CN102921553B - Method for flotation of lithium potassium sulfate in mixture of lithium potassium sulfate and sodium chloride - Google Patents
Method for flotation of lithium potassium sulfate in mixture of lithium potassium sulfate and sodium chloride Download PDFInfo
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- CN102921553B CN102921553B CN201210479652.9A CN201210479652A CN102921553B CN 102921553 B CN102921553 B CN 102921553B CN 201210479652 A CN201210479652 A CN 201210479652A CN 102921553 B CN102921553 B CN 102921553B
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- potassium sulfate
- lithium potassium
- flotation
- lithium
- sodium chloride
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Abstract
A method for flotation of lithium potassium sulfate in a mixture of lithium potassium sulfate and sodium chloride comprises the following steps: (1) performing ore grinding of a mixed salt of potassium sulfate and sodium chloride (NaCl); (2) feeding ore slurry obtained in the step (1) into a flotation machine, wherein the flotation process flow comprises once roughing and once scavenging or once roughing and twice scavenging; and (3) filtering and drying lithium potassium sulfate ore concentrate obtained in the step (2) to obtain coarse lithium potassium sulfate product. The method for flotation of lithium potassium sulfate in the mixture of lithium potassium sulfate and sodium chloride has very high adaptability to lithium potassium sulfate resources of different grades, is simple in process, convenient to operate and low in cost and energy consumption and adopts nontoxic and pollution-free flotation reagents; the obtained lithium potassium sulfate product is good in quality; the lithium resource recovery ratio is high; and good economic benefits are achieved. According to the invention, lithium potassium sulfate is separated from sodium chloride and other impurities through a floatation method, and then potassium sulfate and lithium carbonate are produced through a chemical treatment method, so that the product quality and the yield are greatly improved.
Description
Technical field
The present invention relates to a kind of from lithium potassium sulfate and sodium chloride mixed salt the method for flotation lithium potassium sulfate, particularly relate to a kind of method that lithium potassium sulfate is extracted in salt mixture flotation containing various grade lithium potassium sulfates obtaining after utilizing salt lake bittern to ted.
Background technology
Lithium metal and lithium salts are the important strategic resources of country, are widely used in the various fields such as Aero-Space, equipment manufacture, electronics, metal material, nuclear energy and national defense industry, and the annual whole world to the demand of lithium still in continuous growth.
Lithium resource is mainly composed and is existed in salt lake and granite peamatite mineral deposit, the lithium resource wherein containing in salt lake bittern account for world's lithium reserves lithium reserves basis, the 69%He world 87%.
The solid lithium salts that teds acquisition according to salt lake bittern containing lithium salts lake forms, and mainly can be divided into three major types, i.e. chloride type, carbonate-type, sulfate type.
For exploitation bittern lithium resource, the extracting method of various bittern lithium salts has been carried out to large quantity research both at home and abroad.At present, the technology of extracting bittern lithium resource both at home and abroad mainly contains ion exchange adsorption, the precipitation method, evaporative crystallization method, extraction, solar pond method, calcining leaching method, Xu Shi method and electroosmose process etc.
But it is nearly all based on chloride type, carbonate type salt lake bittern that existing salt lake bittern is put forward lithium technique.The solid lithium salts that is tedded acquisition by sulfate type salt lake bittern often contains the impurity such as a large amount of NaCl, at present, is mainly to process lithium potassium sulfate by chemical industry facture, and then produces lithium carbonate and potassium product.Yet, in chemical industry processing procedure, owing to there is a large amount of sodium chloride as impurity, have a strong impact on quality and the yield of product; And in domestic and international prior art, chemical method can only be processed the Brine resources of high-quality, the Brine resources lower to grade is helpless.
Summary of the invention
The technical problem to be solved in the present invention is; overcome the deficiencies in the prior art; provide a kind of technique simple; energy consumption is low; pollution-free, good product quality, the method for flotation lithium potassium sulfate from lithium potassium sulfate and sodium chloride mixed salt being produced on a large scale; to improve the utilization rate of lithium resource, reduce the production cost of sulfate type salt lake lithium potassium sulfate.
The present invention solves the technical scheme that its technical problem adopts, a kind of from lithium potassium sulfate and sodium chloride mixed salt the method for flotation lithium potassium sulfate, comprise the following steps:
(1) lithium potassium sulfate and NaCl mixed salt are carried out to ore grinding, ore grinding mass concentration is 50%～60%, and milling medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, obtains ore pulp;
(2) step (1) gained ore pulp is sent into flotation device, flotation process is that one roughing once purging selection (i.e. " slightly sweeps ") or one roughing are scanned (i.e. " one thick two sweeps ") for twice, flotation medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, when roughly selecting and scanning, directly add amine floating agent, (stirring is in order to make medicament dispersed after stirring, to carry out flotation, fully contact with mineral grain), floating agent dosage is: it is 200g/t raw ore～300g/t raw ore that the stage of roughly selecting is added dosing, it is 100g/t raw ore～150g/t raw ore that the stage of scanning is added pharmaceutical quantities for the first time, if twice is scanned, scan for the second time pharmaceutical quantities for scanning for the first time 0.5 ~ 1 times, dosing method is: medicament is mixed with to the aqueous solution, and heating, after medicament is all dissolved in water, is added in ore pulp, flotation temperature is normal temperature, the time of roughly selecting is 4 ~ 6min, and the time of scanning is 3 ~ 5min at every turn, obtain lithium potassium sulfate concentrate,
T represents mass unit ton;
(3) step (2) gained lithium potassium sulfate concentrate is filtered, dry, 90 ℃～100 ℃ of bake out temperatures, drying time 1h～2h, obtains the thick product of lithium potassium sulfate.
In step (1), the preferred ball milling of grinding mode or rod milling, mog preferably-200 order mass ratioes is 65%～90%;
In step (2), described amine floating agent is amine cation medicament, is at least one containing the carbon number alkyl fatty amine that is 12～18 of alkyl carbon chain.
Adopt the present invention, flotation lithium potassium sulfate from lithium potassium sulfate and sodium chloride salt, has very strong adaptability to the lithium potassium sulfate resource of different grades, and technique is simple, convenient operation, cost is low, energy consumption is low, floating agent nontoxic pollution-free used, gained lithium potassium sulfate good product quality; The lithium resource rate of recovery is high, good in economic efficiency.
The present invention adopts floatation first that the impurity such as lithium potassium sulfate and sodium chloride is separated, then produces potassium sulfate and lithium carbonate by chemical industry facture, will greatly improve quality and the yield of product.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
Lithium potassium sulfate and NaCl mixed salt (low-grade lithium potassium sulfate solid mineral) ted out in salt lake in China, and it consists of Li
+0.42%, K
+2.38%, Na
+35.94%, Cl
-55.40%, SO
4 2-5.85%.
The method of flotation lithium potassium sulfate from lithium potassium sulfate and sodium chloride mixture of the present embodiment, comprises the following steps:
(1) by lithium potassium sulfate and NaCl mixed salt through ball milling ore grinding, milling medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, ore grinding mass concentration is 55%, ore grinding to-200 order mass ratioes are 80%, obtain ore pulp;
(2) step (1) gained ore pulp is sent into flotation device, adopt " one slightly sweeps " technological process, flotation medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, when roughly selecting and scanning, add cation-collecting agent octadecylamine, stir and carry out flotation after 3 minutes, floating agent dosage is: the stage dosing of roughly selecting is 250g/t raw ore, the stage dosing of scanning is 150g/t raw ore, in rougher process, scraping the bubble time is 4 minutes, scanning and scraping the bubble time in process is 3 minutes, dosing method is: medicament is mixed with to the aqueous solution, be heated to 80 ℃, after medicament is all dissolved in water, be added in ore pulp, flotation temperature is normal temperature, obtain lithium potassium sulfate concentrate,
(3) step (2) gained lithium potassium sulfate concentrate is filtered, then at 90 ℃, dry 1.5 hours, obtain the thick product of lithium potassium sulfate.
The lithium potassium sulfate concentrate of the present embodiment gained is containing Li
+3.08%, Li
+the rate of recovery 72%.
Embodiment 2
Lithium potassium sulfate and NaCl mixed salt (high-grade lithium potassium sulfate solid mineral) ted out in salt lake in China, and it consists of Li
+2.71%, K
+15.38%, Na
+17.46%, Cl
-26.89%, SO
4 2-37.56%.
The method of flotation lithium potassium sulfate from lithium potassium sulfate and sodium chloride mixture of the present embodiment, comprises the following steps:
(1) by lithium potassium sulfate and NaCl mixed salt through ball milling ore grinding, milling medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, ore grinding mass concentration is 55%, ore grinding to-200 order mass ratioes are 80%, obtain ore pulp;
(2) step (1) gained ore pulp is sent into flotation device, adopt " one thick two sweeps " technological process, flotation medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, when roughly selecting and scanning, add cation-collecting agent octadecylamine, stir and carry out flotation after 3 minutes, floating agent dosage is: the stage dosing of roughly selecting is 300g/t raw ore, and it is 150g/t raw ore that the stage of scanning is added pharmaceutical quantities for the first time, and scanning for the second time interpolation pharmaceutical quantities is 75g/t raw ore; Dosing method is: medicament is mixed with to the aqueous solution, is heated to 80 ℃, after medicament is all dissolved in water, be added in ore pulp; Flotation temperature is normal temperature; In rougher process, scraping the bubble time is 4 minutes, scans for twice in process, to scrape the bubble time and be 3 minutes; Obtain lithium potassium sulfate concentrate;
(3) step (2) gained lithium potassium sulfate concentrate is filtered, then at 90 ℃, dry 1.5 hours, obtain the thick product of lithium potassium sulfate.
The thick product of the present embodiment gained lithium potassium sulfate is containing Li
+4.21%, the rate of recovery 87.04%.
Embodiment 3
Lithium potassium sulfate and NaCl mixed salt (low-grade lithium potassium sulfate solid mineral) ted out in salt lake in China, and it consists of Li
+0.42%, K
+2.38%, Na
+35.94%, Cl
-55.40%, SO
4 2-5.85%.
The method of flotation lithium potassium sulfate from lithium potassium sulfate and sodium chloride mixture of the present embodiment, comprises the following steps:
(1) by lithium potassium sulfate and NaCl mixed salt through ball milling ore grinding, milling medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, ore grinding mass concentration is 55 %, ore grinding to-200 order mass ratioes are 80%, obtain ore pulp;
(2) step (1) gained ore pulp is sent into flotation device, adopt " one slightly sweeps " technological process, flotation medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, when roughly selecting and scanning, directly add cation-collecting agent lauryl amine, stir and carry out flotation after 3 minutes, floating agent dosage is: the stage dosing of roughly selecting is 250g/t raw ore, and the stage dosing of scanning is 150g/t raw ore; Dosing method is: medicament is mixed with to the aqueous solution, is heated to 80 ℃, after medicament is all dissolved in water, be added in ore pulp; Flotation temperature is normal temperature; In rougher process, scraping the bubble time is 5 minutes, and scanning and scraping the bubble time in process is 4 minutes; Obtain lithium potassium sulfate concentrate;
(3) step (2) gained lithium potassium sulfate concentrate is filtered, then at 90 ℃, dry 1.5 hours, obtain the thick product of lithium potassium sulfate.
The thick product of the present embodiment gained lithium potassium sulfate is containing Li
+2.98%, Li
+the rate of recovery 71.95%.
Embodiment 4
Lithium potassium sulfate and NaCl mixed salt (high-grade lithium potassium sulfate solid mineral) ted out in salt lake in China, and it consists of Li
+2.66%, K
+15.38%, Na
+17.46%, Cl
-26.89%, SO
4 2-37.56%.
The method of flotation lithium potassium sulfate from lithium potassium sulfate and sodium chloride mixture of the present embodiment, comprises the following steps:
(1) by lithium potassium sulfate and NaCl mixed salt through ball milling ore grinding, milling medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, ore grinding mass concentration is 55%, ore grinding to-200 order mass ratioes are 80%, obtain ore pulp;
(2) step (1) gained ore pulp is sent into flotation device, adopt " one thick two sweeps " technological process, flotation medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, when roughly selecting and scanning, directly add cation-collecting agent lauryl amine, stir and carry out flotation after 3 minutes, floating agent dosage is: the stage dosing of roughly selecting is 300g/t raw ore, and it is 150g/t raw ore that the stage of scanning is added pharmaceutical quantities for the first time, and scanning for the second time interpolation pharmaceutical quantities is 125g/t raw ore; Dosing method is: medicament is mixed with to the aqueous solution, is heated to 80 ℃, after medicament is all dissolved in water, be added in ore pulp; Flotation temperature is normal temperature; In rougher process, scraping the bubble time is 4 minutes, and scanning for twice and scraping the bubble time in process is 3 minutes; Obtain lithium potassium sulfate concentrate;
(3) step (2) gained lithium potassium sulfate concentrate is filtered, then at 90 ℃, dry 1.5 hours, obtain the thick product of lithium potassium sulfate.
The thick product of the present embodiment gained lithium potassium sulfate is containing Li
+4.01%, the rate of recovery 70.04%.
Embodiment 5
Lithium potassium sulfate and NaCl mixed salt (low-grade lithium potassium sulfate solid mineral) ted out in salt lake in China, and it consists of Li
+0.42%, K
+2.38%, Na
+35.94%, Cl
-55.40%, SO
4 2-5.85%.
The method of flotation lithium potassium sulfate from lithium potassium sulfate and sodium chloride mixture of the present embodiment, comprises the following steps:
(1) by lithium potassium sulfate and NaCl mixed salt through ball milling ore grinding, milling medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, ore grinding mass concentration is 55%, ore grinding to-200 order mass ratioes are 80%, obtain ore pulp;
(2) step (1) gained ore pulp is sent into flotation device, adopt " one slightly sweeps " technological process, flotation medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, the mixture (mass ratio of octadecylamine and lauryl amine is 10:3) that adds cation-collecting agent octadecylamine and lauryl amine when roughly selecting and scanning, stir and carry out flotation after 3 minutes, floating agent dosage is: the stage dosing of roughly selecting is 200g/t raw ore, the stage dosing of scanning is 150g/t raw ore, in rougher process, scraping the bubble time is 6 minutes, scanning and scraping the bubble time in process is 5 minutes, dosing method is: medicament is mixed with to the aqueous solution, be heated to 80 ℃, after medicament is all dissolved in water, be added in ore pulp, flotation temperature is normal temperature, obtain lithium potassium sulfate concentrate,
(3) step (2) gained lithium potassium sulfate concentrate is filtered, then at 90 ℃, dry 1.5 hours, obtain the thick product of lithium potassium sulfate.
The lithium potassium sulfate concentrate of the present embodiment gained is containing Li
+3.45%, Li
+the rate of recovery 73.93%.
Claims (5)
1. a method for flotation lithium potassium sulfate from lithium potassium sulfate and sodium chloride mixture, is characterized in that, comprises the following steps:
(1) lithium potassium sulfate and NaCl mixed salt are carried out to ore grinding, ore grinding mass concentration is 50%～60%, and milling medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, obtains ore pulp;
(2) step (1) gained ore pulp is sent into flotation device, flotation process is that one roughing once purging selection or one roughing are scanned for twice, flotation medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, when roughly selecting and scanning, directly add amine floating agent, after stirring, carry out flotation, floating agent dosage is: it is 200g/t raw ore～300g/t raw ore that the stage of roughly selecting is added dosing, it is 100g/t raw ore～150g/t raw ore that the stage of scanning is added pharmaceutical quantities for the first time, if twice is scanned, scan for the second time pharmaceutical quantities for scanning for the first time 0.5 ~ 1 times, dosing method is: medicament is mixed with to the aqueous solution, and heating, after medicament is all dissolved in water, is added in ore pulp, flotation temperature is normal temperature, the time of roughly selecting is 4 ~ 6min, and the time of scanning is 3 ~ 5min at every turn, obtain lithium potassium sulfate concentrate,
T represents mass unit ton;
(3) step (2) gained lithium potassium sulfate concentrate is filtered, dry, 90 ℃～100 ℃ of bake out temperatures, drying time 1h～2h, obtains the thick product of lithium potassium sulfate.
According to claim 1 from lithium potassium sulfate and sodium chloride mixture the method for flotation lithium potassium sulfate, it is characterized in that, in step (1), grinding mode is ball milling or rod milling.
According to claim 1 and 2 from lithium potassium sulfate and sodium chloride mixture the method for flotation lithium potassium sulfate, it is characterized in that, in step (1), mog for-200 order mass ratioes be 65%～90%.
According to claim 1 and 2 from lithium potassium sulfate and sodium chloride mixture the method for flotation lithium potassium sulfate, it is characterized in that, in step (2), described amine floating agent is amine cation medicament.
According to claim 4 from lithium potassium sulfate and sodium chloride mixture the method for flotation lithium potassium sulfate, it is characterized in that, described amine cation medicament is that to contain carbon number be at least one of 12～18 alkyl fatty amine to alkyl carbon chain.
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| CN104998748A (en) * | 2015-06-19 | 2015-10-28 | 化工部长沙设计研究院 | Technology for extracting potassium and removing sodium from high-sodium polyhalite ore |
| CN105350081A (en) * | 2015-11-14 | 2016-02-24 | 中国科学院新疆理化技术研究所 | Preparation method and use of potassium lithium sulfate nonlinear optical crystal |
| CN112916211A (en) * | 2019-12-05 | 2021-06-08 | 宁波行殊新能源科技有限公司 | Mineral agent for flotation of lithium potassium sulfate |
| CN112479232B (en) * | 2020-12-16 | 2023-04-11 | 深圳清华大学研究院 | Floatation separation method for industrial by-product sodium chloride and sodium sulfate |
| CN114762842B (en) * | 2021-01-13 | 2023-09-19 | 中蓝长化工程科技有限公司 | Method for extracting lithium carbonate from mixed salt of carbonate and chloride |
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| CN101481265A (en) * | 2009-02-25 | 2009-07-15 | 化工部长沙设计研究院 | Production process for extracting potash fertilizer form low grade potassium mixed salt |
| CN102120592A (en) * | 2011-04-25 | 2011-07-13 | 化工部长沙设计研究院 | Method for extracting lithium carbonate by flotation of mixed salt of NaCl and lithium carbonate |
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| RU2112601C1 (en) * | 1996-01-16 | 1998-06-10 | Петухов Василий Николаевич | Foarming reagent for coal flotation process |
| CN1321893C (en) * | 2002-09-25 | 2007-06-20 | 国投新疆罗布泊钾盐有限责任公司 | Method for preparing potassium sulfate from bittern containing potassium and magnesium sulfate |
| CN101318670A (en) * | 2008-07-16 | 2008-12-10 | 化工部长沙设计研究院 | Processing technique for extracting lithium salt from lithium containing salt lake bittern water |
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| CN101481265A (en) * | 2009-02-25 | 2009-07-15 | 化工部长沙设计研究院 | Production process for extracting potash fertilizer form low grade potassium mixed salt |
| CN102120592A (en) * | 2011-04-25 | 2011-07-13 | 化工部长沙设计研究院 | Method for extracting lithium carbonate by flotation of mixed salt of NaCl and lithium carbonate |
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