CN101875497A - Production process for extracting lithium from raw brine of high magnesium-lithium ratio lithium salt-containing lake - Google Patents
Production process for extracting lithium from raw brine of high magnesium-lithium ratio lithium salt-containing lake Download PDFInfo
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Abstract
The invention relates to a production process for extracting lithium from raw brine of a high magnesium-lithium ratio lithium salt-containing lake, which comprises the following steps: (1) tedding raw brine of a high magnesium-lithium ratio lithium salt-containing lake on a brine pan; (2) tedding solid-liquid products and a solid mixed ore-cleaning solution mixture of previous batch, and dissolving by heating; (3) concentrating by evaporation; (4) cooling the concentrated mixture, and separating out solid mixed ores by crystallization; (5) filtering, and separating to obtain a condensed saturated low magnesium-lithium ratio mother solution and lithium-containing solid mixed ores; (6) carrying out magnesium removal and lithium precipitation on the saturated low magnesium-lithium ratio mother solution to obtain lithium carbonate; (7) adding an amount of fresh water to the lithium-containing solid mixed ores, thoroughly mixing, and cleaning; (8) carrying out solid-liquid separation to obtain a cleaning solution and solid salts, and discarding the solid salts or using the solid salts as raw materials for producing magnesium salts; and (9) returning to the step (2) with the cleaning solution. Compared with a common process, the process of the invention reduces the magnesium-lithium ratio in raw brine from more than 10 to lower than 3, increases the lithium content in raw brine to more than 1.5%, greatly lowers the magnesium removal cost in the lithium extracting process, improves the yield of lithium, and has the advantages of low energy consumption, convenient operation and low production cost.
Description
Technical field
The present invention relates to a kind of production technique, especially relate to and a kind ofly contain the production technique that the old halogen in lithium salts lake is carried lithium system Quilonum Retard with high Mg/Li ratio with the old stew in soy sauce Quilonum Retard in salt lake.
Background technology
Lithium is a kind of important strategic resource, uses very extensive.Be mainly used in fields such as glass, pottery and lithium cell.Because lithium ion battery energy height is in light weight, become the important component part of aerospace operations.Quilonum Retard is as one of a kind of most important lithium salts, its demand is along with the growth of global economy constantly increases, price is also raised on the way, under the powerful drive of global lithium cell market growth, grow up steadily in lithium cell novel material market, the world market on average increases progressively 5%～6% to the demand of Quilonum Retard every year.
China is lithium resource big country, and explored lithium ore resources industrial reserves occupies the whole world the second, but wherein the bittern lithium accounts for 79% of total reserves, and mainly is distributed in the salt lake in Qinghai and Tibet.The solid lithium ore resources of China is along with the decline of ore grade, and production cost sharply rises, and has seriously restricted the production and the development of lithium salts enterprise, and the lithium salts manufacturing enterprise that has closes down.The nineties in last century, China is lithium salts export State, and at present, and the market requirement of domestic lithium salts industrial development is satisfied in a large amount of imports of having had to of lithium salts such as industrial required Quilonum Retard.The scientific and technical personnel of domestic units concerned have carried out a large amount of research and unremitting effort to the extraction process of lithium in the ground salt lake brines such as Qinghai, the existing breakthrough, but still exist technology immature, disadvantages such as production cost height.
Because salt lake brine lithium resource reserves account for 70～80% of lithium resource total amount, so salt lake brine is put forward the main means that lithium has become lithium salts production.In recent years, Atacama (Atacama) salt lake of Chile, the Sears of the U.S. (Searles) lake, silver-colored peak (SilverPeak) lake subsurface brine and Argentinian HombeMuerto salt lake form stronger throughput.The global at present lithium salts product of producing from bittern is (with Li
2CO
3Meter) accounted for more than 85% of product population.
Since the nineties in last century, the operational path of lithium is carried in countries in the world to salt lake brine research also begins to enter into from small-scale test the extension research of situ extraction technology.
Generally speaking, the domestic and international technology of extraction separation lithium salts from salt lake brine, conclusion is got up, and mainly contains evaporative crystallization method, the precipitator method, extraction process, ion exchange adsorption, calcining leaching method, Xu Shi method and electroosmose process etc.Wherein the precipitator method, extraction process, ion exchange adsorption and carborization are studied extensively and profoundly, are that main salt lake brine is put forward the lithium method, and extracting the lithium salts the finished product from bittern generally all is Quilonum Retard.
The precipitator method: the precipitator method are carried lithium and are comprised methods such as carbonate precipitation method, hydration Lithium Sulphate crystalline deposit method from salt lake brine.Carbonate precipitation method is carried lithium from salt lake brine be to study the earliest and in the method for industrial application, this method is calcined soda for industry to be added lithium is separated out with the Quilonum Retard form.This method is suitable for the salt lake brine of low Mg/Li ratio and carries lithium.This method exploitation Li is all adopted in U.S. Sears lake, lithium ore deposit, silver-colored peak and Chilean Atacama salt lake
2CO
3Product.The hydration Lithium Sulphate crystalline deposit method existing reported in literature eighties in last century, but gained Li
2SO
4H
2O purity＜95%, the rate of recovery＜76%.Recently, obtain two kinds of different bittern of forming by human Atacama salt lake brine evaporation concentration, the Lithium Sulphate after mixing in the bittern surpasses its solubleness, divides three phases to be settled out Li again
2SO
4H
2The O crystal.Li
2SO
4H
2O purity can reach 98.97%, and the total yield of lithium reaches 73.3%.This method does not need to add in addition chemical feedstocks, comparatively is suitable for the sulfate type salt lake bittern of low Mg/Li ratio, is not suitable for carrying lithium from the high Mg/Li ratio salt lake brine.
In recent years, carbonate precipitation method is used for from the report of high Mg/Li ratio salt lake brine extraction Quilonum Retard have been appearred in China.Lu Zeng etc. utilize the solar evaporation pond that the salt lake intercrystalline bittern is carried out spontaneous evaporation and concentrate, and fractional crystallizaton separates and adds precipitation agent, and the Quilonum Retard precipitation is separated out, and through separation, drying, make lithium carbonate product.Technological process adopts Crystallization Separation stage by stage, the by-product multiple product.Wang Rigong etc. reach supersaturation concentration with the high Mg/Li ratio salt lake brine 40～100 ℃ of scope inner control, under the state of insulation, be pumped into immediately in the vibration knockout tower of belt stirrer, add yellow soda ash, and stir simultaneously and vibrate, leave standstill the back separated in synchronization and go out magnesiumcarbonate and Quilonum Retard, this method magnesium lithium separates not thorough, and Quilonum Retard purity is not high, and yield is on the low side.
Solvent extration:, once studied multiple extraction agent both at home and abroad and extract and propose lithium research, as phosphorous organic extractant, amine extractant, diketone, ketone, alcohol, crown ether, mixed extractant etc. at the especially high magnesium chloride salt lake brine of bittern system.The extraction system of lithium can reach separating effect preferably as being that the extraction system of extraction agent is studied morely with trioctyl phosphine oxide [TOPO] to lithium and other alkalimetal ion.Separation factor in the external at present report
β Li/NaThe highlyest can reach 1620, adopt acyl group pyrazolone compounds and TOPO to neutrallty condition, to extract lithium in acidity.
At present, the experimental size of proposing lithium research with the TBP extraction process in China greatly and the most deep, all there is research in units such as the Chinese Academy of Sciences, Qinghai Province's related production enterprise, colleges and universities, it is the most effective to carry lithium from high Mg/Li ratio bittern, be that the salt lake high Mg/Li ratio bittern with prospects for commercial application is put forward one of lithium method, but this method remain the problems such as molten damage at technical process length, equipment corrosion and extraction agent at present.
Ion exchange adsorption: more about the synthetic report with experimental study of lithium adsorbent, this method mainly is applicable to from contain the lower bittern of lithium carries lithium.Studies show that at present lithium adsorbent more likely is a Manganse Dioxide, MnO
2Ion(ic)sieve is to Li
+Special selection adsorptivity is arranged, and this method is the lithium manganese oxide presoma that earlier lithium salts and Mn oxide reaction generation is had the cubic spinel structure, and it removes Li in the lattice by acid
+And change the λ-MnO of spinel structure into
2, λ-MnO
2Adsorb the Li in the salt lake brine again
+Be reduced to the lithium manganese oxide of normal spinel structure, extract lithium ion with the HCl eluant solution again, be applicable to salinity height, Ca
2+And Mg
2+The bittern that concentration is big.The Japan scholar will make lithium adsorbent H
1.6Mn
1.6O
4, the adsorptive power of lithium in the seawater is reached 40mg/g, the highest in the present various sorbent materials of studying.
The Zhang Shaocheng of Chinese Academy of Sciences Qinghai salt lake institute contains lithium salts lake bittern water and salt pan at high Mg/Li ratio and concentrates and contain the old halogen of lithium, has invented aluminium salt type sorbent material LiClAl
2(OH)
3NH
2O, with granulations such as high molecular polymer cellulose acetate butyrates, sorbent material work loading capacity is 2～3mgLi
+/ g, absorption-desorption device and water or 0.02～4g/LiCl solution fractionation adverse current wash-out, the lithium yield reaches 92%.This invented technology flow process is simple, the water wash-out and need not acid, reduced cost.But compare with manganese bioxide ionic sieve, little, the molten damage of aluminium salt type ion exchange absorbent exchange capacity is bigger.
Calcination method: this method is that the bittern evaporation that will carry behind the boron anhydrates 50%, obtain four aqueous magnesium chlorides, 700 ℃ of calcination 2 hours, obtain magnesium oxide, add water extraction lithium (it is 0.14% that leaching liquid contains Li) then, remove impurity such as calcium, magnesium with milk of lime and soda ash, solution evaporation is concentrated into to contain Li be about 2%, add soda ash and be settled out Quilonum Retard, the yield about 90% of lithium.Can obtain the magnesium oxide byproduct of purity 98.5% after magnesium oxide slag after the calcination is refining.This method helps fully utilizing resources such as lithium magnesium, and raw material consumption is few, but the utilization of magnesium makes the flow process complexity, and equipment corrosion is serious, and the water yield that need evaporate is big, power consumption is big.
Electroosmose process: in recent years, the Ma Peihua of Chinese Academy of Sciences Qinghai salt lake institute etc. has carried out the research of electroosmose process separating magnesium and concentrated lithium from salt lake brine.This method will contain magnesium lithium salts lake bittern water or the salt pan Exposure to Sunlight concentrates old halogen (Mg/Li weight ratio 1: 1～300: 1) by one or more levels electrodialyzer, utilize monovalent cation selective ion exchange membrane and univalent anion selective ion exchange membrane (continous way, sequential portion the is circulating or the batch circulation formula) technology that circulates to concentrate lithium, the mother liquor reusable edible of generation.The single extraction rate reached of lithium is more than 80% in this method, the decreasing ratio of magnesium 〉=95%, the decreasing ratio of boron 〉=99%, the decreasing ratio of sulfate ion 〉=99%, solved that lithium separates with other ionic with magnesium in the high Mg/Li ratio salt lake brine, realized comprehensive utilizations of resources such as salt lake lithium, boron, potassium.But production cost is higher relatively.
Summary of the invention
The object of the present invention is to provide a kind of high Mg/Li ratio salt lake brine to put forward the production technique of lithium,, reduce production costs to make full use of lithium resource.
Target of the present invention is achieved through the following technical solutions: it may further comprise the steps: (1) contains the salt pan high Mg/Li ratio that the old halogen in lithium salts lake (Mg/Li ratio of the old halogen in described salt lake can more than 10) teds, concentrates, crystallization, obtains to ted the solid-liquid product; (2) step (1) gained is tedded the solid-liquid product and mix (blending ratio is not limit) with last batch solid mixing ore deposit washings, heat temperature raising is to 〉=80 ℃, all dissolves to solids; (3) step (2) gained mixed solution continues heat temperature raising to boiling, and temperature is 110 ℃～120 ℃, evaporation concentration, and evaporation diminishing amount is the 5wt%～20wt% of amount of the mixture; (4) enriched mixture that step (3) is obtained is cooled to normal temperature, and sufficient crystallising is separated out and contained lithium solid mixing ore deposit, and solid-liquid separation must concentrate saturated low Mg/Li ratio mother liquor and contain lithium solid mixing ore deposit; (5) the saturated low Mg/Li ratio mother liquor that step (4) is obtained carries out the demagging sinker, the system Quilonum Retard; (6) the lithium solid mixing ore deposit that contains that step (4) is obtained adds an amount of fresh water, adds 5wt%～20wt% that the fresh water amount is the solid mineral total amount, fully stirs, and washs; (7) solidliquid mixture behind step (6) agitator treating is carried out solid-liquid separation, get washing lotion and solid salt, solid salt abandons or is used as production magnesium salts raw material; (8) step (7) gained washing lotion is returned step (2), ted the solid-liquid product with step (1) gained and mix.
Described high Mg/Li ratio contains the old halogen in lithium salts lake, is generally the old halogen of chloride type or sulfate type salt lake.
Abandoning the solid ore deposit after the described washing is magnesium chloride or sal epsom, and wherein lithium content is less than 0.05wt%.
Technology of the present invention is compared with ordinary process, has reduced the Mg/Li ratio in the old halogen significantly, and Mg/Li ratio reaches more than 1.5% by lithium content in the old halogen after this art breading from reducing to more than 10 below 3 in the old halogen; Thereby reduced the cost of proposing demagging in the lithium process significantly; Increase substantially the yield of lithium; Energy consumption is low, and is easy and simple to handle, and production cost is low, good in economic efficiency.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
The invention will be further described below in conjunction with embodiment.
Per-cent is mass percent described in each embodiment.
Embodiment 1
(1) with the old halogen in certain salt lake, by existing known method ted, concentrate, crystallization, obtain to ted the solid-liquid product, solid-to-liquid ratio is 11.2:4.5; This solid mixing ore deposit magnesium, lithium content are respectively Li
+0.40%, Mg
2+10.75%; Ted in the solid-liquid product, magnesium, the lithium content of liquid are respectively Li
+0.95%, Mg
2+7.975;
(2) take by weighing step (1) gained and ted solid-liquid product 100k, mix with last crowd solid mixing ore deposit washings 10kg, heat temperature raising to 86 ℃, the solid mineral in the mixture all dissolves;
(3) step (2) gained mixed solution is continued to be heated to boiling, system temperature is 112 ℃, evaporation diminishing 10Kg;
(4) step (3) gained mixed solution is cooled to normal temperature, sufficient crystallising is separated out solid mixing ore deposit, and solid-liquid separation obtains concentrated saturated low Mg/Li ratio mother liquor of 35kg and 65kg and contains lithium solid mixing ore deposit, and mother liquor magnesium, lithium content are respectively Li
+1.79%, Mg
2+5.25%, magnesium, the lithium content in solid mixing ore deposit are respectively Li
+0.51%, Mg
2+10.73%;
(5) step (4) gained is concentrated saturated low Mg/Li ratio mother liquor and go on foot sinker by heavy magnesium one of two steps, make Quilonum Retard, heavy magnesium of two steps is respectively the ammoniacal liquor of the first step with 15kg1:1, and second step was used the NaOH of 8.75kg40%, used the Na of 14kg40% at last
2CO
3Sinker, the Quilonum Retard purity that makes reaches 90.5%;
(6) step (4) gained is contained lithium solid mixing ore deposit and add an amount of fresh water, adding the fresh water amount is 10% of solid mineral total amount, fully stirs, and washs; Magnesium, the lithium content of washing back solid mineral are respectively Li
+0.042%, Mg
2+11.39%; Get wash water 10kg;
(7) solid-liquid separation gets wash water and solid salt, and solid salt abandons or be used as production magnesium salts raw material;
(8) wash water returns (2) and teds the solid-liquid product and mix rising temperature for dissolving.
Embodiment 2
Step (1) (2) is with embodiment 1 step (1), (2);
(3) with step (2) gained mixed solution heat temperature raising to 113 ℃, evaporation at constant temperature 18kg moisture;
(4) mixed solution behind step (3) evaporation at constant temperature is cooled to normal temperature, sufficient crystallising is separated out solid mixing ore deposit, and solid-liquid separation obtains concentrated saturated low Mg/Li ratio mother liquor of 27kg and 65kg and contains lithium solid mixing ore deposit, and mother liquor magnesium, lithium content are respectively Li
+2.08%, Mg
2+5.66%, magnesium, the lithium content in solid mixing ore deposit are respectively Li
+0.54%, Mg
2+10.65%;
(5) the saturated low Mg/Li ratio mother liquor of step (4) gained is gone on foot sinker by heavy magnesium one of two steps and make Quilonum Retard, heavy magnesium of two steps is respectively the ammoniacal liquor of the first step with 15kg1:1, and second step was used the NaOH of 8.75kg40%, used the Na of 14kg40% at last
2CO
3Sinker makes Quilonum Retard purity and reaches 92.5%;
(6) step (4) gained is contained lithium solid mixing ore deposit and add an amount of fresh water, adding the fresh water amount is 10% of solid mineral total amount, fully stirs, and washs; Wash the Li that consists of of back solid mineral
+0.034%, Mg
2+11.25%, Cl
-34.69%; Get wash water 10kg;
(7) solid-liquid separation gets wash water and solid salt, and solid salt abandons or be used as production magnesium salts raw material;
(8) wash water returns step (2), and teds the solid-liquid product and mixes.
Embodiment 3
Step (1) (2) is with embodiment 1 step (1), (2);
(3) step (2) gained mixing solutions is heated to 114 ℃, evaporation 20kg moisture content;
(4) mixture behind step (3) evaporation at constant temperature is cooled to normal temperature, sufficient crystallising is separated out solid mixing ore deposit, and solid-liquid separation obtains concentrated saturated low Mg/Li ratio mother liquor of 15kg and 75kg and contains lithium solid mixing ore deposit, and mother liquor magnesium, lithium content are respectively Li
+3.37%, Mg
2+3.61%, magnesium, the lithium content in solid mixing ore deposit are respectively Li
+0.70%, Mg
2+10.15%;
(5) the saturated low Mg/Li ratio mother liquor of step (4) gained is gone on foot sinker by heavy magnesium one of two steps and can make Quilonum Retard, heavy magnesium of two steps is respectively the ammoniacal liquor of the first step with 15kg1:1, and second step was used the NaOH of 8.75kg40%, used the Na of 14kg40% at last
2CO
3Sinker makes Quilonum Retard purity and can reach 95.7%;
(6) step (4) gained is contained lithium solid mixing ore deposit and add an amount of fresh water, adding the fresh water amount is 10% of solid mineral total amount, fully stirs, and washs; Wash the Li that consists of of back solid mineral
+0.047%, Mg
2+11.73%, Cl
-33.77%; Get wash water 10kg;
(7) separate wash water and solid salt, solid salt abandons or as producing the magnesium salts raw material;
(8) wash water returns step (2), and teds the solid-liquid product and mixes.
Claims (2)
1. a high Mg/Li ratio contains the production technique that the old halogen in lithium salts lake is carried lithium, it is characterized in that, may further comprise the steps: (1) contains high Mg/Li ratio that the old halogen in lithium salts lake teds, concentrates, crystallization, obtains to ted the solid-liquid product; (2) step (1) gained is tedded the solid-liquid product and mix with last batch solid mixing ore deposit washings, heat temperature raising is to 〉=80 ℃, all dissolves to solids; (3) step (2) gained mixed solution continues heat temperature raising to boiling, and temperature is 110 ℃～120 ℃, evaporation concentration, and evaporation diminishing amount is the 5wt%～20wt% of amount of the mixture; (4) enriched mixture that step (3) is obtained is cooled to normal temperature, and sufficient crystallising is separated out and contained lithium solid mixing ore deposit, and solid-liquid separation must concentrate saturated low Mg/Li ratio mother liquor and contain lithium solid mixing ore deposit; (5) the saturated low Mg/Li ratio mother liquor that step (4) is obtained carries out the demagging sinker, the system Quilonum Retard; (6) the lithium solid mixing ore deposit that contains that step (4) is obtained adds an amount of fresh water, adds 5wt%～20wt% that the fresh water amount is the solid mineral total amount, fully stirs, and washs; (7) solidliquid mixture behind step (6) agitator treating is carried out solid-liquid separation, get washing lotion and solid salt, solid salt abandons or is used as production magnesium salts raw material; (8) step (7) gained washing lotion is returned step (2), ted the solid-liquid product with step (1) gained and mix.
2. high Mg/Li ratio according to claim 1 contains the production technique that the old halogen in lithium salts lake is carried lithium, it is characterized in that, described high Mg/Li ratio contains the old halogen in lithium salts lake, is chloride type or the old halogen of sulfate type salt lake.
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| CN102154563A (en) * | 2010-12-09 | 2011-08-17 | 江南大学 | Flotation method for enriching lithium from brine of salt lake brine |
| CN102491378A (en) * | 2011-10-14 | 2012-06-13 | 陈兆华 | Producing method for preparing lithium carbonate by taking carbonate type brine and sulphate type brine as raw material and by repeatedly mixing brine |
| CN102633284A (en) * | 2012-05-08 | 2012-08-15 | 湘潭大学 | Method for separating magnesium and extracting lithium from salt lake brine with high magnesium-lithium ratio |
| CN102757072A (en) * | 2012-08-02 | 2012-10-31 | 化工部长沙设计研究院 | Process for preparing magnesium sulfate heptahydrate |
| CN103253689A (en) * | 2012-02-17 | 2013-08-21 | 西藏国能矿业发展有限公司 | Method for extracting lithium and magnesium from salt lake brine |
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| CN103517877A (en) * | 2010-11-17 | 2014-01-15 | 韩国地质资源研究院 | Method for preparing high-purity lithium carbonate from brine |
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| CN102491378A (en) * | 2011-10-14 | 2012-06-13 | 陈兆华 | Producing method for preparing lithium carbonate by taking carbonate type brine and sulphate type brine as raw material and by repeatedly mixing brine |
| CN103253689A (en) * | 2012-02-17 | 2013-08-21 | 西藏国能矿业发展有限公司 | Method for extracting lithium and magnesium from salt lake brine |
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| CN115011816A (en) * | 2022-06-02 | 2022-09-06 | 紫金矿业集团股份有限公司 | Method for recovering lithium from salt field calcium chloride crystal |
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| CN115739004A (en) * | 2022-11-25 | 2023-03-07 | 中国科学院青海盐湖研究所 | Lithium-aluminum adsorption material prepared from salt lake brine with high magnesium-lithium ratio and method thereof |
| CN115786734A (en) * | 2022-11-25 | 2023-03-14 | 厦门紫金矿冶技术有限公司 | Method for recovering lithium from brine concentrated crystal salt |
| CN115786734B (en) * | 2022-11-25 | 2023-12-08 | 厦门紫金矿冶技术有限公司 | Method for recovering lithium by concentrating crystalline salt of brine |
| CN115739004B (en) * | 2022-11-25 | 2024-04-16 | 中国科学院青海盐湖研究所 | Lithium-aluminum adsorption material prepared from salt lake brine with high magnesium-lithium ratio and method thereof |
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