CN109179457A - The extracting method of lithium in a kind of waste slag of electrolytic aluminium - Google Patents
The extracting method of lithium in a kind of waste slag of electrolytic aluminium Download PDFInfo
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- CN109179457A CN109179457A CN201811200798.9A CN201811200798A CN109179457A CN 109179457 A CN109179457 A CN 109179457A CN 201811200798 A CN201811200798 A CN 201811200798A CN 109179457 A CN109179457 A CN 109179457A
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- CN
- China
- Prior art keywords
- filtrate
- lithium
- waste slag
- obtains
- electrolytic aluminium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/06—Preparation of sulfates by double decomposition
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
Abstract
The invention discloses a kind of extracting methods of lithium in waste slag of electrolytic aluminium, include the following steps: (1) for waste slag of electrolytic aluminium and strong sulfuric acid response, reaction obtains mixture A；(2) it is filtered after mixture A being dissolved in water, obtains liquor B, calcium oxide is slowly added in liquor B, acquired solution is filtered, obtain filter residue C and filtrate D；(3) filtrate D is heated and is concentrated by evaporation, and filtrate is further concentrated by evaporation after filtering, obtains filtrate E, and filtrate E maintains heated condition；(4) saturated sodium carbonate solution in filtrate E, obtains suspension F, and suspension F is filtered, filter cake is obtained, and is washed, is dried to filter cake, lithium carbonate product can be obtained.For this method using the waste residue of Aluminium Industry as raw material, raw material sources are wide, and cost is lower than lithium ore raw material, and extracts and be easy, high income, other low in raw material price used in extracting method, at low cost, gained byproduct can also recycle.
Description
Technical field
The present invention relates to lithium extractive technique fields, and in particular to the extracting method of lithium in a kind of waste slag of electrolytic aluminium.
Background technique
China is a lithium resource country abundant, but the development and utilization of lithium resource always exists certain difficulty,
Difficult, the problem of the problems such as withdrawal ratio is not high and some lithium resources are not utilized is extracted including lithium resource.With
The development of new energy field, the demand to lithium ion battery quickly promoted, which results in the prices of lithium raw material rapidly to go up.
Currently, China extracts, lithium raw material is mainly extracted by lithium ore and brine extracts.And in the northern area of China, aluminium ore
A certain amount of lithium is associated in stone resource.And in Aluminium Industry, the auxiliary agent as electrolytic process such as lithium fluoride is also added.
These lithiums are enriched in waste slag of electrolytic aluminium, and content can achieve 1-5%.And these lithiums are not utilized adequately, Hen Duoshi
Time is directly discharged in slag library.The waste slag of electrolytic aluminium that China generates every year is no less than 20,000 tons, can extract here close
Kiloton lithium carbonate can effectively alleviate demand of China's battery industry to lithium resource.
In existing technology, two patents of CN10054161C and CN102079534B disclose two kinds and utilize electrolytic aluminium
The method that waste residue prepares ice crystal, method, which is based on the concentrated sulfuric acid, reacts with fluoride in waste residue and produces hydrogen fluoride and hydroxide
Then aluminium prepares ice crystal.The above method utilizes waste residue, improves resource utilization, and reduces waste sludge discharge.But
It is not fully utilize to being worth higher lithium in waste residue.
CN105293536A discloses a kind of method that waste slag of electrolytic aluminium extracts lithium.Method is waste slag of electrolytic aluminium and 1-3
Times weight the concentrated sulfuric acid 200-400 DEG C reaction 5-12 hours, obtain mixture A；Mixture A is added into the A that filters to get filtrate after water extraction
With filter residue A；Filtrate A addition sodium carbonate is subjected to Basic fluxing raction under the conditions of 20~40 DEG C, after filter to get filtrate B and filter residue B；It will
Filter residue B adds water slurry is made to add lime to carry out causticizing reaction, after filter to get filtrate C and filter residue C；It will be in step 4) liquor C
It is passed through CO2Carry out carburizing reagent, after be filtered, washed, dry to get.This method can effectively extract lithium carbonate from waste residue,
Several byproducts can complete the preparation of ice crystal simultaneously.But this method extraction step is excessive, and first uses sodium carbonate, after
Using lime, lead to need in feed liquid that sodium carbonate largely is added, Na ion concentration is excessively high, and solution can not effectively be concentrated, and reduces
The recovery rate of lithium carbonate.The use of carbon dioxide is increased simultaneously, and needs to improve equipment throwing using high pressure reactor
Enter cost and cost of material.Causticizing reaction generates a large amount of lye, makes troubles to subsequent liquid waste processing.And currently without
See, using less extraction step, the report of the extraction lithium method of the reaction condition of milder and cheaper raw material.
Summary of the invention
The invention proposes a kind of extracting method of lithium in waste slag of electrolytic aluminium, using less step, more cheap raw material,
The reaction condition of milder extracts elemental lithium from Aluminium Industry waste residue, finally obtains lithium carbonate product.
Realize the technical scheme is that in a kind of waste slag of electrolytic aluminium lithium extracting method, comprise the following steps:
(1) by waste slag of electrolytic aluminium and strong sulfuric acid response, reaction temperature is 100-300 DEG C, and reaction obtains mixture A；
(2) it is filtered after mixture A being dissolved in water, obtains liquor B, calcium oxide is slowly added in liquor B, until solution ph
Reach 7-7.5, acquired solution is filtered, obtains filter residue C and filtrate D；
(3) filtrate D is heated and is concentrated by evaporation, and pH value is increased to 10-11, and filtrate is further concentrated by evaporation after filtering, obtains filtrate
E, filtrate E maintain heated condition；
(4) saturated sodium carbonate solution in filtrate E, obtains suspension F, and suspension F is filtered, filter cake is obtained, and carries out to filter cake
Washing, drying, can be obtained lithium carbonate product.
The mass ratio of waste slag of electrolytic aluminium and the concentrated sulfuric acid is 1:(1.5-2.5 in the step (1)).
It is 60-99 DEG C that filtrate D, which is concentrated by evaporation temperature, in the step (3).
The temperature of saturated sodium carbonate solution is 60-99 DEG C in the step (4).
The mass ratio of filtrate E and saturated sodium carbonate solution is 1:(0.2-2 in the step (4)).
Chemical equation of the present invention are as follows:
LiF+H2SO4→LiHSO4+HF↑
NaF+H2SO4→NaHSO4+HF↑
2AlF3+3H2SO4→Al2(SO4)3+6HF↑
CaO+H2O→Ca(OH)2↓
Ca(OH)2+H2SO4→CaSO4
3Ca(OH)2+ Al2(SO4)3→2Al(OH)3↓+3CaSO4
Li2SO4+Na2CO3→Li2CO3↓+Na2SO4
The beneficial effects of the present invention are:
(1) process flow steps that the present invention uses are less, can effectively improve waste slag of electrolytic aluminium and extract the efficiency of lithium, and drop
The low cost for extracting lithium；
(2) raw material that uses of the present invention, other than waste slag of electrolytic aluminium, the respectively concentrated sulfuric acid, calcium oxide, sodium carbonate and water are used
Raw material sources are extensive, cheap；
(3) in step of the present invention (2), first using in calcium oxide and excessive sulfuric acid, low raw-material cost, and
Excessive sodium ion will not be introduced in feed liquid, the calcium sulfate of generation is also insoluble matter, can be by sulfate radical a large amount of in feed liquid
Removal, the step are significantly better than existing neutralization technology；
(4) it in step of the present invention (3), is slowly increased by evaporating concentration process, further controlling pH, it can
So that the aluminium hydroxide in feed liquid is sufficiently precipitated, the generation of lithium metaaluminate is avoided, reduces the pollution in product；
(5) in step of the present invention (4), using saturated sodium carbonate solution, the use of high-temperature high-pressure apparatus is avoided,
Not only cost of material is low, and equipment investment is also smaller；
(6) reaction condition of the present invention is mild, is not necessarily to high temperature high pressure process, considerably reduces the throwing in production equipment
Enter, and then reduces the cost for extracting lithium；
(7) in process flow of the present invention, utilization that byproduct can also more economically be changed；
(8) process flow of the present invention does not generate acid or alkaline waste water discharge, work by the utilization to byproduct
Skill process is more environmentally protective；
(9) method that the waste residue of the present invention using Aluminium Industry mentions lithium, improves resource utilization, generated by-product
Product are available, do not generate the waste water and gas of pollution, environmentally friendly；
(10) method that the waste residue of the present invention using Aluminium Industry mentions lithium, step is few, low in raw material price, reaction condition
Mildly, byproduct can make full use of, no pollutant treatment emission problem, economic value with higher and environmental value.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the process flow diagram that waste slag of electrolytic aluminium of the present invention extracts lithium method.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Those of ordinary skill in the art's every other embodiment obtained under that premise of not paying creative labor, belongs to this hair
The range of bright protection.
Embodiment 1
The extracting method of lithium in a kind of waste slag of electrolytic aluminium, steps are as follows:
The waste slag of electrolytic aluminium 50kg for having been removed carbon and iron is reacted with concentrated sulfuric acid 100kg, reaction temperature is 250 DEG C, and reaction 6 is small
Shi Hou obtains mixture A, while the HF generated using water absorbing reaction, gained HF aqueous solution can be used for preparing ice crystal；
It is filtered after adding 500kg water to dissolve mixture A, obtains liquor B, calcium oxide is slowly added in liquor B, until pH value of solution
Value reaches 7.5, and acquired solution is filtered, and obtains filter residue C and filtrate D, and gained filter residue C main component is aluminium hydroxide and sulfuric acid
Calcium, aluminium hydroxide can be used for preparing the byproducts such as ice crystal, and calcium sulfate can be used for preparing the byproducts such as land plaster.
Filtrate D is heated to 90 DEG C of evaporation and concentration, concentration process pH value is increased to 10.5 stoppings, the hydrogen that filtering removal is precipitated
Aluminium oxide then proceedes to evaporative concn filtrate to loss of weight to 80kg, obtains filtrate E, filtrate E maintains 90 DEG C.
90 DEG C of saturated sodium carbonate solution 80kg is added in 90 DEG C of filtrate E, suspension F is obtained, by suspension F mistake
Filter, obtains filter cake, is washed, dried to filter cake, lithium carbonate product can be obtained.Filtrate is used to prepare sodium sulphate, ice crystal
Equal byproducts can also flow back and continue processing extraction residual lithium.
In conclusion the method in the present invention can adequately utilize the waste residue of Aluminium Industry.Meanwhile the method
Step is few, and method is simple, low in raw material price.
Embodiment 2
The extracting method of lithium in a kind of waste slag of electrolytic aluminium, steps are as follows:
The waste slag of electrolytic aluminium 50kg for having been removed carbon and iron is reacted with concentrated sulfuric acid 125kg, reaction temperature is 100 DEG C, reaction 20
After hour, mixture A is obtained, while the HF generated using water absorbing reaction, gained HF aqueous solution can be used for preparing ice crystal；
It is filtered after adding 500kg water to dissolve mixture A, obtains liquor B, calcium oxide is slowly added in liquor B, until pH value of solution
Value reaches 7, and acquired solution is filtered, and obtains filter residue C and filtrate D, and gained filter residue C main component is aluminium hydroxide and calcium sulfate,
Aluminium hydroxide can be used for preparing the byproducts such as ice crystal, and calcium sulfate can be used for preparing the byproducts such as land plaster.
Filtrate D is heated to 60 DEG C of evaporation and concentration, concentration process pH value is increased to 10 stoppings, the hydrogen-oxygen that filtering removal is precipitated
Change aluminium, then proceedes to evaporative concn filtrate to loss of weight to 80kg, obtain filtrate E, filtrate E maintains 60 DEG C.
60 DEG C of saturated sodium carbonate solution 16kg is added in 60 DEG C of filtrate E, suspension F is obtained, by suspension F mistake
Filter, obtains filter cake, is washed, dried to filter cake, lithium carbonate product can be obtained.Filtrate is used to prepare sodium sulphate, ice crystal
Equal byproducts can also flow back and continue processing extraction residual lithium.
Embodiment 3
The extracting method of lithium in a kind of waste slag of electrolytic aluminium, steps are as follows:
The waste slag of electrolytic aluminium 50kg for having been removed carbon and iron is reacted with concentrated sulfuric acid 75kg, reaction temperature is 300 DEG C, and reaction 6 is small
Shi Hou obtains mixture A, while the HF generated using water absorbing reaction, gained HF aqueous solution can be used for preparing ice crystal；
It is filtered after adding 500kg water to dissolve mixture A, obtains liquor B, calcium oxide is slowly added in liquor B, until pH value of solution
Value reaches 7.5, and acquired solution is filtered, and obtains filter residue C and filtrate D, and gained filter residue C main component is aluminium hydroxide and sulfuric acid
Calcium, aluminium hydroxide can be used for preparing the byproducts such as ice crystal, and calcium sulfate can be used for preparing the byproducts such as land plaster.
Filtrate D is heated to 99 DEG C of evaporation and concentration, concentration process pH value is increased to 11 stoppings, the hydrogen-oxygen that filtering removal is precipitated
Change aluminium, then proceedes to evaporative concn filtrate to loss of weight to 80kg, obtain filtrate E, filtrate E maintains 99 DEG C.
99 DEG C of saturated sodium carbonate solution 160kg is added in 99 DEG C of filtrate E, suspension F is obtained, by suspension F mistake
Filter, obtains filter cake, is washed, dried to filter cake, lithium carbonate product can be obtained.Filtrate is used to prepare sodium sulphate, ice crystal
Equal byproducts can also flow back and continue processing extraction residual lithium.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (5)
1. the extracting method of lithium in a kind of waste slag of electrolytic aluminium, characterized by comprising the steps of:
(1) by waste slag of electrolytic aluminium and strong sulfuric acid response, reaction temperature is 100-300 DEG C, and reaction obtains mixture A；
(2) it is filtered after mixture A being dissolved in water, obtains liquor B, calcium oxide is slowly added in liquor B, until solution ph
Reach 7-7.5, acquired solution is filtered, obtains filter residue C and filtrate D；
(3) filtrate D is heated and is concentrated by evaporation, and pH value is increased to 10-11, and filtrate is further concentrated by evaporation after filtering, obtains filtrate
E, filtrate E maintain heated condition；
(4) saturated sodium carbonate solution in filtrate E, obtains suspension F, and suspension F is filtered, filter cake is obtained, and carries out to filter cake
Washing, drying, can be obtained lithium carbonate product.
2. the extracting method of lithium in waste slag of electrolytic aluminium according to claim 1, it is characterised in that: electric in the step (1)
The mass ratio for solving waste slag of aluminum and the concentrated sulfuric acid is 1:(1.5-2.5).
3. the extracting method of lithium in waste slag of electrolytic aluminium according to claim 1, it is characterised in that: filter in the step (3)
It is 60-99 DEG C that liquid D, which is concentrated by evaporation temperature,.
4. the extracting method of lithium in waste slag of electrolytic aluminium according to claim 1, it is characterised in that: the step (4) is embezzled
Temperature with sodium carbonate liquor is 60-99 DEG C.
5. the extracting method of lithium in waste slag of electrolytic aluminium according to claim 1, it is characterised in that: filter in the step (4)
The mass ratio of liquid E and saturated sodium carbonate solution is 1:(0.2-2).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811200798.9A CN109179457B (en) | 2018-10-16 | 2018-10-16 | Method for extracting lithium from electrolytic aluminum waste residues |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811200798.9A CN109179457B (en) | 2018-10-16 | 2018-10-16 | Method for extracting lithium from electrolytic aluminum waste residues |
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| CN109179457A true CN109179457A (en) | 2019-01-11 |
| CN109179457B CN109179457B (en) | 2021-03-02 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109930174A (en) * | 2019-03-01 | 2019-06-25 | 郑州经纬科技实业有限公司 | The method that aluminium electrolyte takes off lithium purification and recycling lithium |
| CN109972175A (en) * | 2019-04-28 | 2019-07-05 | 沈阳北冶冶金科技有限公司 | A kind of separation and recovery method of the difficult electrolyte of aluminium electroloysis |
| CN111892022A (en) * | 2020-06-29 | 2020-11-06 | 中国铝业股份有限公司 | Method for utilizing fluorine-containing waste and surplus electrolyte resources in aluminum electrolysis |
| CN115557520A (en) * | 2022-08-29 | 2023-01-03 | 昆明理工大学 | Method for recovering lithium from lithium silicate waste residue |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102041380A (en) * | 2010-11-17 | 2011-05-04 | 山东瑞福锂业有限公司 | Production process for extracting lithium from ore with low-temperature method |
| CN105293536A (en) * | 2015-12-01 | 2016-02-03 | 多氟多化工股份有限公司 | Method of extracting lithium from electrolytic aluminium waste residues |
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2018
- 2018-10-16 CN CN201811200798.9A patent/CN109179457B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102041380A (en) * | 2010-11-17 | 2011-05-04 | 山东瑞福锂业有限公司 | Production process for extracting lithium from ore with low-temperature method |
| CN105293536A (en) * | 2015-12-01 | 2016-02-03 | 多氟多化工股份有限公司 | Method of extracting lithium from electrolytic aluminium waste residues |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109930174A (en) * | 2019-03-01 | 2019-06-25 | 郑州经纬科技实业有限公司 | The method that aluminium electrolyte takes off lithium purification and recycling lithium |
| CN109930174B (en) * | 2019-03-01 | 2020-07-14 | 郑州经纬科技实业有限公司 | Method for lithium removal, purification and lithium recovery of aluminum electrolyte |
| CN109972175A (en) * | 2019-04-28 | 2019-07-05 | 沈阳北冶冶金科技有限公司 | A kind of separation and recovery method of the difficult electrolyte of aluminium electroloysis |
| CN111892022A (en) * | 2020-06-29 | 2020-11-06 | 中国铝业股份有限公司 | Method for utilizing fluorine-containing waste and surplus electrolyte resources in aluminum electrolysis |
| CN115557520A (en) * | 2022-08-29 | 2023-01-03 | 昆明理工大学 | Method for recovering lithium from lithium silicate waste residue |
| CN115557520B (en) * | 2022-08-29 | 2023-11-10 | 昆明理工大学 | Method for recycling lithium from lithium silicate waste residues |
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Effective date of registration: 20230103 Address after: 318000 He Fang Cun, Shifeng Street, Tiantai County, Taizhou City, Zhejiang Province (in Zhejiang Fengruichen Fire Equipment Co., Ltd.) Patentee after: Taizhou shanneng Technology Co.,Ltd. Address before: 451191 Xianghe Road, Longhu Town, Zhengzhou City, Henan Province Patentee before: HENAN INSTITUTE OF ENGINEERING |
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