CN100427394C - Method for preparing lithium chloride free from water - Google Patents
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- CN100427394C CN100427394C CNB2006100859824A CN200610085982A CN100427394C CN 100427394 C CN100427394 C CN 100427394C CN B2006100859824 A CNB2006100859824 A CN B2006100859824A CN 200610085982 A CN200610085982 A CN 200610085982A CN 100427394 C CN100427394 C CN 100427394C
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Abstract
The present invention discloses a method for preparing anhydrous lithium chloride, which comprises: calcium chloride is added to a lithium sulfate solution, and lithium chloride and calcium sulphate are obtained; the products are filtered and washed, CaSO4 is removed, and an LiCl solution (mother liquor 1) is obtained; after the mother liquor 1 is decompressed and concentrated, a barium chloride solution is added to the mother liquor 1; SO4<2-> is removed by filtering and washing after reaction; a lithium carbonate solution is added to the obtained mother liquor 1, impurities such as Ba2+ and Ca2+ are removed by filtering and washing after reaction, and an LiCl solution (mother liquor 2) is obtained; the mother liquor 2 is decompressed, concentrated, crystallized by cooling, separated and dried, and anhydrous lithium chloride is obtained. The present invention adopts a technological method for preparing and producing anhydrous lithium chloride directly by lithium raw materials of leaching liquor from lithium ores and a lithium sulfate solution, and therefore, technological lines are substantially shortened, operation steps are greatly simplified, operation is easy, energy consumption and water consumption are reduced, the loss of lithium in the process is reduced, and the yield of lithium is increased. The present invention fundamentally overcomes various defects existing in the traditional technological methods, and realizes the innovation of lithium chloride preparation technology.
Description
Technical field:
The present invention relates to a kind of preparation method of Lithium chloride (anhydrous).
Background technology:
Lithium chloride is a kind of important lithium salts product, except being used for air conditioner dehumidification agent, chlorinated lime, sterilant, synthon, pharmaceutical industry, lithium cell, metal alloy welding compound or fusing assistant, also has a very important purposes to be used to produce metallic lithium exactly.At present, metallic lithium not only becomes one of strategic materials the most significant on the national defence, also becomes the closely bound up important meals element of a kind of and human daily life simultaneously.Metallic lithium and alloy thereof and compound have purposes widely in many fields such as nuclear industry, metallurgical industry, battery, glass, pottery, chemical industry, space industry manufacturings.Lithium chloride also begins to be used widely in fields such as biology, medical science in recent years, medically is being used for the treatment of diabetes, genetic research etc.; As mutagenic compound, be applied to industry seed selection good quality strains such as food (beer), medicine, environmental protection, cultivate superior strain, synthetic medicine intermediate carries out genetic modification to bacterial classification; Aspect organic structural analysis, lithium chloride is a kind of important cationic additive; In field of new, be widely used in the production of chitin (matter).The demand of lithium chloride and derived product thereof the industries such as nonlinear optical material in controlled nuclear fusion reaction, Al-Li alloy, lithium ion battery, optical communication increases substantially.Lithium chloride of many uses, the electrolysis production metallic lithium is the field of lithium chloride consumption maximum.
Existing is that feedstock production or production lithium chloride method mainly are with the lithium ore deposit:
Quilonum Retard or lithium hydroxide conversion method are preparations and produce the topmost method of lithium chloride.This method generates lithium chloride with finished product Quilonum Retard or lithium hydroxide and hydrochloric acid reaction, through a series of separation, washing, concentrate, obtain lithium chloride after the crystallization, drying step.And the production of finished product Quilonum Retard or lithium hydroxide be with by the lithium ore deposit through roasting, acidifying, slurrying, leaching with tentatively concentrate that the lithium ore leaching liquid-lithium sulfate solution that obtains generates Quilonum Retard with the yellow soda ash reaction or generate lithium hydroxide with calcium hydroxide reaction, through a series of separation, washing, removal of impurities, concentrate, step is made Quilonum Retard or lithium hydroxide product after the crystallization, drying.
Though existing is feedstock production or the processing method comparative maturity of producing lithium chloride with the lithium ore deposit, has many drawbacks.First, at first must make Quilonum Retard or lithium hydroxide product through roasting, acidifying, slurrying, leaching and the preliminary lithium ore leaching liquid-lithium sulfate solution that obtains that concentrates by the lithium ore deposit, turn to the lithium feedstock production or produce lithium chloride with Quilonum Retard or hydrogen-oxygen again, technology is long, step is many must increase the loss of lithium in the process, reduce the total recovery of lithium, caused the waste of valuable lithium resource; The second, produce earlier that Quilonum Retard or lithium hydroxide regeneration are produced in the technology of lithium chloride through repeated washing repeatedly, concentrated, crystallisation by cooling by Lithium Sulphate, cause a large amount of wastes of the energy and water; The 3rd, production line is long, and facility investment is big, and operation sequence is many, the working cost height.
Other preparation lithium chloride methods mainly contain:
The lithium hydroxide chlorination process.Be about to lithium hydroxide and be scattered in the water, adverse current feeds chlorine and makes it circulation, obtains the thick mother liquor of lithium chloride, through separation, washing, removal of impurities, concentrate, obtain Lithium chloride (anhydrous) after the crystallization, drying.
The salt lake brine extraction method, mainly by solvent extraction, ion-exchange absorption or the method for saltouing from containing the salt lake of lithium chloride
Extract lithium chloride in the bittern, but the prematurity still of this method still is in conceptual phase.
Summary of the invention:
The object of the present invention is to provide a kind of operation simple, the preparation method of easy-operating Lithium chloride (anhydrous).
Technical solution of the present invention is:
A kind of preparation method of Lithium chloride (anhydrous) is characterized in that: comprise the following steps:
(1), in lithium sulfate solution, add calcium chloride, obtain lithium chloride and calcium sulfate;
Li
2SO
4+CaCl
2→2LiCl+CaSO
4↓
(2), after filtration and washing, remove CaSO with products therefrom in the step (1)
4, get LiCl solution (mother liquor 1);
(3), with behind mother liquor 1 concentrating under reduced pressure, add barium chloride solution, remove SO with washing after filtration after the reaction
4 2-
SO
4 2-+Ba
2+→BaSO
4↓
(4), the Quilonum Retard solution that in step (3) gained lithium chloride solution, adds, remove Ba with washing after filtration after the reaction
2+, Ca
2+Impurity gets LiCl solution (mother liquor 2);
Ba
2++CO
3 2-→BaCO
3↓
Ca
2++CO
3 2-→CaCO
3↓
(5), step (4) mother liquid obtained 2 is got Lithium chloride (anhydrous) after concentrating under reduced pressure, crystallisation by cooling, separation, drying.
Lithium sulfate solution is lithium ore leaching liquid-lithium sulfate solution in the step (1).
The production method of described Lithium chloride (anhydrous), its concrete steps are as follows:
(1), calcium chloride solution is joined stirring reaction in lithium ore leaching liquid-lithium sulfate solution, reactant molar ratio (CaCl
2/ Li
2SO
4) be 1.0～1.03, temperature of reaction is 70～90 ℃, in 30 minutes～45 minutes reaction times, reaction stops the back insulation and leaves standstill more than 1 hour;
(2), products therefrom in the step (1) is filtered, and with obtain behind 80～95 ℃ of no ion hot wash filter cakes 2～4 times LiCl solution (mother liquor 1):
(3), with the pH value to 7 that hydrochloric acid is regulated mother liquor 1, concentrating under reduced pressure is measured wherein SO
4 2-Content, add and SO
4 2-The barium chloride solution of equimolar amount, stirring reaction, filtration are also removed SO with after 5 ℃～10 ℃ deionized waters washings 2～3 times
4 2-
(4), according to the Ca in step (3) the gained concentrated solution
2+Content, add and Ca
2+The Quilonum Retard solution of equimolar amount washs 2～3 times after the reaction after filtration and with 10～20 ℃ of deionized waters, removes Ba
2+, Ca
2+Deng behind the impurity LiCl solution (mother liquor 2);
(5), the pH value to 7 of regulating mother liquor 2 with hydrochloric acid, concentrating under reduced pressure (secondary concentrates) is to state of saturation, cooling, crystallization, separation, separating back mother liquid obtained 3, to deliver to secondary concentrated.Separate the Lithium chloride (anhydrous) that gained wet crystallization drying in back must meet GB10575-89 industry first grade standard.
It is that the lithium raw material directly prepares the processing method of producing Lithium chloride (anhydrous) that the present invention adopts with lithium ore leaching liquid-lithium sulfate solution.With existing be that the processing method of raw material production lithium chloride is compared with the lithium ore deposit, saved the whole technological process of elder generation by lithium sulfate solution preparation or production Quilonum Retard or lithium hydroxide, thereby operational path shortens greatly, operation steps is greatly simplified, and is easy to operate, reduced energy consumption and water consumption, reduced the loss of lithium in the process, improve the lithium yield, fundamentally overcome many drawbacks that above-mentioned traditional technology method exists, realized lithium chloride preparation technology's innovation.
Description of drawings:
The invention will be further described below in conjunction with drawings and Examples.
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
Embodiment 1
(1) pipetting concentration is that lithium ore leaching liquid-lithium sulfate solution 800ml of 1.6103mol/L is in the beaker of 2000ml.Beaker is placed 70 ℃ water bath with thermostatic control, slowly add the calcium chloride solution that 860ml concentration is 1.5mol/L while stirring, fully react to be incubated after half an hour and left standstill 1.5 hours.
(2) products therefrom in the vacuum filtration step (1), and twice must LiCl solution (mother liquor 1) with 80 ℃ deionized water washing calcium sulfate filter cake.
(3) be evaporated to 500ml after with hydrochloric acid the pH value of mother liquor 1 being transferred to 7, measure its SO
4 2-And Ca
2+Content.
(4) in the concentrated solution of step (3) gained, add the barium chloride solution 85ml of 0.5mol/L concentration while stirring, stirred 20 minutes and left standstill 1 hour after-filtration, and with 10 ℃ of deionized water washed twice.
(5) in the LiCl solution of step (4) gained, add the Quilonum Retard solution 115ml of 0.05mol/L concentration while stirring, stirred 20 minutes and left standstill 1 hour after-filtration, and with after 20 ℃ of deionized water washed twice LiCl solution (mother liquor 2).
(6) be evaporated to saturation concentration after with hydrochloric acid the pH value of mother liquor 2 being transferred to 7, crystallisation by cooling, separation, behind the wet crystallizing and drying of gained the Lithium chloride (anhydrous) product.Measure products obtained therefrom LiCl content 99.05% with atomic absorption spectrophotometry and chemical analysis; SO
4 2-Content 0.04%; K+Na 0.31%; All the other indexs all accord with industrial first grade standard among the GB10575-89.
Embodiment 2
The water bath with thermostatic control temperature is 80 ℃ in embodiment 1 step (1); Temperature of washing water is 85 ℃ in the step (2), and all the other are with embodiment 1.Assay determination products obtained therefrom LiCl content 99.15%; SO
4 2-Content 0.03%; K+Na 0.3%; All the other indexs all accord with industrial first grade standard among the GB10575-89.
Embodiment 3
The calcium chloride solution of the 1.5mol/L that adds in embodiment 1 step (1) is 884ml, and the water bath with thermostatic control temperature is 85 ℃, reacts to be incubated after 45 minutes to leave standstill 2 hours; Temperature of washing water is 85 ℃ in the step (2), washs three times; Add the Quilonum Retard solution 350ml of 0.1mol/L concentration in the step (4), stirred 30 minutes and left standstill 2 hours after-filtration; All the other are with embodiment 1.Assay determination products obtained therefrom LiCl content 99.21%; SO
4 2-Content can't check; K+Na 0.24%; All the other indexs all accord with industrial first grade standard among the GB10575-89.
Embodiment 4
The water bath with thermostatic control temperature is 90 ℃ in embodiment 3 steps (1), reacts to be incubated after 45 minutes to leave standstill 3 hours; Temperature of washing water is 90 ℃ in the step (2); All the other are with embodiment 3.Assay determination products obtained therefrom LiCl content 99.39%; SO
4 2-Content can't check; K+Na 0.21%; All the other indexs all accord with industrial first grade standard among the GB10575-89.
Embodiment 5
The water bath with thermostatic control temperature is 95 ℃ in embodiment 4 steps (1); Temperature of washing water is 95 ℃ in the step (2), and all the other are with embodiment 3.Measure products obtained therefrom LiCl content 99.42% by analysis; SO
4 2-Content can't check; K+Na0.19%; All the other indexs all accord with industrial first grade standard among the GB10575-89.
Embodiment 6
Lithium ore leaching liquid-lithium sulfate solution the concentration that pipettes in embodiment 3 steps (1) is 1.804mol/L, and adding 980ml concentration is the calcium chloride solution of 1.5mol/L; All the other are with embodiment 3.Measure products obtained therefrom LiCl content 99.22% by analysis; SO
4 2-Content can't check; K+Na0.25%; All the other indexs all accord with industrial first grade standard among the GB10575-89.
Embodiment 7
Lithium ore leaching liquid-lithium sulfate solution the concentration that pipettes in embodiment 4 steps (1) is 1.804mol/L, and adding 980ml concentration is the calcium chloride solution of 1.5mol/L; All the other are with embodiment 4.Measure products obtained therefrom LiCl content 99.32% by analysis; SO
4 2-Content can't check; K+Na0.21%; All the other indexs all accord with industrial first grade standard among the GB10575-89.
Embodiment 8
Lithium ore leaching liquid-the lithium sulfate solution that pipettes 1600ml in embodiment 6 steps (1) adds the calcium chloride solution of 1960ml in the reaction vessel of 5000ml; All the other are with embodiment 6.Measure products obtained therefrom LiCl content 99.26% by analysis; SO
4 2-Content can't check; K+Na 0.21%; All the other indexs all accord with industrial first grade standard among the GB10575-89,
Embodiment 9
Lithium ore leaching liquid-the lithium sulfate solution that pipettes 1600ml in embodiment 7 steps (1) in the reaction vessel of 5000ml,
The calcium chloride solution that adds 1960ml; All the other are with embodiment 7.Measure products obtained therefrom LiCl content 99.37% by analysis; SO
4 2-Content can't check; K+Na 0.19%; All the other indexs all accord with industrial first grade standard among the GB10575-89.
Claims (3)
1, a kind of preparation method of Lithium chloride (anhydrous) is characterized in that: comprise the following steps:
(1), in lithium sulfate solution, add calcium chloride, obtain lithium chloride and calcium sulfate;
Li
2SO
4+CaCl
2→2LiCl+CaSO
4↓
(2), after filtration and washing, remove CaSO with products therefrom in the step (1)
4, must be as the LiCl solution of mother liquor 1;
(3), with behind mother liquor 1 concentrating under reduced pressure, add barium chloride solution, remove SO with washing after filtration after the reaction
4 2-
SO
4 2-+Ba
2+→BaSO
4↓
(4), the Quilonum Retard solution that in step (3) gained lithium chloride solution, adds, remove Ba with washing after filtration after the reaction
2+, Ca
2+Impurity must be as the LiCl solution of mother liquor 2;
Ba
2++CO
3 2-→BaCO
3↓
Ca
2++CO
3 2-→CaCO
3↓
(5), step (4) mother liquid obtained 2 is got Lithium chloride (anhydrous) after concentrating under reduced pressure, crystallisation by cooling, separation, drying.
2, the preparation method of Lithium chloride (anhydrous) according to claim 1 is characterized in that: lithium sulfate solution is lithium ore leaching liquid-lithium sulfate solution in the step (1).
3, the preparation method of Lithium chloride (anhydrous) according to claim 1 and 2 is characterized in that: its concrete steps are as follows:
(1), calcium chloride solution is joined stirring reaction in lithium ore leaching liquid-lithium sulfate solution, the mol ratio of reactant calcium chloride and Lithium Sulphate is 1.0～1.03, temperature of reaction is 70～90 ℃, and in 30 minutes～45 minutes reaction times, reaction stops the back insulation and leaves standstill more than 1 hour;
(2), products therefrom in the step (1) is filtered, and with must be behind 80～95 ℃ of no ion hot wash filter cakes 2～4 times as the LiCl solution of mother liquor 1;
(3), with the pH value to 7 that hydrochloric acid is regulated mother liquor 1, concentrating under reduced pressure is measured wherein SO
4 2-Content, add and SO
4 2-The barium chloride solution of equimolar amount, stirring reaction, filtration are also removed SO with after 5 ℃～10 ℃ deionized waters washings 2～3 times
4 2-
(4), according to the Ca in step (3) the gained concentrated solution
2+Content, add and Ca
2+The Quilonum Retard solution of equimolar amount washs 2～3 times after the reaction after filtration and with 10～20 ℃ of deionized waters, removes Ba
2+, Ca
2+Deng must be behind the impurity as the LiCl solution of mother liquor 2;
(5), with the pH value to 7 that hydrochloric acid is regulated mother liquor 2, second depressurized is concentrated into state of saturation, cooling, crystallization, separation separate back mother liquid obtained 3 and deliver to secondary and concentrate, and separate the back gained crystallization drying that wets and get Lithium chloride (anhydrous).
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|---|---|---|---|
| CNB2006100859824A CN100427394C (en) | 2006-06-12 | 2006-06-12 | Method for preparing lithium chloride free from water |
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|---|---|---|---|
| CNB2006100859824A CN100427394C (en) | 2006-06-12 | 2006-06-12 | Method for preparing lithium chloride free from water |
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| CN100427394C true CN100427394C (en) | 2008-10-22 |
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| CN102249471B (en) * | 2011-05-12 | 2012-10-17 | 江西赣锋锂业股份有限公司 | Method for processing battery-level lithium carbonate mother liquor |
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| CN108517423B (en) * | 2018-05-21 | 2020-06-02 | 江西南氏锂电新材料有限公司 | Method for extracting lithium and lithium salt by roasting lepidolite in rotary kiln |
| CN109292798B (en) * | 2018-10-22 | 2021-01-22 | 天齐锂业(射洪)有限公司 | Process for producing anhydrous lithium chloride by crystallization method |
| CN110668474B (en) * | 2019-10-15 | 2022-03-04 | 赣州有色冶金研究所有限公司 | Method for preparing lithium chloride by using chlorine |
| CN110697739B (en) * | 2019-10-18 | 2022-08-12 | 中国铝业股份有限公司 | Method for preparing anhydrous lithium chloride by leaching lithium in aluminum-based lithium-rich slag |
| CN111017965B (en) * | 2019-11-29 | 2022-06-10 | 湖北金泉新材料有限公司 | Preparation method of industrial-grade lithium chloride |
| CN113716587A (en) * | 2021-09-07 | 2021-11-30 | 江苏容汇通用锂业股份有限公司 | Preparation method of lithium fluoride with high lithium yield |
| CN113697829A (en) * | 2021-09-07 | 2021-11-26 | 江苏容汇通用锂业股份有限公司 | Preparation method of lithium fluoride |
| CN116040659A (en) * | 2023-01-17 | 2023-05-02 | 天齐锂业(射洪)有限公司 | Preparation method of battery-grade anhydrous lithium chloride |
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