CN105439176B - It is a kind of that the process for preparing high-purity lithium salts is extracted from high-Mg Li-contained bittern - Google Patents
It is a kind of that the process for preparing high-purity lithium salts is extracted from high-Mg Li-contained bittern Download PDFInfo
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Abstract
The invention discloses the process that a kind of extraction from high-Mg Li-contained bittern prepares high-purity lithium salts.The process comprises the following steps：Extraction step, FeCl is added into high-Mg Li-contained bittern3With extractant tributyl phosphate, the extraction system that load lithium is obtained by extraction of lithium is carried out；Exchange step, is mixed using Aqueous Lithium Salts with the extraction system of foregoing load lithium, and the other impurities in extraction system to remove load lithium obtain loading the extraction system of high purity lithium；Stripping steps, the extraction system of foregoing load high purity lithium is stripped with acid solution, the aqueous phase containing high-purity lithium salts is obtained, aqueous phase obtains high-purity lithium salts after being evaporated.Using the present invention, increase exchange step in the lithium extraction process of high-Mg Li-contained bittern, the aqueous solution containing lithium is swapped with the impurity in extraction system, so as to improve the purity that lithium is loaded in extraction system, high-purity lithium salts is made.
Description
Technical field
The invention belongs to technical field of chemical separation, and in particular to one kind extraction from high-Mg Li-contained bittern prepares high purity lithium
The process of salt.
Background technology
The pollution of environment and the reduction of petroleum reserves, energy crisis have increasingly threatened the stable sustainable development of society,
Lithium as a kind of high-energy-density electric energy carrier, it has also become reduce environmental pollution, the strategy metal restructured the use of energy claimed
For " energy metal of 21st century ", " industrial monosodium glutamate ", strategic position is notable.Current high-purity lithium salts is in electronics new material and newly
The application of the high-technology fields such as the energy constantly expands, and is widely used in industries such as lithium battery, medicine.Lithium power vehicle
Rise so that the demand to pure lithium salts is more urgent.
China is a lithium resource big country, and wherein salt lake bittern resource accounts for the 80% of gross reserves.Only Qinghai and Tibetan Salt Lakes
The reserves of lithium are just suitable with the gross reserves that other countries of the world have been verified at present in bittern.It is estimated that Chaidamu Basin, Qinghai Province
Petrographic province lithium chloride reserves are 27,000,000 tons, are ranked first in the country.The utilization of Lithium from Salt Lake Brine resource is the exploitation heat of countries in the world
Point, China's saline lake lithium resource enriches, and the exploitation of saline lake lithium resource have important strategic importance to China.However, China
Magnesium ion content is high in salt lake, generally high-Mg Li-contained bittern.The alkali number for being consumed magnesium precipitate using chemical method is too big, and cost is high
It is big with environmental hazard.Simultaneously as obtaining the lithium salts ratio of high-purity in separation process containing other a large amount of ions in salt lake bittern
It is more difficult, complex technical process.Therefore realize that the extraction of high purity lithium is extremely important using simple process conditions.
It is the effective ways that salt lake bittern lithium is extracted using extraction.Current extraction extracts the work of lithium from salt lake bittern
Skill technology Patents have：Robert D in 1963 just extract lithium using urea ketone extractant from sulphate lake
(US3306712A)；Qinghai Yanhu Inst., Chinese Academy of Sciences Huang Shi Qiang in 1987 et al. by extraction system of tributyl phosphate from
Lithium (CN1005145B) is extracted in salt lake bittern；Southern Yangtze University is disclosed using TBP- ion liquid abstractions system separation salt lake halogen
Lithium (CN1017678 0A) in water；Yanhu Inst., Chinese Academy of Sciences's Lee's hamming is with TBP-CON-KS extraction systems separation bittern
Lithium ion (CN101698488A)；Organic chemistry research institute of the Chinese Academy of Sciences also has with tributyl phosphate (TBP) and amide-type
The research (CN201210164159) of lithium ion in extraction system separation bittern.Above-mentioned patent document is proved from high-Mg Li-contained bittern
Middle extraction lithium ion, is feasible using the extracting process of the extraction system of tributyl phosphate (TBP).Using TBP extractants
Extracting technological method generally comprises extracting-back extraction technical process.Patent of invention CN87103431 report extraction-washing-back extraction-
Sour technique separation bittern lithium resource is washed, patent CN201210055323 adds alkali metal on the basis of patent CN87103431
The technique of chloride or alkaline-earth metal phase inversion.But still have a certain amount of impurity, such as magnesium ion in final products, patent report
Lithium salts product purity also needs to improve in many applications.Existing high-Mg Li-contained bittern carries in lithium technology and does not refer to high purity lithium
The committed step of production, usually using the means for further refining thick lithium, but this approach complex process, cost mistake
It is high.Using as disclosed in CN102992358 patents is precipitated and filtered filter residue method and obtain high-purity lithium salts product, but precipitates
The method technique of filtering is relative complex, and cost is higher.
Therefore seek high-purity lithium salts preparation technology that a kind of technique is simple, cost is low has weight for development lithium energy metal
The impetus wanted.
The content of the invention
It is an object of the present invention to provide the process that a kind of extraction from high-Mg Li-contained bittern prepares high-purity lithium salts, solution
The technical problem that certainly high-purity lithium salts extraction and preparation technique is complicated in the prior art, cost is high.
The present invention is as follows to solve the technical scheme that above-mentioned technical problem is used：
The invention discloses the process that a kind of extraction from high-Mg Li-contained bittern prepares high-purity lithium salts, this method includes
Following steps：
Extraction step, FeCl is added into high-Mg Li-contained bittern3, extractant tributyl phosphate (TBP) and diluent, carry out
The extraction system that load lithium is obtained by extraction of lithium (contains LiFeCl4* 2TBP and a small amount of Mg (FeCl4)2*2TBP)；Extract in the step
It is 30~100% to take percents by volume of the agent TBP in extraction system；The diluent is organic solvent, preferably sulfonated coal
Oil, aviation gasoline or aromatic hydrocarbon；
Exchange step, is mixed using Aqueous Lithium Salts with the extraction system of foregoing load lithium, to remove the extraction of load lithium
Other impurities in system, obtain loading the extraction system of high purity lithium；The principle of exchange reaction is in the step：
2Li++Mg(FeCl4)2* 2TBP=2LiFeCl4*2TBP+Mg2+
The aqueous phase solution obtained in the exchange step can be further applicable in extraction step, reenter lithium therein
Extraction system；
Stripping steps, the extraction system of foregoing load high purity lithium is stripped with acid solution, obtained containing high-purity lithium salts
Aqueous phase, aqueous phase obtains high-purity lithium salts after being evaporated；The acid solution is hydrochloric acid solution, sulfuric acid solution, salpeter solution or phosphoric acid solution.
Further, also include after the stripping steps：Wash the organic phase after sour step, foregoing stripping steps using go from
Sub- water carries out washing acid, obtains washing extraction system and aqueous phase after acid.
This is washed the aqueous phase obtained in sour step and can be further applicable in exchange step or stripping steps.
Further, the lithium salts that Aqueous Lithium Salts are used in the exchange step is in lithium chloride, lithium sulfate or lithium nitrate
One or more.Lithium concentration in the Aqueous Lithium Salts is 0.05-10mol/L, the Aqueous Lithium Salts and extraction system
Volume ratio be 0.01-1, the exchange reaction time be 0.2-15 minutes.
Further, added in the Aqueous Lithium Salts in hydrochloric acid, the Aqueous Lithium Salts add hydrochloric acid concentration be
0-12mol/L。
It is further preferred that lithium concentration is 0.1-5mol/L, the Aqueous Lithium Salts and extraction in the Aqueous Lithium Salts
The volume ratio of system is 0.02-0.5, and the exchange reaction time is 0.5-5 minutes.
Further, the extraction step and stripping steps use membrane extraction equipment or tower；The exchange step
Using film switching equipment.
Compared with prior art, beneficial effects of the present invention are as follows：
1, change for the process extracted in the prior art using TBP extractants to high-Mg Li-contained bittern
Enter, increase exchange step between extraction step and stripping steps so that other a small amount of impurity in extraction system are by exchanging
Reaction is got rid of, so that the lithium salts product purity finally given is improved, the lithium salts obtained by the process of the present invention
Purity is up to more than 95%.
2, the present invention is to increase a step in the extraction process of lithium salts to purify final lithium salts product, this technique
Further the refined operating procedure purified is easier, save into relative to thick lithium product is first prepared in the prior art for method
This.
Embodiment
If the high-Mg Li-contained bittern used in specific embodiment contains boron ion, it is necessary to carry out boron lithium separation in advance.Such as
Fruit contains other impurities, can first carry out pretreatment and remove partial impurities.
Embodiment 1
Adding bittern containing lithium using separatory funnel, (Mg/Li=15 mol ratios, hydrionic concentration is 0.01), dissolving is certain
The iron chloride of amount contains in lithium bittern to this (iron chloride concentration in bittern is 0.9 mole every liter).Separatory funnel cascade extraction, should
Bittern is with extract with volume ratio 1:6 carry out 2 stage countercurrent hybrid extractions, and (extract is extractant TBP and diluent sulfonation
50%) mixed liquor of kerosene, wherein extractant TBP percent by volume is.Organic phase (purity 71% of lithium) and 1 after extraction
Mole every liter of lithium chloride solution mixing, swaps reaction, wherein being compared to (organic phase and the volume ratio of lithium chloride solution)
10:1, the aqueous-phase reflux after exchange is added in bittern, and the organic phase (purity of lithium is 95.8%) after exchange carries out 2 with hydrochloric acid
Level back extraction, the aqueous phase after back extraction is evaporated as product (purity 95.8% of lithium), and the organic phase after back extraction is carried out using deionized water
Acid is washed, volume ratio is 10:1, wash the aqueous phase after acid be applied to exchange the aqueous solution in mixed with lithium salt solution.
If above-described embodiment is according to process of the prior art, the organic phase after extraction is walked without exchange
Suddenly, stripping steps are directly entered, the aqueous phase after back extraction is evaporated obtained product, and the purity of its lithium is 71%.
Embodiment 2
Adding bittern containing lithium using separatory funnel, (Mg/Li=15 mol ratios, hydrionic concentration is 0.01), dissolving is certain
The iron chloride of amount contains in lithium bittern to this (iron chloride concentration in bittern is 0.9 mole every liter).Carried out using mixer-settler
Experiment, the bittern is with extract with volume ratio 1:4 carry out 3 stage countercurrent hybrid extractions, and (extract is extractant TBP and dilution
75%) mixed liquor of agent sulfonated kerosene, wherein extractant TBP percent by volume is.Organic phase (the purity of lithium after extraction
79%) lithium chloride solution with 3 moles every liter is mixed, and swaps reaction, wherein compared to the (body of organic phase and lithium chloride solution
Product ratio) it is 15:1, the aqueous-phase reflux after exchange is added in bittern, organic phase (purity of lithium is 97%) and hydrochloric acid after exchange
Carry out 2 stage countercurrent back extraction, the aqueous phase after back extraction is evaporated as product (purity 97% of lithium), and the organic phase after back extraction uses deionization
Water carries out washing acid, and volume ratio is 20:1, wash the aqueous phase after acid and be applied in stripping steps with being stripped after mixed in hydrochloric acid.
If the embodiment is according to process of the prior art, the organic phase after extraction without exchange step,
Stripping steps are directly entered, the aqueous phase after back extraction is evaporated obtained product, and the purity of its lithium is 79%.
Embodiment 3
In certain salt lake bittern containing lithium, (Mg/Li=19 mol ratios, hydrionic concentration is 0.01) middle a certain amount of chlorine of dissolving
Change iron (iron chloride concentration in bittern containing lithium is 0.75 mole every liter).Carried out using mixer-settler, the bittern and extract
With volume ratio 1:43 stage countercurrent hybrid extractions of progress (extract is the mixed liquor of extractant TBP and diluent sulfonated kerosene,
Wherein 75%) extractant TBP percent by volume is.Organic phase (purity 77% of lithium) after extraction is using 3 moles every liter
The mixed solution of lithium chloride and 1.8 moles every liter of hydrochloric acid swaps reaction, wherein compared to (organic phase is mixed with lithium chloride hydrochloric acid
Close the volume ratio of solution) it is 25:1 carries out two-stage countercurrent exchange, and the aqueous-phase reflux after exchange is added in bittern, having after exchange
Machine phase (purity of lithium is 96.4%) carries out 4 stage countercurrent back extraction with hydrochloric acid, and the aqueous phase after back extraction is evaporated as the product (purity of lithium
96.4%), the organic phase after back extraction carries out washing acid using deionized water, and volume ratio is 20:1, the aqueous phase washed after acid is applied to instead
Extract in step with being stripped after mixed in hydrochloric acid.
If the embodiment is according to process of the prior art, the organic phase after extraction without exchange step,
Stripping steps are directly entered, the aqueous phase after back extraction is evaporated obtained product, and the purity of its lithium is 77%.
Embodiment 4
In certain salt lake bittern containing lithium, (Mg/Li=19 mol ratios, hydrionic concentration is 0.01) middle a certain amount of chlorine of dissolving
Change iron (iron chloride concentration in bittern is 0.75 mole every liter).Carried out using mixer-settler, the bittern is with extract with body
Product compares 1:43 stage countercurrent hybrid extractions of progress (extract is the mixed liquor of extractant TBP and diluent sulfonated kerosene, wherein
75%) extractant TBP percent by volume is.Organic phase (purity 77% of lithium) after extraction uses 3 moles every liter of chlorination
The mixed solution of lithium and 3 moles every liter of hydrochloric acid swaps reaction, wherein compared to (organic phase and lithium chloride hydrochloric acid mixed solution
Volume ratio) be 20:1 carries out 3 stage countercurrent exchanges, and the aqueous-phase reflux after exchange is added in bittern, the organic phase (lithium after exchange
Purity 98%) to carry out 5 stage countercurrent back extraction with hydrochloric acid, the aqueous phase after back extraction is evaporated as product (purity 98% of lithium), back extraction
Organic phase afterwards carries out washing acid using deionized water, and volume ratio is 20:1, the aqueous phase washed after acid is applied in stripping steps and salt
It is stripped after acid mixing.
If the embodiment is according to process of the prior art, the organic phase after extraction without exchange step,
Stripping steps are directly entered, the aqueous phase after back extraction is evaporated obtained product, and the purity of its lithium is 77%.
Embodiment 5
In certain salt lake bittern containing lithium, (Mg/Li=19 mol ratios, hydrionic concentration is 0.01) middle a certain amount of chlorine of dissolving
Change iron (iron chloride concentration in bittern is 0.75 mole every liter).The step uses membrane extraction method, using 4 cun of membrane modules, the halogen
Water is with extract with volume ratio 1:4 carry out 11 stage countercurrent hybrid extractions, and (extract is extractant TBP and diluent sulfonated coal
The mixed liquor of oil, wherein extractant TBP percent by volume is 75%), the organic phase (purity 70% of lithium) after extraction use 3
Mole every liter of lithium chloride and the mixed solution of 3 moles every liter of hydrochloric acid swap reaction, wherein compared to (organic phase and chlorination
The volume ratio of lithium hydrochloric acid mixed solution) it is 20:1 carries out counterflow exchange, and the aqueous-phase reflux after exchange is added in bittern, after exchange
Organic phase (purity of lithium be 95.1%) and hydrochloric acid carry out 14 stage countercurrent back extraction, the aqueous phase after back extraction be evaporated for product (lithium
Purity 95.1%), the organic phase after back extraction carries out washing acid using deionized water, and volume ratio is 20:1, the aqueous phase application washed after acid
Into stripping steps with being stripped after mixed in hydrochloric acid.
If the embodiment is according to process of the prior art, the organic phase after extraction without exchange step,
Stripping steps are directly entered, the aqueous phase after back extraction is evaporated obtained product, and the purity of its lithium is 70%.
The part preferred embodiment of the present invention is above are only, the present invention is not limited in the content of embodiment.For ability
For technical staff in domain, can there are various change and change in the concept of technical solution of the present invention, that is made appoints
What changes and changed, within the scope of the present invention.
Claims (8)
1. a kind of extract the process for preparing high-purity lithium salts from high-Mg Li-contained bittern, this method comprises the following steps：
Extraction step, FeCl is added into high-Mg Li-contained bittern3, extractant tributyl phosphate and diluent, carry out extracting for lithium
To the extraction system of load lithium；Extractant tributyl phosphate in the extraction step is in the percent by volume of extraction system
30-100%；
Exchange step, is mixed using Aqueous Lithium Salts with the extraction system of foregoing load lithium, to remove the extraction system of load lithium
In other impurities, obtain load high purity lithium extraction system；The condition of the exchange step is：Lithium in the Aqueous Lithium Salts
Concentration is 0.05-10mol/L, and the volume ratio of the Aqueous Lithium Salts and extraction system is 0.01-1, the exchange reaction time
For 0.2-15 minutes；The lithium salts that Aqueous Lithium Salts in the exchange step are used is in lithium chloride, lithium sulfate or lithium nitrate
It is one or more of；
Stripping steps, the extraction system of foregoing load high purity lithium is stripped with acid solution, the aqueous phase containing high-purity lithium salts is obtained,
Aqueous phase obtains high-purity lithium salts after being evaporated.
2. the process for preparing high-purity lithium salts is extracted from high-Mg Li-contained bittern as claimed in claim 1, it is characterised in that
Also include after the stripping steps：
The organic phase washed after sour step, foregoing stripping steps carries out washing acid using deionized water, obtains washing the extraction system after acid
And aqueous phase.
3. the process for preparing high-purity lithium salts is extracted from high-Mg Li-contained bittern as claimed in claim 1, it is characterised in that：
The aqueous phase solution obtained in the exchange step is further applicable in the extraction step, lithium therein is reentered extraction
System.
4. the process for preparing high-purity lithium salts is extracted from high-Mg Li-contained bittern as claimed in claim 1, it is characterised in that
The condition of the exchange step is：Lithium concentration is 0.1-5mol/L, the Aqueous Lithium Salts and extraction in the Aqueous Lithium Salts
The volume ratio of system is 0.02-0.5, and the exchange reaction time is 0.5-5 minutes.
5. the process for preparing high-purity lithium salts is extracted from high-Mg Li-contained bittern as claimed in claim 1, it is characterised in that：
The aqueous phase obtained in sour step of washing is further applicable in the exchange step or stripping steps.
6. the process for preparing high-purity lithium salts is extracted from high-Mg Li-contained bittern as claimed in claim 1, it is characterised in that：
Diluent in the extraction step is sulfonated kerosene, aviation gasoline or aromatic hydrocarbon.
7. the process for preparing high-purity lithium salts is extracted from high-Mg Li-contained bittern as claimed in claim 1, it is characterised in that：
The extraction step and stripping steps use membrane extraction equipment or tower；The exchange step uses film switching equipment.
8. the process for preparing high-purity lithium salts is extracted from high-Mg Li-contained bittern as claimed in claim 1, it is characterised in that：
Hydrochloric acid is added in Aqueous Lithium Salts in the exchange step.
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| CN107253732B (en) * | 2016-07-13 | 2019-06-11 | 合肥通用机械研究院有限公司 | A kind of production technology of industrial grade methanol |
| CN107119196A (en) * | 2017-03-21 | 2017-09-01 | 中国科学院上海高等研究院 | The method that industrial grade methanol is prepared from bittern containing lithium |
| CN108149030B (en) * | 2017-11-15 | 2020-05-05 | 青海柴达木兴华锂盐有限公司 | Efficient integrated lithium ion extraction equipment and extraction process |
| CN107904416B (en) * | 2017-11-16 | 2019-11-26 | 中国科学院青岛生物能源与过程研究所 | A method of it is big to extract compared to bubbling oil film from salt lake original brine enriching low-concentration lithium |
| CN111793755A (en) * | 2020-08-03 | 2020-10-20 | 苏州增华新能源科技有限公司 | Organic phase online purification method and device in lithium extraction process of salt lake and application |
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