CN102921553A - 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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- CN102921553A CN102921553A CN2012104796529A CN201210479652A CN102921553A CN 102921553 A CN102921553 A CN 102921553A CN 2012104796529 A CN2012104796529 A CN 2012104796529A CN 201210479652 A CN201210479652 A CN 201210479652A CN 102921553 A CN102921553 A CN 102921553A
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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 the method that lithium potassium sulfate is extracted in a kind of salt mixture flotation that contains various grade lithium potassium sulfates that obtains 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 manufacturing, 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 the granite peamatite mineral deposit, the lithium resource that wherein contains in the salt lake bittern account for world's lithium reserves 69% and lithium reserves basis, the world 87%.
Contain the lithium salts lake and form according to the solid lithium salts that salt lake bittern teds acquisition, 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 large quantity research both at home and abroad.At present, the technology of extracting the 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 existing salt lake bittern is put forward lithium technique and nearly all is based on chloride type, carbonate type salt lake bittern.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, mainly is to process lithium potassium sulfate by the chemical industry facture, and then produces lithium carbonate and potassium product.Yet, in the 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 the domestic and international prior art, chemical method can only be processed the Brine resources of high-quality, and 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 that is 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, may further comprise the steps:
(1) lithium potassium sulfate and NaCl mixed salt are carried out ore grinding, the ore grinding mass concentration is 50%～60%, and milling medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, gets 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, directly add the amine floating agent when roughly selecting and scanning, (stirring is in order to make the medicament Uniform Dispersion to carry out flotation after stirring, 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 0.5 ~ 1 times for the pharmaceutical quantities of scanning for the first time the second time; Dosing method is: medicament is mixed with the aqueous solution, and heating after medicament all is dissolved in the water, is added in the 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; Get the lithium potassium sulfate concentrate;
T represents the mass unit ton;
(3) step (2) gained lithium potassium sulfate concentrate is filtered, oven dry, 90 ℃～100 ℃ of bake out temperatures, drying time 1h～2h gets the thick product of lithium potassium sulfate.
In the step (1), the preferred ball milling of grinding mode or rod milling, preferred-200 order mass ratioes of mog are 65%～90%;
In the step (2), described amine floating agent is the amine cation medicament, is at least a of 12～18 alkyl fatty amine for alkyl carbon chain contains carbon number.
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, and cost is low, energy consumption is low, used floating agent nontoxic pollution-free, gained lithium potassium sulfate good product quality; The lithium resource rate of recovery is high, and is good in economic efficiency.
The present invention adopts floatation first the impurity such as lithium potassium sulfate and sodium chloride to be separated, and produces potassium sulfate and lithium carbonate by the chemical industry facture again, 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 the 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 present embodiment may further comprise the steps:
(1) with lithium potassium sulfate and NaCl mixed salt through the ball milling ore grinding, milling medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, the ore grinding mass concentration is 55%, ore grinding to-200 order mass ratioes are 80%, get 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, add the cation-collecting agent octadecylamine when roughly selecting and scanning, stir and carry out flotation after 3 minutes, floating agent dosage is: the stage dosing of roughly selecting is the 250g/t raw ore, the stage dosing of scanning is the 150g/t raw ore, scraping the bubble time in the rougher process is 4 minutes, scanning and scraping the bubble time in the process is 3 minutes, and dosing method is: medicament is mixed with the aqueous solution, is heated to 80 ℃, after medicament all is dissolved in the water, be added in the ore pulp; Flotation temperature is normal temperature; Get the lithium potassium sulfate concentrate;
(3) step (2) gained lithium potassium sulfate concentrate is filtered, then 90 ℃ of lower bakings 1.5 hours, get the thick product of lithium potassium sulfate.
The lithium potassium sulfate concentrate of present embodiment gained contains 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 the 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 present embodiment may further comprise the steps:
(1) with lithium potassium sulfate and NaCl mixed salt through the ball milling ore grinding, milling medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, the ore grinding mass concentration is 55%, ore grinding to-200 order mass ratioes are 80%, get 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, add the cation-collecting agent octadecylamine when roughly selecting and scanning, stir and carry out flotation after 3 minutes, floating agent dosage is: the stage dosing of roughly selecting is the 300g/t raw ore, and it is the 150g/t raw ore that the stage of scanning is added pharmaceutical quantities for the first time, and scanning the interpolation pharmaceutical quantities for the second time is the 75g/t raw ore; Dosing method is: medicament is mixed with the aqueous solution, is heated to 80 ℃, after medicament all is dissolved in the water, be added in the ore pulp; Flotation temperature is normal temperature; Scraping the bubble time in the rougher process is 4 minutes, scans for twice to scrape the bubble time in the process and be 3 minutes; Get the lithium potassium sulfate concentrate;
(3) step (2) gained lithium potassium sulfate concentrate is filtered, then 90 ℃ of lower bakings 1.5 hours, get the thick product of lithium potassium sulfate.
The thick product of present embodiment gained lithium potassium sulfate contains 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 the 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 present embodiment may further comprise the steps:
(1) with lithium potassium sulfate and NaCl mixed salt through the ball milling ore grinding, milling medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, the ore grinding mass concentration is 55 %, ore grinding to-200 order mass ratioes are 80%, get 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, directly add the cation-collecting agent 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 the 250g/t raw ore, and the stage dosing of scanning is the 150g/t raw ore; Dosing method is: medicament is mixed with the aqueous solution, is heated to 80 ℃, after medicament all is dissolved in the water, be added in the ore pulp; Flotation temperature is normal temperature; Scraping the bubble time in the rougher process is 5 minutes, and scanning and scraping the bubble time in the process is 4 minutes; Get the lithium potassium sulfate concentrate;
(3) step (2) gained lithium potassium sulfate concentrate is filtered, then 90 ℃ of lower bakings 1.5 hours, get the thick product of lithium potassium sulfate.
The thick product of present embodiment gained lithium potassium sulfate contains 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 the 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 present embodiment may further comprise the steps:
(1) with lithium potassium sulfate and NaCl mixed salt through the ball milling ore grinding, milling medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, the ore grinding mass concentration is 55%, ore grinding to-200 order mass ratioes are 80%, get 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, directly add the cation-collecting agent 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 the 300g/t raw ore, and it is the 150g/t raw ore that the stage of scanning is added pharmaceutical quantities for the first time, and scanning the interpolation pharmaceutical quantities for the second time is the 125g/t raw ore; Dosing method is: medicament is mixed with the aqueous solution, is heated to 80 ℃, after medicament all is dissolved in the water, be added in the ore pulp; Flotation temperature is normal temperature; Scraping the bubble time in the rougher process is 4 minutes, and scanning for twice and scraping the bubble time in the process is 3 minutes; Get the lithium potassium sulfate concentrate;
(3) step (2) gained lithium potassium sulfate concentrate is filtered, then 90 ℃ of lower bakings 1.5 hours, get the thick product of lithium potassium sulfate.
The thick product of present embodiment gained lithium potassium sulfate contains 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 the 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 present embodiment may further comprise the steps:
(1) with lithium potassium sulfate and NaCl mixed salt through the ball milling ore grinding, milling medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, the ore grinding mass concentration is 55%, ore grinding to-200 order mass ratioes are 80%, get 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 the 200g/t raw ore, the stage dosing of scanning is the 150g/t raw ore, scraping the bubble time in the rougher process is 6 minutes, scanning and scraping the bubble time in the process is 5 minutes, dosing method is: medicament is mixed with the aqueous solution, be heated to 80 ℃, after medicament all is dissolved in the water, be added in the ore pulp; Flotation temperature is normal temperature; Get the lithium potassium sulfate concentrate;
(3) step (2) gained lithium potassium sulfate concentrate is filtered, then 90 ℃ of lower bakings 1.5 hours, get the thick product of lithium potassium sulfate.
The lithium potassium sulfate concentrate of present embodiment gained contains Li
+3.45%, Li
+The rate of recovery 73.93%.
Claims (5)
1. the method for a flotation lithium potassium sulfate from lithium potassium sulfate and sodium chloride mixture is characterized in that, may further comprise the steps:
(1) lithium potassium sulfate and NaCl mixed salt are carried out ore grinding, the ore grinding mass concentration is 50%～60%, and milling medium is the common saturated mother liquor of lithium potassium sulfate and NaCl mixed salt, gets 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, directly add the amine floating agent when roughly selecting and scanning, carry out flotation after stirring, 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 0.5 ~ 1 times for the pharmaceutical quantities of scanning for the first time the second time; Dosing method is: medicament is mixed with the aqueous solution, and heating after medicament all is dissolved in the water, is added in the 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; Get the lithium potassium sulfate concentrate;
T represents the mass unit ton;
(3) step (2) gained lithium potassium sulfate concentrate is filtered, oven dry, 90 ℃～100 ℃ of bake out temperatures, drying time 1h～2h gets 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 the 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 the step (1), mog is 65%～90% for-200 order mass ratioes.
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 the step (2), described amine floating agent is the 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 a of 12～18 alkyl fatty amine to alkyl carbon chain.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112479232A (en) * | 2020-12-16 | 2021-03-12 | 深圳清华大学研究院 | Floatation separation method for industrial by-product sodium chloride and sodium sulfate |
| 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 |
| CN114762842A (en) * | 2021-01-13 | 2022-07-19 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| 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 |
| CN114762842A (en) * | 2021-01-13 | 2022-07-19 | 中蓝长化工程科技有限公司 | Method for extracting lithium carbonate from mixed salt of carbonate and chloride |
| 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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