CN102275956A - Method for extracting lithium carbonate from salt lake brine with high magnesium/lithium ratio - Google Patents

Method for extracting lithium carbonate from salt lake brine with high magnesium/lithium ratio Download PDF

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CN102275956A
CN102275956A CN2011102059769A CN201110205976A CN102275956A CN 102275956 A CN102275956 A CN 102275956A CN 2011102059769 A CN2011102059769 A CN 2011102059769A CN 201110205976 A CN201110205976 A CN 201110205976A CN 102275956 A CN102275956 A CN 102275956A
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solution
salt lake
lake brine
organic phase
extraction agent
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CN102275956B (en
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秦炜
周智勇
谭元忠
梁胜轲
费维扬
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Tsinghua University
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Abstract

The invention discloses a method for extracting lithium carbonate from salt lake brine with high magnesium/lithium ratio, belonging to the technical filed of inorganic salt extraction. The method comprises the following steps of: carrying out extraction, washing and stripping steps to obtain a stripping solution composed of NaCl and LiCl or NH4Cl and LiCl, then introducing CO2 or adding Na2CO3, and controlling the pH value and dynamic conditions to obtain a nanoscale or microscale Li2CO3 product. The method disclosed by the invention has the advantages of simple steps, low equipment requirement and wide sources of raw materials, and is suitable for industrial production.

Description

A kind of method of from the high Mg/Li ratio salt lake brine, extracting Quilonum Retard
Technical field
The invention belongs to inorganic salt extractive technique field, be specifically related to a kind of method of from the high Mg/Li ratio salt lake brine, extracting Quilonum Retard.
Background technology
In recent years, the elemental lithium that is called as " 21st century energy metal " is becoming in the modern industry production to be paid close attention to and hot of research and development.Over nearly 10 years, the aggregate demand of world's lithium is with annual 7%～11% speed sustainable growth, and in the speed increment with annual 20%～25% of the market demand of China's lithium and lithium salts, market value is also being kept ascendant trend always.Lithium resource content is quite abundant in China's salt lake brine, and it is significant for national economy that Quilonum Retard is extracted in exploitation.Quilonum Retard is the basic compound of lithium industry, all is widely used in Production of Ceramics, glass manufacturing, aluminum smelting technology industry and pharmaceutical industries, especially as the base mateiral of producing lithium cell, along with the fast development of lithium cell has a very wide range of applications.Patent US3537813A has proposed a kind of interpolation iron trichloride, does extraction agent extraction lithium, water back extraction organic phase, the method that empty organic phase recycles with 80% diisobutyl ketone-20% tributyl phosphate.Need to add NaCl in the process and replenish the chlorine root, and extract FeCl with two-(2-ethylhexyl) phosphoric acid-tributyl phosphate 3, water is stripped and is reclaimed molysite again.The subject matter that this method exists is that molysite recovery technical process is too loaded down with trivial details, and operation easier is bigger.Patent CN87103431A has proposed to reach in high-content lithium more than the 6mol/L, magnesium, the chloride soln in chlorine root concentration on this basis, add iron trichloride, adopt 50-70%TBP and 30-50%200# solvent kerosene to do extraction agent extraction lithium, organic phase is washed with dilute hydrochloric acid, carry out back extraction with 6-9mol/L HCl again, wash free acid with clear water after the back extraction, with alkali neutralization H wherein +, iron is with HFeCl 4Form is present in organic phase and loops back the extraction section use.The extraction agent that the subject matter that this method exists is to use easily forms third phase in extraction process, accumulation causes working cycle efficient more and more lower, can't extract at last; Use concentration of hydrochloric acid too high in the back extraction process, easily cause acid mist, and serious to equipment corrosion, cyclical operation continuously.
Summary of the invention
The object of the invention is to provide a kind of method of extracting Quilonum Retard from the high Mg/Li ratio salt lake brine.
A kind of method of from the high Mg/Li ratio salt lake brine, extracting Quilonum Retard, carry out according to following steps:
(1) tributyl phosphate and solubility promoter are mixed, make extraction agent, tributyl phosphate, solubility promoter account for 30-80%, the 20%-70% of tributyl phosphate and solubility promoter total mass respectively;
(2) synergist and extraction agent are joined in the salt lake brine successively, the concentration of synergist and lithium concentration ratio are 1: 10～10: 1, and the volume of extraction agent and the volume ratio of salt lake brine are 1: 30～10: 1, extract;
(3) HCl solution and LiCl solution are mixed, make washing composition, the strength of solution of HCl and LiCl is respectively 0.1～6mol/L and 0.1～6mol/L; Add step (2) and separate in the organic phase that obtains, the volume ratio of organic phase and washing composition is 1: 1～30: 1, the washing organic phase;
(4) HCl solution is mixed mutually with NaCl solution, make reverse-extraction agent, the concentration range of HCl solution and NaCl solution is respectively 1～5.99mol/L and 1-5.99mol/L, perhaps with HCl solution and NH 4Cl solution mixes mutually, makes reverse-extraction agent, HCl solution and NH 4The concentration range of Cl solution is respectively 1～5.99mol/L and 1-5.99mol/L, joining step (3) washing back separates in the organic phase that obtains, the volume ratio of organic phase and reverse-extraction agent is 1: 1～20: 1, and back extraction obtains consisting of the strip liquor of NaCl and LiCl, perhaps obtains consisting of NH 4The strip liquor of Cl and LiCl;
(5) use maturation process with NaCl in the strip liquor or NH 4Cl removes, and feeds CO then 2Or adding Na 2CO 3, control pH value and dynamic conditions obtain nano level or micron order Li 2CO 3Product.
Described solubility promoter is alcohol or ketone.
Described alcohol is secondary octanol, isooctyl alcohol or n-Octanol; Described ketone is hexone, methyl phenyl ketone, valerone or 2-heptanone.
Described synergist is iron trichloride, cobalt chloride, Manganous chloride tetrahydrate or chromium trichloride.
Beneficial effect of the present invention: 1, use alcohols or ketone to make solubility promoter, divide phase velocity fast, equal no third occurs mutually in the experimental concentration scope, the working cycle smoothness, organic phase recycles efficient and does not occur reducing, and lithium partition ratio and lithium magnesium separation factor significantly are the system of thinner greater than kerosene, and the solvent loss in the full cycle process of high level salt solution of alcohols or ketone is less.2, washing composition consists of LiCl+HCl, to the corrosion of equipment and carrying secretly of HCl, saves subsequent processing steps in the reduction washing process.3, for guarantee that molysite resides in organic phase and recycles always, need to guarantee certain chlorine root concentration in the back extraction process, on this basis with NaCl or NH 4Cl substitutes the part concentrated hydrochloric acid, to reduce its acid mist that brings and to the corrosion of equipment, can save simultaneously clear water wash acid and in and step such as H+.4, combining global CO 2The reduction of discharging theory is to removing NaCl or NH 4Feed CO in the solution that Cl obtains 2Or adding Na 2CO 3, control pH and dynamic conditions directly obtain nano level or micron-sized Li 2CO 3, can directly sell as finished product, saved the cost of post-treatment.
Description of drawings
Fig. 1 extracts the process flow sheet of Quilonum Retard from the high Mg/Li ratio salt lake brine for the present invention.
Embodiment
The present invention will be further described below in conjunction with the drawings and specific embodiments.
Following examples all adopt technology as shown in Figure 1.
Embodiment 1
Preparation simulation salt lake brine consists of lithium (0.05mol/L), magnesium (3.5mol/L) and chlorine (7.05mol/L).
The step of extracting Quilonum Retard from above-mentioned simulation salt lake brine is as follows:
(1) tributyl phosphate and valerone are mixed, make extraction agent, tributyl phosphate, valerone account for 50%, 50% of tributyl phosphate and solubility promoter cumulative volume respectively;
(2) iron trichloride and extraction agent are joined in the salt lake brine successively, the concentration of iron trichloride and lithium concentration ratio are 2: 1, and the volume of extraction agent and the volume ratio of salt lake brine are 1: 1, extract;
(3) HCl solution and LiCl solution are mixed, make washing composition, the strength of solution of HCl and LiCl is respectively 1mol/L and 1mol/L; Add step (2) and separate in the organic phase that obtains, the volume ratio of organic phase and washing composition is 20: 1, the washing organic phase;
(4) HCl solution is mixed mutually with NaCl solution, make reverse-extraction agent, the concentration of HCl solution and NaCl solution is respectively 1mol/L and 2mol/L, joining step (3) washing back separates in the organic phase that obtains, the volume ratio of organic phase and reverse-extraction agent is 10: 1, and back extraction obtains consisting of the strip liquor of NaCl and LiCl;
(5) use maturation process that the NaCl in the strip liquor is removed, feed CO then 2Or adding Na 2CO 3, control pH value and dynamic conditions obtain nano level or micron order Li 2CO 3Product.
Present embodiment single-stage lithium percentage extraction is 75%, and single-stage lithium magnesium separation factor can reach 270.Through the two-stage extraction, the one-level washing, the lithium total yield reaches more than 92% after the two-stage back extraction.
Embodiment 2
Preparation simulation salt lake brine consists of lithium (0.05mol/L), magnesium (3.5mol/L) and chlorine (7.05mol/L).
The step of extracting Quilonum Retard from above-mentioned simulation salt lake brine is as follows:
(1) tributyl phosphate and secondary octanol are mixed, make extraction agent, tributyl phosphate, secondary octanol account for 80%, 20% of tributyl phosphate and solubility promoter cumulative volume respectively;
(2) chromium trichloride and extraction agent are joined in the salt lake brine successively, the concentration of chromium trichloride and lithium concentration ratio are 2: 1, and the volume of extraction agent and the volume ratio of salt lake brine are 2: 1, extract;
(3) HCl solution and LiCl solution are mixed, make washing composition, the strength of solution of HCl and LiCl is respectively 1mol/L and 1mol/L; Add step (2) and separate in the organic phase that obtains, the volume ratio of organic phase and washing composition is 15: 1, the washing organic phase;
(4) HCl solution is mixed mutually with NaCl solution, make reverse-extraction agent, the concentration of HCl solution and NaCl solution is respectively 2mol/L and 1mol/L, joining step (3) washing back separates in the organic phase that obtains, the volume ratio of organic phase and reverse-extraction agent is 10: 1, and back extraction obtains consisting of the strip liquor of NaCl and LiCl;
(5) use maturation process that the NaCl in the strip liquor is removed, feed CO then 2Or adding Na 2CO 3, control pH value and dynamic conditions obtain nano level or micron order Li 2CO 3Product.
Present embodiment single-stage lithium percentage extraction is 22%.Through seven grades of extractions, the one-level washing, the lithium total yield reaches more than 85% after the two-stage back extraction.
Embodiment 3
Preparation simulation salt lake brine, lithium (0.2mol/L), magnesium (4.0mol/L), sodium (0.07mol/L), potassium (0.02) and chlorine (8.29mol/L).
The step of extracting Quilonum Retard from above-mentioned simulation salt lake brine is as follows:
(1) tributyl phosphate and n-Octanol are mixed, make extraction agent, tributyl phosphate, n-Octanol account for 80%, 20% of tributyl phosphate and solubility promoter cumulative volume respectively;
(2) iron trichloride and extraction agent are joined in the salt lake brine successively, the concentration of iron trichloride and lithium concentration ratio are 1.5: 1, and the volume of extraction agent and the volume ratio of salt lake brine are 1: 1, extract;
(3) HCl solution and LiCl solution are mixed, make washing composition, the strength of solution of HCl and LiCl is respectively 1mol/L and 1mol/L; Add step (2) and separate in the organic phase that obtains, the volume ratio of organic phase and washing composition is 30: 1, the washing organic phase;
(4) HCl solution is mixed mutually with NaCl solution, make reverse-extraction agent, the concentration of HCl solution and NaCl solution is respectively 2mol/L and 2mol/L, joining step (3) washing back separates in the organic phase that obtains, the volume ratio of organic phase and reverse-extraction agent is 10: 1, and back extraction obtains consisting of the strip liquor of NaCl and LiCl;
(5) use maturation process that the NaCl in the strip liquor is removed, feed CO then 2Or adding Na 2CO 3, control pH value and dynamic conditions obtain nano level or micron order Li 2CO 3Product.
Present embodiment single-stage lithium percentage extraction is 70%, and single-stage lithium magnesium separation factor can reach 210.Through the two-stage extraction, the one-level washing, the lithium total yield reaches more than 89% after the two-stage back extraction.
Embodiment 4
Preparation simulation salt lake brine, lithium (0.2mol/L), magnesium (4.0mol/L), sodium (0.07mol/L), potassium (0.02) and chlorine (8.29mol/L).
The step of extracting Quilonum Retard from above-mentioned simulation salt lake brine is as follows:
(1) tributyl phosphate and hexone are mixed, make extraction agent, tributyl phosphate, hexone account for 80%, 20% of tributyl phosphate and solubility promoter cumulative volume respectively;
(2) iron trichloride and extraction agent are joined in the salt lake brine successively, the concentration of iron trichloride and lithium concentration ratio are 1.5: 1, and the volume of extraction agent and the volume ratio of salt lake brine are 1: 1, extract;
(3) HCl solution and LiCl solution are mixed, make washing composition, the strength of solution of HCl and LiCl is respectively 1mol/L and 1mol/L; Add step (2) and separate in the organic phase that obtains, the volume ratio of organic phase and washing composition is 20: 1, the washing organic phase;
(4) HCl solution is mixed mutually with NaCl solution, make reverse-extraction agent, the concentration of HCl solution and NaCl solution is respectively 0.5mol/L and 2mol/L, joining step (3) washing back separates in the organic phase that obtains, the volume ratio of organic phase and reverse-extraction agent is 10: 1, and back extraction obtains consisting of the strip liquor of NaCl and LiCl;
(5) use maturation process that the NaCl in the strip liquor is removed, feed CO then 2Or adding Na 2CO 3, control pH value and dynamic conditions obtain nano level or micron order Li 2CO 3Product.
Present embodiment single-stage lithium percentage extraction is 75%, and single-stage lithium magnesium separation factor can reach 200.Through the two-stage extraction, the one-level washing, the lithium total yield reaches more than 90% after the two-stage back extraction.
Embodiment 5
Preparation simulation salt lake brine, lithium (0.05mol/L), magnesium (3.5mol/L) and chlorine (7.05mol/L).
The step of extracting Quilonum Retard from above-mentioned simulation salt lake brine is as follows:
(1) tributyl phosphate and hexone are mixed, make extraction agent, tributyl phosphate, hexone account for 50%, 50% of tributyl phosphate and solubility promoter cumulative volume respectively;
(2) iron trichloride and extraction agent are joined in the salt lake brine successively, the concentration of iron trichloride and lithium concentration ratio are 2: 1, and the volume of extraction agent and the volume ratio of salt lake brine are 1: 1, extract;
(3) HCl solution and LiCl solution are mixed, make washing composition, the strength of solution of HCl and LiCl is respectively 1mol/L and 1mol/L; Add step (2) and separate in the organic phase that obtains, the volume ratio of organic phase and washing composition is 15: 1, the washing organic phase;
(4) HCl solution is mixed mutually with NaCl solution, make reverse-extraction agent, the concentration of HCl solution and NaCl solution is respectively 1mol/L and 2mol/L, joining step (3) washing back separates in the organic phase that obtains, the volume ratio of organic phase and reverse-extraction agent is 10: 1, and back extraction obtains consisting of the strip liquor of NaCl and LiCl;
(5) use maturation process that the NaCl in the strip liquor is removed, feed CO then 2Or adding Na 2CO 3, control pH value and dynamic conditions obtain nano level or micron order Li 2CO 3Product.
Present embodiment single-stage lithium percentage extraction is 80%, and single-stage lithium magnesium separation factor can reach 230.Through the two-stage extraction, the one-level washing, the lithium total yield reaches more than 93% after the two-stage back extraction..

Claims (4)

1. a method of extracting Quilonum Retard from the high Mg/Li ratio salt lake brine is characterized in that, carries out according to following steps:
(1) tributyl phosphate and solubility promoter are mixed, make extraction agent, tributyl phosphate, solubility promoter account for 30-80%, the 20%-70% of tributyl phosphate and solubility promoter total mass respectively;
(2) synergist and extraction agent are joined in the salt lake brine successively, the concentration of synergist and lithium concentration ratio are 1: 10～10: 1, and the volume of extraction agent and the volume ratio of salt lake brine are 1: 30～10: 1, extract;
(3) HCl solution and LiCl solution are mixed, make washing composition, the strength of solution of HCl and LiCl is respectively 0.1～6mol/L and 0.1～6mol/L; Add step (2) and separate in the organic phase that obtains, the volume ratio of organic phase and washing composition is 1: 1～30: 1, the washing organic phase;
(4) HCl solution is mixed mutually with NaCl solution, make reverse-extraction agent, the concentration range of HCl solution and NaCl solution is respectively 1～5.99mol/L and 1-5.99mol/L, perhaps with HCl solution and NH 4Cl solution mixes mutually, makes reverse-extraction agent, HCl solution and NH 4The concentration range of Cl solution is respectively 1～5.99mol/L and 1-5.99mol/L, joining step (3) washing back separates in the organic phase that obtains, the volume ratio of organic phase and reverse-extraction agent is 1: 1～20: 1, and back extraction obtains consisting of the strip liquor of NaCl and LiCl, perhaps obtains consisting of NH 4The strip liquor of Cl and LiCl;
(5) use maturation process with NaCl in the strip liquor or NH 4Cl removes, and feeds CO then 2Or adding Na 2CO 3, control pH value and dynamic conditions obtain nano level or micron order Li 2CO 3Product.
2. according to the described a kind of method of from the high Mg/Li ratio salt lake brine, extracting Quilonum Retard of claim 1, it is characterized in that described solubility promoter is alcohol or ketone.
3. according to the described a kind of method of from the high Mg/Li ratio salt lake brine, extracting Quilonum Retard of claim 2, it is characterized in that described alcohol is secondary octanol, isooctyl alcohol or n-Octanol; Described ketone is hexone, methyl phenyl ketone, valerone or 2-heptanone.
4. according to the described a kind of method of from the high Mg/Li ratio salt lake brine, extracting Quilonum Retard of claim 1, it is characterized in that described synergist is iron trichloride, cobalt chloride, Manganous chloride tetrahydrate or chromium trichloride.
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CN102633284A (en) * 2012-05-08 2012-08-15 湘潭大学 Method for separating magnesium and extracting lithium from salt lake brine with high magnesium-lithium ratio
CN102897804A (en) * 2012-09-18 2013-01-30 清华大学 Method for preparing lithium carbonate directly from lithium chloride and carbon dioxide
CN102992358A (en) * 2012-02-24 2013-03-27 中国科学院青海盐湖研究所 Method for extracting lithium salt from lithium brine
CN105152190A (en) * 2015-09-18 2015-12-16 湘潭大学 Method for producing lithium carbonate by separating magnesium out of low-lithium bittern and enriching lithium
CN105347364A (en) * 2015-10-30 2016-02-24 华陆工程科技有限责任公司 Method for closed-loop recycling of lithium precipitation mother liquor in lithium carbonate production
CN105645443A (en) * 2016-01-07 2016-06-08 上海颐润科技有限公司 Method for lithium salts from high-magnesium lithium-containing brine
CN106745102A (en) * 2017-01-17 2017-05-31 青海盐湖工业股份有限公司 A kind of preparation technology of lithium carbonate
CN109019642A (en) * 2018-10-11 2018-12-18 清华大学 A method of extracting lithium carbonate from salt lake bittern
CN109536741A (en) * 2017-12-16 2019-03-29 虔东稀土集团股份有限公司 A kind of extracting process of elemental lithium
CN109762987A (en) * 2019-03-06 2019-05-17 清华大学 Dialkyl sulfone extractant and the method that lithium is extracted from salt lake bittern
WO2019114815A1 (en) * 2017-12-16 2019-06-20 虔东稀土集团股份有限公司 Extraction solvent for lithium element and extraction method therefor
WO2019114817A1 (en) * 2017-12-16 2019-06-20 虔东稀土集团股份有限公司 Extraction solvent and method thereof for extracting and separating lithium element
CN112342405A (en) * 2019-08-09 2021-02-09 浙江新化化工股份有限公司 Method for extracting lithium from lithium-containing solution
CN112342406A (en) * 2019-08-09 2021-02-09 浙江新化化工股份有限公司 Method for extracting lithium from salt lake brine
CN114318937A (en) * 2020-09-27 2022-04-12 牡丹江市海洋新材料科技有限责任公司 Novel method for combined use of soluble silicate, polyaluminium chloride and flocculant in multiple fields

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CN102992358A (en) * 2012-02-24 2013-03-27 中国科学院青海盐湖研究所 Method for extracting lithium salt from lithium brine
CN102633284B (en) * 2012-05-08 2014-03-19 湘潭大学 Method for separating magnesium and extracting lithium from salt lake brine with high magnesium-lithium ratio
CN102633284A (en) * 2012-05-08 2012-08-15 湘潭大学 Method for separating magnesium and extracting lithium from salt lake brine with high magnesium-lithium ratio
CN102897804A (en) * 2012-09-18 2013-01-30 清华大学 Method for preparing lithium carbonate directly from lithium chloride and carbon dioxide
CN105152190A (en) * 2015-09-18 2015-12-16 湘潭大学 Method for producing lithium carbonate by separating magnesium out of low-lithium bittern and enriching lithium
WO2017045485A1 (en) * 2015-09-18 2017-03-23 湘潭大学 Method for producing lithium carbonate by separating magnesium from and enriching lithium in low-lithium brine
CN105347364A (en) * 2015-10-30 2016-02-24 华陆工程科技有限责任公司 Method for closed-loop recycling of lithium precipitation mother liquor in lithium carbonate production
CN105645443B (en) * 2016-01-07 2018-07-20 上海颐润科技有限公司 A method of extracting lithium salts from high-Mg Li-contained bittern
CN105645443A (en) * 2016-01-07 2016-06-08 上海颐润科技有限公司 Method for lithium salts from high-magnesium lithium-containing brine
CN106745102B (en) * 2017-01-17 2018-11-23 青海盐湖工业股份有限公司 A kind of preparation process of lithium carbonate
CN106745102A (en) * 2017-01-17 2017-05-31 青海盐湖工业股份有限公司 A kind of preparation technology of lithium carbonate
CN109536741A (en) * 2017-12-16 2019-03-29 虔东稀土集团股份有限公司 A kind of extracting process of elemental lithium
WO2019114815A1 (en) * 2017-12-16 2019-06-20 虔东稀土集团股份有限公司 Extraction solvent for lithium element and extraction method therefor
WO2019114817A1 (en) * 2017-12-16 2019-06-20 虔东稀土集团股份有限公司 Extraction solvent and method thereof for extracting and separating lithium element
CN109536741B (en) * 2017-12-16 2020-11-06 虔东稀土集团股份有限公司 Extraction method of lithium element
CN109019642A (en) * 2018-10-11 2018-12-18 清华大学 A method of extracting lithium carbonate from salt lake bittern
CN109019642B (en) * 2018-10-11 2020-09-11 清华大学 Method for extracting lithium carbonate from salt lake brine
CN109762987A (en) * 2019-03-06 2019-05-17 清华大学 Dialkyl sulfone extractant and the method that lithium is extracted from salt lake bittern
CN112342405A (en) * 2019-08-09 2021-02-09 浙江新化化工股份有限公司 Method for extracting lithium from lithium-containing solution
CN112342406A (en) * 2019-08-09 2021-02-09 浙江新化化工股份有限公司 Method for extracting lithium from salt lake brine
CN114318937A (en) * 2020-09-27 2022-04-12 牡丹江市海洋新材料科技有限责任公司 Novel method for combined use of soluble silicate, polyaluminium chloride and flocculant in multiple fields

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