CN1179885C - Lithium carbonate crystal separating process from carbonate-type bittern by means of solar battery - Google Patents
Lithium carbonate crystal separating process from carbonate-type bittern by means of solar battery Download PDFInfo
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- CN1179885C CN1179885C CNB021293554A CN02129355A CN1179885C CN 1179885 C CN1179885 C CN 1179885C CN B021293554 A CNB021293554 A CN B021293554A CN 02129355 A CN02129355 A CN 02129355A CN 1179885 C CN1179885 C CN 1179885C
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Abstract
The present invention belongs to a method for separating lithium by crystallization from carbonate type bittern. Lithium carbonate is separated out by crystallization from carbonate type bittern by taking a solar pond as a crystallization pond, and an operating medium of the solar pond is the raw bittern for producing lithium carbonate. The solar pond is directly encircled by clay, the daylight area is from 1000 to 10000m<2>, and the pond depth is from 3 to 4m; the pond bottom is in a sandwich structure of a plastic membrane and hydromagnesite, and a black geomembrane or high-density polyethylene, polyvinyl chloride, etc. are laid on the inner wall of a pond body to be used as a liner. The present invention utilizes the solar pond as the crystallization pond to precipitate a large quantity of lithium carbonate and integrates the heat accumulation process of the solar pond with the separating process of lithium carbonate; thus, mixed salts in which 80% of lithium carbonate is contained can be obtained. The present invention has the advantages of low cost, simple structure, full utilization of solar energy and high economic benefit.
Description
Affiliated technical field
The invention belongs to a kind of from carbonate type bittern crystallization analyse the method for lithium.
Background technology
Lithium is the lightest metallic element, has the physics and the chemical property of a series of uniquenesses, thereby lithium and its esters have purposes widely in modern industry and science and technology, and the consumption of world's lithium is the trend that continues to increase.In world's lithium total resources, bittern lithium ore deposit accounts for 75%, and hard rock lithium ore deposit accounts for 25%; China bittern lithium ore deposit accounts for 72%, and hard rock lithium ore deposit accounts for 28%.Because to carry lithium low more than 1 times than the hard rock cost in the salt lake, from the salt lake, produce lithium salts at present and surpassed and from hard rock lithium ore deposit, produce lithium salts, thereby the extraction lithium salts become the megatrend of world development lithium industry from salt lake brine.
Chinese patent 99105828.3 provides a kind of method of extracting lithium salts from carbonate type bittern, and this method utilizes plateau cold conditions of living in to impel Na
2SO
410H
2The a large amount of sedimentary resources characteristics of O, from the salt lake, extract the low sulfate radical bittern of high lithium and make raw material, adopt multistage freezing Exposure to Sunlight on-swimmer's pool-control pond-crystallizing pond-mother liquor pond, make halite, saltcake separate (evaporation precipitation) in a large number in the shallow pond of Exposure to Sunlight, make lithium in bittern, reach pre-concentration, focus on the control pond then, make the lithium content 1500-2800mg/l of bittern and temperature more than 5 ℃, control is fallen halogen to crystallizing pond, makes enrichment higher-grade in the crystallizing pond, high lithium mixed salt that thickness is big, and it contains Li
2CO
3Grade is more than 5%.On the basis of this method, the present invention continues to explore the technique means that the raising Quilonum Retard is separated out.
The solubleness of Quilonum Retard in water reduces along with the rising of temperature, and the 0.85g during during by 30 ℃ 1.25g to 80 ℃ has reduced by 32%.Therefore when lithium content in the bittern reach or near saturation point after, it is temperature that the control Quilonum Retard precipitates the index of separating out.If adopt the rich lithium bittern of artificial heating to analyse lithium, effect is fine, but artificial heating means are also infeasible under the situation of energy shortage.Utilize plastic greenhouse as the sinker crystallizing pond, bittern is heated up and do not have evaporation substantially, and prevent sleet bittern desalting in season and when blowing silt particle enter crystallizing pond, kept the cleaning of the mixed salt that produces, Quilonum Retard content reaches about 30% in the obtained mixed salt.But the unfavorable factor of moulding the canopy crystallizing pond is: volume is little, and it is few to handle the bittern amount, and receiving salt wastes time and energy; Being subjected to influences greatly sunshine, and heat storage capacity is poor, and the temperature difference is bigger sooner or later in the canopy, cause halite, scale etc. at low temperatures crystallization separate out, influenced the purity of lithium salts; In addition, because many at highlands strong wind heavy snow weather, wind and snow very easily damages moulds canopy, makes production cost raise.
Summary of the invention
The object of the present invention is to provide and a kind ofly having inconvenient traffic and lacking highlandss such as fossil energy, utilize natural condition (solar energy resources) high benefit, contamination-freely the method for lithium is analysed in crystallization from carbonate type bittern.
Technical solution of the present invention is:
With solar pond as crystallizing pond crystallization from carbonate type bittern separate out Quilonum Retard, the working medium of solar pond is promptly produced the raw brine of Quilonum Retard; Said solar pond directly surrounds with clay, daylighting area 1000-10000m
2, the dark 3-4m in pond is the sandwich structure of plastic film and hydromagnesite at the bottom of the pond, pond body inwall is covered with black geomembrane or high density polyethylene(HDPE), polyvinyl chloride as liner.
Solar pond is divided into 3 zones from top to bottom: surperficial troposphere is made up of fresh water, and its temperature and envrionment temperature are close, mainly plays the effect that forms and protect the salt gradient layer under it; Troposphere, bottom (energy storage district) is made up of saturated salts solution, main heat absorption and the heat accumulation function of rising.During non-uniform temperature, can reach uniform state, thereby its effect is thermal-arrest and accumulation of heat by convection current and thermal conduction; Non-troposphere, middle part, its salt concn increases with the degree of depth, makes this layer pseudo adiabatic device, stop heat passage, heat is scattered and disappeared in the pond face, thereby can make the temperature variation in energy storage floor district, bottom more much higher, thereby reach the effect of collecting and storing sun power than the temperature of last convective region.
Advantage of the present invention is:
Make full use of the advantage of the climate resources (sun power) of nature,, make to be easy to the dispersive Quilonum Retard in the bittern and to concentrate precipitation in a large number and extract, and reduce cost to greatest extent and reduce the consumption of mineral fuel with the crystallizing pond of solar pond as Quilonum Retard;
Solar pond is fully accumulated sun power, and it is big to handle the bittern amount, has a narrow range of temperature at the bottom of the steady running after-bay, helps the Quilonum Retard sufficient crystallising and separates out;
Solar pond can be striden the season store heat, the temperature about 20 ℃ still can be kept in the bottom, pond in the winter time, though temperature is than reducing more summer, but winter, the bittern lithium concentration was higher, therefore Quilonum Retard still can deposit in solar pond and separate out, reach annual purpose of producing thus, can only store up the old technology of halogen before having upgraded winter, improved production efficiency;
Present method directly can reduce the cost of solar pond with bittern as working medium greatly, utilizes highlands abundant sun power and salt resource, the solar pond technology is applied to the salt pan produces in the Quilonum Retard mixed salt and go, and the cost of producing the Quilonum Retard mixed salt is reduced greatly.
Description of drawings
Accompanying drawing is the structural representation of solar pond.
Wherein 1. clays, 2. geomembrane, 3. plastic film, 4. lagging material
Embodiment:
With solar pond as crystallizing pond crystallization from carbonate type bittern separate out Quilonum Retard, said solar pond directly surrounds with clay 1, daylighting area 1000-10000m
2, the dark 3-4m in pond, pond body inwall is covered with black geomembrane 2 as liner, is the sandwich structure of plastic film 3 and lagging material 4 at the bottom of the pond, and lagging material 4 is hydromagnesite or porous plastics.
Bittern with high lithium, high-carbon acid group in the salt lake is made raw material, obtains rich lithium bittern after it is concentrated, and rich lithium brine depth is 1.5～2.5m in the control solar pond.
Pour into clean fresh water 30-50cm on the bittern layer, rich lithium bittern and fresh water aquifer total depth are 1.8～3m in the solar pond at this moment.After absorbing solar heat-preservation in 20-40 days, temperature can reach 15～40 ℃ at the bottom of the winter-spring season pond, temperature can reach more than 40～60 ℃ at the bottom of the summer and autumn ponds, bittern is after the solar pond heating, lithium single yield reaches 20% and reaches high lithium mixed salt about 3mm with enrichment thickness in the upper storage reservoir, and crystallization mixed salt lithium carbonate containing grade is more than 80%;
According to the evaporation situation, periodically replenish fresh water during the sinker, keep the pool inner water invariant position, guaranteed that fresh water aquifer thickness is basicly stable, guarantee the accumulated temperature effect in the pond for solar pond;
The operating method of crystallizing pond has two kinds:
Intermittent type: when lithium concentration drops to the quasi-equilibrium concentration of this district's temperature in the energy storage district bittern, tail halogen is extracted out, poured into rich lithium bittern again, carry out the crystallization of second cycle and analyse lithium.
Continous way: after solar pond started, continuously poured into fresh rich lithium bittern with certain flow every day, and discharge tail halogen continuously with certain flow, to keep the pool inner water invariant position.
Embodiment 1
1936 meters of solar pond daylighting areas
2, the ratio of slope 1: 1, pond body inwall is covered with the black geomembrane as liner, makes thermofin with magnesite at the bottom of the pond.
Bittern with high lithium, high-carbon acid group in the salt lake is made raw material, obtains Li after it is concentrated
+Concentration is the rich lithium bittern of 2.64g/l, and the degree of depth of rich lithium bittern is about 2.5m in the control solar pond; Pouring on the bittern layer about clean fresh water 50cm, bittern and fresh water aquifer total depth are about 3m in the solar pond at this moment.The running time be on March 19th, 2002 to May 4, after absorbing solar heat-preservation in 40 days, solar pond energy storage district temperature reaches about 31.5 ℃, enrichment thickness reaches the high lithium mixed salt about 3mm in the pond, crystallization mixed salt lithium carbonate containing grade is 83.1%.According to the evaporation situation, periodically replenish fresh water during the sinker, keep the pool inner water invariant position, guarantee the accumulated temperature effect of solar pond for solar pond.To May 8, bittern in the solar pond is extracted out, lithium concentration is 2.04g/l in the bittern at this moment, acquisition Quilonum Retard grade is 83.1% 8.31 tons of mixed salts (dry weight).
Embodiment 2
1936 meters of solar pond daylighting areas
2, the ratio of slope 1: 1, pond body inwall is covered with the black geomembrane as liner, makes thermofin with magnesite at the bottom of the pond.
Bittern with high lithium, high-carbon acid group in the salt lake is made raw material, obtains Li after it is concentrated
+Concentration is the rich lithium bittern of 1.8g/l, and the degree of depth of rich lithium bittern is about 1.69m in the control solar pond; Pouring on the bittern layer about clean fresh water 40cm, bittern and fresh water aquifer total depth are about 2.09m in the solar pond at this moment.The running time be on May 17th, 2002 to June 9, after absorbing solar heat-preservation in 23 days, solar pond energy storage district temperature reaches about 40 ℃, enrichment thickness reaches the high lithium mixed salt about 3mm in the pond, crystallization mixed salt lithium carbonate containing grade is 81.6%.According to the evaporation situation, periodically replenish fresh water during the sinker, keep the pool inner water invariant position, guarantee the accumulated temperature effect of solar pond for solar pond.To June 9, bittern in the solar pond is extracted out, lithium concentration is 1.22g/l in the bittern at this moment, acquisition Quilonum Retard grade is 81.6% 7.6 tons of mixed salts (dry weight).
Embodiment 3
1936 meters of solar pond daylighting areas
2, the ratio of slope 1: 1, pond body inwall is covered with the black geomembrane as liner, uses the last plastic production thermofin of bubble at the bottom of the pond.
Bittern with high lithium, high-carbon acid group in the salt lake is made raw material, obtains Li after it is concentrated
+Concentration is the rich lithium bittern of 1.59g/l, and the degree of depth of rich lithium bittern is about 1.5m in the control solar pond; Pouring on the bittern layer about clean fresh water 30cm, bittern and fresh water aquifer total depth are about 1.8m in the solar pond at this moment.The running time be on June 4th, 2002 to June 30, after absorbing solar heat-preservation in 26 days, solar pond energy storage district temperature reaches about 47 ℃, enrichment thickness reaches the high lithium mixed salt about 3mm in the pond, crystallization mixed salt lithium carbonate containing grade is 82.8%.According to the evaporation situation, periodically replenish fresh water during the sinker, keep the pool inner water invariant position, guarantee the accumulated temperature effect of solar pond for solar pond.To June 30, bittern in the solar pond to be extracted out, this moment, the bittern lithium concentration was 1.07g/l, acquisition Quilonum Retard grade is 82.8% 4.43 tons of mixed salts (dry weight).
Claims (4)
1, a kind ofly utilize solar pond crystallization from carbonate type bittern to separate out the method for Quilonum Retard, it is characterized in that with solar pond as crystallizing pond crystallization from carbonate type bittern separate out Quilonum Retard, the working medium of solar pond is promptly produced the raw brine of Quilonum Retard; Said solar pond directly surrounds with clay, daylighting area 1000-10000m
2, the dark 3-4m in pond is the sandwich structure of plastic film and hydromagnesite at the bottom of the pond, pond body inwall is covered with black geomembrane or high density polyethylene(HDPE), polyvinyl chloride as liner.
2, according to claim 1 from carbonate type bittern crystallization separate out the method for Quilonum Retard, it is characterized in that rich lithium brine depth is 1.5～2.5m in the solar pond, on rich lithium bittern layer, pour into clean fresh water 30-50cm, rich lithium bittern and fresh water aquifer total depth are 1.8～3m in the solar pond, during the sinker according to the evaporation situation, periodically replenish fresh water, keep the pool inner water invariant position, guarantee that fresh water aquifer thickness is basicly stable for solar pond.
3, according to claim 1 and 2 from carbonate type bittern crystallization separate out the method for Quilonum Retard, the operating method that it is characterized in that crystallizing pond is an intermittent type: when lithium concentration drops to the quasi-equilibrium concentration of this district's temperature in the energy storage district bittern, tail halogen is extracted out, again pour into rich lithium bittern, carry out the crystallization of second cycle and analyse lithium.
4, according to claim 1 and 2 from carbonate type bittern crystallization separate out the method for Quilonum Retard, the operating method that it is characterized in that crystallizing pond is a continous way: after solar pond starts, pour into rich lithium bittern every day continuously, and discharge tail halogen continuously, to keep the pool inner water invariant position.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021293554A CN1179885C (en) | 2002-09-04 | 2002-09-04 | Lithium carbonate crystal separating process from carbonate-type bittern by means of solar battery |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021293554A CN1179885C (en) | 2002-09-04 | 2002-09-04 | Lithium carbonate crystal separating process from carbonate-type bittern by means of solar battery |
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| CN1179885C true CN1179885C (en) | 2004-12-15 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928023B (en) * | 2010-09-03 | 2012-05-09 | 山西大学 | Device and method for preparing lithium carbonate from brine by utilizing solar energy |
| CN102267708B (en) * | 2011-07-01 | 2013-05-22 | 清华大学 | Method for preparing lithium carbonate nano-particle by crystallization method |
| CN102295303B (en) * | 2011-08-08 | 2013-09-04 | 江西本源新材料科技有限公司 | Extraction method of lithium carbonate |
| CN102583454A (en) * | 2012-02-13 | 2012-07-18 | 中国地质科学院盐湖与热水资源研究发展中心 | Method for extracting lithium carbonate from carbonate brine |
| CN103420400B (en) * | 2012-05-14 | 2015-06-10 | 中国地质科学院盐湖与热水资源研究发展中心 | Salt lake brine evaporation method and equipment thereof, and salt lake brine treatment method by utilizing salt lake brine evaporation method and device thereof |
| CN109824067B (en) * | 2018-12-22 | 2022-10-21 | 魏万仁 | Extracting lithium concentrate by natural evaporation crystallization lithium precipitation, combined heating crystallization lithium precipitation and dissolution lithium washing |
| CN113336249B (en) * | 2021-05-28 | 2022-02-25 | 中国地质科学院矿产资源研究所 | Lithium extraction solar cell and lithium extraction method |
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- 2002-09-04 CN CNB021293554A patent/CN1179885C/en not_active Expired - Lifetime
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