CN102372295A - Method for separating magnesium and concentrating lithium in brine - Google Patents
Method for separating magnesium and concentrating lithium in brine Download PDFInfo
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- CN102372295A CN102372295A CN2010102500649A CN201010250064A CN102372295A CN 102372295 A CN102372295 A CN 102372295A CN 2010102500649 A CN2010102500649 A CN 2010102500649A CN 201010250064 A CN201010250064 A CN 201010250064A CN 102372295 A CN102372295 A CN 102372295A
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- Prior art keywords
- bittern
- lithium
- magnesium
- evaporation
- high temperature
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a method for separating magnesium and concentrating lithium in brine, comprising the following steps: first, changing the brine composition through chemical reactions to form brine comprising lithium, magnesium, chlorine ions, and sulfate radical as major ingredients; second, carrying out forced high temperature evaporation on the brine comprising lithium, magnesium, chlorine ions, and sulfate radical as major ingredients to form a solid comprising magnesium sulfate and magnesium chloride as major ingredients and brine with reduced magnesium-lithium ratio, and carrying out forced high temperature evaporation on the brine to further reduce the magnesium-lithium ratio, wherein, the forced high temperature evaporation comprises reduced pressure evaporation and normal pressure evaporation, and the formed solid can be washed, returned to the salt pan, returned to forced evaporation and the like to recover lithium. The method has the characteristics of energy saving, environmental protection, high lithium recovery rate and the like.
Description
Technical field
The present invention relates to the method for separating magnesium and concentrated lithium from bittern, after especially changing bittern and form, force high temperature evaporation to come separating magnesium and concentrated lithium through chemical reaction.
Background technology
Contain in the bittern that the lithium salts lake bittern water progressively concentrates gained after the Crystallization Separation crystal salt and often contain materials such as potassium, magnesium, sulfate radical, carbonate, cl ions, be from bittern economic extraction lithium then must be earlier separating magnesium lithium effectively.At present, in the method for the multiple separating magnesium lithium that people have developed, as: alkaline process precipitate and separate magnesium lithium, membrane separation process, salimetry, organic solvent extractionprocess, ionic adsorption method, hydrothermal decomposition-roasting lixiviation process etc.When Mg/Li ratio was higher in the feed liquid, it was big to run into material cost height, equipment corrosion, chemical reagent consumption with aforesaid method separating magnesium lithium, etc. problem.These problems will seriously influence the economic worth of from salt lake brine, extracting lithium.
Summary of the invention
The purpose of this invention is to provide and a kind ofly form, adopt the method for forcing high temperature evaporation crystallization process separating magnesium lithium and concentrated lithium from salt lake brine then through changing bittern.This method technology is simple, strong operability, comprehensive cost are low.
The object of the invention can be realized through following measure:
First: will contain lithium, the magnesium salts lake bittern water is sent into reaction kettle, and through some chemical reactions bittern formed and changed, and add calcium chloride or liming like carbon containing acid group bittern; Form ZG 301; The sulfur-bearing acid group is higher than 5% bittern adding calcium chloride or liming clear liquid, generates calcium sulfate precipitation, after the solid-liquid separation; Becoming staple is the bittern of lithium, magnesium, chlorine root, sulfate radical; After can carrying out spontaneous evaporation, acidifying earlier and put forward means such as boron and separate potassium, boron for the bittern that contains elements such as potassium, boron in the bittern, carry out some chemical reactions again, making bittern become with lithium, magnesium, chlorine root, sulfate radical is the bittern of staple.
Second: to staple is that the bittern of lithium, magnesium, chlorine root, sulfate radical is analyzed; Sulfate radical content does not generate lithium potassium sulfate etc. with evaporative process and contains lithium vitriol and exceed (not being higher than 4% usually) in the bittern, bittern is evaporated, through forcing high temperature evaporation; The evaporation means comprise reduction vaporization and atmospheric evaporation; Steam part moisture, crystallisation by cooling separates out with magnesium chloride and sal epsom to be master's solid, to obtain the low bittern of Mg/Li ratio then.The mother liquor that this step is separated can be used as carries lithium solution, also can utilize once more and force high temperature evaporation crystallization, the mother liquor that the output Mg/Li ratio is lower, the also available reduction vaporization of available atmospheric evaporation.The solid of being separated can be through washing, return the salt pan or returning the forced evaporation crystallisation process and fall the recovery of realization elemental lithium.
Effect of the present invention: compare with prior art, the present invention has following advantage:
1. the invention provides the new technology that reclaims lithium from the salt lake brine kind.
2. this method is simple to operate, and through the bittern behind the chemistry remodeling, through the one or many evaporation operation, it is low to obtain Mg/Li ratio, is convenient to directly carry the solution of lithium, greatly reduces reagent consumption.
3. the lithium in the solid can reclaim through returning the salt pan, wash or return the forced evaporation process, and the yield of lithium is improved.
Below in conjunction with embodiment the present invention is done further explain.
Embodiment
Embodiment one:
To contain SO
4 2-4%, Li
+0.5%, Mg
2+7.5% original bittern spontaneous evaporation obtains containing magnesium 9%, contains the solid of lithium 0.7% and contains magnesium 9%, contains the liquid of lithium 0.3%, and this solid adds that lithium content still is 0.5% after the water washing, and original bittern adds the calcium chloride reaction and generates SO
4 2-1.5%, Li
+0.5%, Mg
2+Behind 7.5% the bittern, forced evaporation, cooling, separating out with sal epsom and magnesium chloride is the solid of staple, and its liquid phase consists of and contains magnesium 8%, contains the liquid of lithium 0.9%, and its solid is after washing, and lithium content is 0.03%.
Embodiment two:
To contain SO
4 2-4%, Li
+0.5%, Mg
2+7.5% original bittern adds the liming reaction and generates SO
4 2-1.2%, Li
+0.5%, Mg
2+Behind 6.7% the bittern, forced evaporation, cooling, separating out with sal epsom and magnesium chloride is the solid of staple, and liquid phase consists of and contains magnesium 5.7% after separating, and contains the liquid of lithium 2.2%, and its solid is after washing, and lithium content is 0.03%.
Embodiment three:
To contain SO
4 2-3.7%, CO
3 2-1.9%, Li
+0.1%, Mg
2+0.3% original bittern adds the calcium chloride reaction, after the solid-liquid separation, and the bittern forced evaporation; Cooling, separating out with sal epsom and magnesium chloride is the solid of staple, its liquid phase consists of and contains magnesium 1.1%; The solid that the liquid that contains lithium 0.9%, evaporative crystallization are separated out is after washing, and lithium content is 0.02%.
Embodiment four:
To contain SO
4 2-3.7%, CO
3 2-1.9%, Li
+0.1%, Mg
2+0.3% original bittern adds the liming reaction, after the solid-liquid separation, and the bittern forced evaporation; Cooling, separating out with sal epsom and magnesium chloride is the solid of staple, its liquid phase consists of and contains magnesium 0.7%; The solid that the liquid that contains lithium 0.4%, evaporative crystallization are separated out is after washing, and lithium content is 0.02%.
Embodiment five:
To contain SO
4 2-4.1%, B
2O
31.7%, Li
+0.4%, Mg
2+10.7% original bittern adds hydrochloric acid reaction, and solid-liquid separation is removed B
2O
3After, the bittern forced evaporation, cooling, separating out with sal epsom and magnesium chloride is the solid of staple, and its liquid phase consists of and contains magnesium 6.2%, contains the liquid of lithium 2.3%, and the solid that evaporative crystallization is separated out is after washing, and lithium content is 0.02%.
Embodiment six:
To contain K
+2.1%, SO
4 2-2.9%, Cl
-15%Li
+0.04%, Mg
2+1.6% original bittern through spontaneous evaporation, is removed sylvite successively, after epsom salt, carnallitite etc. contain potassium, magnesium elements salt, at Li
+Before separating out, add hydrochloric acid, calcium chloride and bittern reaction, solid-liquid separation after reaction is accomplished; The bittern warp is forced evaporation repeatedly, cooling, and separating out with sal epsom and magnesium chloride is the solid of staple; Its liquid phase consists of and contains magnesium 3.3%; The solid that the liquid that contains lithium 2.7%, evaporative crystallization are separated out is after washing, and lithium content is 0.02%.
Claims (4)
1. the purpose of this invention is to provide and a kind ofly form, adopt the method for forcing high temperature evaporation crystallization process separating magnesium lithium and concentrated lithium from salt lake brine then through changing bittern.It is characterized by first: will contain lithium, the magnesium salts lake bittern water is sent into reaction kettle; Through some chemical reactions bittern is formed change; Becoming with lithium, magnesium, chlorine root, sulfate radical is the bittern of staple; After can carrying out spontaneous evaporation, acidifying earlier and put forward means such as boron and separate potassium, boron for the bittern that contains elements such as potassium, boron in the bittern, carry out some chemical reactions again, make bittern become the bittern that staple is lithium, magnesium, chlorine root, sulfate radical.Second: to staple is that the bittern of lithium, magnesium, chlorine root, sulfate radical is analyzed; Sulfate radical content does not generate lithium potassium sulfate etc. with evaporative process and contains lithium vitriol and exceed (not being higher than 4% usually) in the bittern, bittern is evaporated, through forcing high temperature evaporation; The evaporation means comprise reduction vaporization and atmospheric evaporation; Steam part moisture, crystallisation by cooling separates out with bischofite and epsom salt to be master's solid, to obtain the low bittern of Mg/Li ratio then.The mother liquor that this step is separated can be used as carries lithium solution, also can utilize once more and force high temperature evaporation crystallization, the mother liquor that the output Mg/Li ratio is lower, the also available reduction vaporization of available atmospheric evaporation.The solid of being separated can be through washing, return the salt pan or returning the forced evaporation crystallisation process and fall the recovery of realization elemental lithium.
2. of right 1; To contain lithium, the magnesium salts lake bittern water is sent into reaction kettle; Through some chemical reactions bittern form is changed, becoming staple is the bittern of lithium, magnesium, chlorine root, sulfate radical, after can carrying out spontaneous evaporation, acidifying earlier and put forward means such as boron and separate potassium, boron for the bittern that contains elements such as potassium, boron in the bittern; Carry out some chemical reactions again, make bittern become the bittern that staple is lithium, magnesium, chlorine root, sulfate radical.
3. of right 1; To staple is that the bittern of lithium, magnesium, chlorine root, sulfate radical is analyzed, and sulfate radical content does not generate lithium potassium sulfate etc. with evaporative process and contains lithium vitriol and exceed (not being higher than 4% usually) in the bittern, and bittern is evaporated; Through forcing high temperature evaporation; The evaporation means comprise reduction vaporization and atmospheric evaporation part moisture, and crystallisation by cooling separates out with magnesium chloride and sal epsom to be master's solid, to obtain the low bittern of Mg/Li ratio then.
4. of right 1, can be used as through the mother liquor of forcing high temperature evaporation to be separated and to carry lithium solution, also can utilize once more and force the high temperature evaporation crystallization, the mother liquor that the output Mg/Li ratio is lower, forced evaporation can also can be reduction vaporization with atmospheric evaporation.The solid of being separated can be through washing, return the salt pan or returning the forced evaporation crystallisation process and fall the recovery of realization elemental lithium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102500649A CN102372295A (en) | 2010-08-11 | 2010-08-11 | Method for separating magnesium and concentrating lithium in brine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102500649A CN102372295A (en) | 2010-08-11 | 2010-08-11 | Method for separating magnesium and concentrating lithium in brine |
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| Publication Number | Publication Date |
|---|---|
| CN102372295A true CN102372295A (en) | 2012-03-14 |
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|---|---|---|---|
| CN2010102500649A Pending CN102372295A (en) | 2010-08-11 | 2010-08-11 | Method for separating magnesium and concentrating lithium in brine |
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| Country | Link |
|---|---|
| CN (1) | CN102372295A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103318928A (en) * | 2013-06-20 | 2013-09-25 | 西藏金浩投资有限公司 | Method and system for rapid extraction of lithium carbonate from salt lake water |
| CN103508472A (en) * | 2013-10-08 | 2014-01-15 | 中国科学院青海盐湖研究所 | Method for enriching lithium and removing calcium in oil filed water by utilizing evaporating-freezing principle |
| CN106334445A (en) * | 2016-08-23 | 2017-01-18 | 中国科学院青海盐湖研究所 | Method for concentrating mother liquor before extraction of lithium of saline lake |
| CN108439436A (en) * | 2018-04-10 | 2018-08-24 | 中蓝长化工程科技有限公司 | A kind of preparation process of sulfuric acid monohydrate lithium |
| CN110713195A (en) * | 2019-11-27 | 2020-01-21 | 青海民族大学 | Method for improving production efficiency of chloride type salt pan and chloride type salt pan product |
| 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 |
-
2010
- 2010-08-11 CN CN2010102500649A patent/CN102372295A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103318928A (en) * | 2013-06-20 | 2013-09-25 | 西藏金浩投资有限公司 | Method and system for rapid extraction of lithium carbonate from salt lake water |
| CN103318928B (en) * | 2013-06-20 | 2014-12-03 | 西藏金浩投资有限公司 | Method and system for rapid extraction of lithium carbonate from salt lake water |
| CN103508472A (en) * | 2013-10-08 | 2014-01-15 | 中国科学院青海盐湖研究所 | Method for enriching lithium and removing calcium in oil filed water by utilizing evaporating-freezing principle |
| CN106334445A (en) * | 2016-08-23 | 2017-01-18 | 中国科学院青海盐湖研究所 | Method for concentrating mother liquor before extraction of lithium of saline lake |
| CN108439436A (en) * | 2018-04-10 | 2018-08-24 | 中蓝长化工程科技有限公司 | A kind of preparation process of sulfuric acid monohydrate lithium |
| CN110713195A (en) * | 2019-11-27 | 2020-01-21 | 青海民族大学 | Method for improving production efficiency of chloride type salt pan and chloride type salt pan product |
| 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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Application publication date: 20120314 |