06-29 | 2017-11-14 | 周宇 | The preparation technology of elemental lithium in sulfuric acid straight dipping process extraction lithium ore |
| WO2019015011A1 (en) * | 2017-07-15 | 2019-01-24 | 汕头市泛世矿产资源股份有限公司 | Process for extracting lithium carbonate from amblygonite using acidification method |
| CN110526250A (en) * | 2019-09-27 | 2019-12-03 | 福州大学 | A kind of silicates acid system containing lithium ore directly proposes the method for comprehensive utilization of lithium |
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| CN1059702A (en) * | 1990-09-10 | 1992-03-25 | 新疆有色金属研究所 | The method for preparing Quilonum Retard with the volatile salt precipitation |
| CN101948115A (en) * | 2010-09-14 | 2011-01-19 | 薛彦辉 | Method for processing potassium-containing rocks |
| CN101955211A (en) * | 2010-10-29 | 2011-01-26 | 江西本源新材料科技有限公司 | Method for extracting lithium carbonate from lepidolite |
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2011
- 2011-11-15 CN CN201110361621.9A patent/CN102502721B/en not_active Expired - Fee Related
Patent Citations (3)
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| CN1059702A (en) * | 1990-09-10 | 1992-03-25 | 新疆有色金属研究所 | The method for preparing Quilonum Retard with the volatile salt precipitation |
| CN101948115A (en) * | 2010-09-14 | 2011-01-19 | 薛彦辉 | Method for processing potassium-containing rocks |
| CN101955211A (en) * | 2010-10-29 | 2011-01-26 | 江西本源新材料科技有限公司 | Method for extracting lithium carbonate from lepidolite |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495880A (en) * | 2014-12-29 | 2015-04-08 | 宜春市科远化工有限公司 | Method for preparing lithium chloride and byproducts of lithium chloride from lepidolite |
| CN104591232A (en) * | 2014-12-29 | 2015-05-06 | 宜春市科远化工有限公司 | Method for extracting lithium carbonate from Yichun tantalum niobium tailings lithium mica and obtaining by-product |
| CN105152188A (en) * | 2015-08-06 | 2015-12-16 | 昊青薪材（北京）技术有限公司 | Method for preparing lithium carbonate and potassium sulfate by using zinnwaldite |
| WO2017096646A1 (en) * | 2015-12-08 | 2017-06-15 | 范兵 | Three-in-one preparation process for high-purity lithium carbonate |
| CN106044804A (en) * | 2016-05-26 | 2016-10-26 | 四川思达能环保科技有限公司 | Novel process for producing lithium salt by aid of sulfuric acid methods |
| CN107344725A (en) * | 2017-06-29 | 2017-11-14 | 周宇 | The preparation technology of elemental lithium in sulfuric acid straight dipping process extraction lithium ore |
| WO2019015011A1 (en) * | 2017-07-15 | 2019-01-24 | 汕头市泛世矿产资源股份有限公司 | Process for extracting lithium carbonate from amblygonite using acidification method |
| CN110526250A (en) * | 2019-09-27 | 2019-12-03 | 福州大学 | A kind of silicates acid system containing lithium ore directly proposes the method for comprehensive utilization of lithium |
| CN110526250B (en) * | 2019-09-27 | 2023-01-10 | 福州大学 | Comprehensive utilization method for directly extracting lithium from silicate lithium-containing ore by acid process |
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