CN107188205A - The technique that a kind of acidization extracts lithium sulfate from amblygonite - Google Patents
The technique that a kind of acidization extracts lithium sulfate from amblygonite Download PDFInfo
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- CN107188205A CN107188205A CN201710577804.1A CN201710577804A CN107188205A CN 107188205 A CN107188205 A CN 107188205A CN 201710577804 A CN201710577804 A CN 201710577804A CN 107188205 A CN107188205 A CN 107188205A
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- amblygonite
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- lithium sulfate
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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
- C01D15/06—Sulfates; Sulfites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
Research and development technology field is extracted the present invention relates to the lithium of amblygonite, more particularly to a kind of acidization extracts the technique of lithium sulfate from amblygonite, adopts the following technical scheme that：The technique that a kind of acidization extracts lithium sulfate from amblygonite, it is characterised in that：Comprise the following steps：(1) raw material is levigate：Raw material in amblygonite is carried out levigate；(2) dispensing：Amblygonite of the step (1) after levigate and the concentrated sulfuric acid are mixed；(3) it is calcined：Step (2) mixed material is calcined；(4) size mixing leaching：Step (3) clinker is placed in reactor and adds water progress heating stirring；(5) purification and impurity removal：To removing the impurity such as aluminium or calcium in the solution of leaching in step (4)；(6) solution after the completion of being reacted in step (5) is evaporated concentration, the advantage of the invention is that：The technique that lithium sulfate is extracted there is provided a kind of brand-new amblygonite, the reliability and economy of technical scheme is high.
Description
Technical field：
Research and development technology field is extracted the present invention relates to the lithium of amblygonite, more particularly to a kind of acidization is from amblygonite
The technique for extracting lithium sulfate.
Background technology：The industrial mineral of lithium mainly has following several on the earth：
The industrial mineral of the lithium of table 1
Wherein the most famous with spodumene, because spodumene is big into ore deposit scale, composition is simple, carries lithium technical maturity, is mesh
It is preceding to use most lithium minerals.And although lepidolite is also into ore deposit scale than larger, but due to its complicated component, put forward lithium technique
Complexity, thus it is less for carrying lithium, it is mainly used in glass ceramics industry.Zinnwaldite, amblygonite and petalite then due to
Distribution is rare, into ore deposit small scale, does not there is the report of commercial Application so far, and on putting forward lithium process then to this three kinds of mineral
More not disclosed report.
Our amblygonites to be studied are a kind of highest lithium minerals of amount containing lithium, and its minal oxide containing lithium amount is
10.1%, but it is not common in nature, and it is also very little scale to be occasionally found, not as the value of commercial mining.But it is existing
Then there is certain scale in this amblygonite ore deposit found in Africa, the value for possessing commercial mining.
Amblygonite is often the shaft-like such as irregular block and near, and color is grey, yellowish-white, green white etc., a certain amount of due to having
Other paragenous minerals, it is actual to contain Li2O8~9.5%, is the industrial mineral of highest containing lithium, originates in granite peamatite, sometimes
Also see in greisen and high quartz arteries and veins.Amblygonite is a kind of fluorophosphate containing lithium, aluminium, originates in granite peamatite, with
Spodumene, tourmaline, lepidolite and apatite symbiosis, are mainly used as extracting the resource of lithium.
The composition of amblygonite is as follows：%
Table 2
The content of the invention：
An object of the present invention is to provide the technique that a kind of acidization extracts lithium sulfate from amblygonite, especially
The technique that a kind of initiative acidization extracts lithium sulfate from amblygonite.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：A kind of acidization extracts sulfuric acid from amblygonite
The technique of lithium, it is characterised in that：Comprise the following steps：
(1) raw material is levigate：Raw material in amblygonite is carried out levigate；
(2) dispensing：By amblygonite of the step (1) after levigate and the concentrated sulfuric acid using weight ratio as 1:0.25~0.37 is carried out
Mixing；
(3) it is calcined：Step (2) mixed material is calcined；
(4) size mixing leaching：Step (3) clinker is placed in reactor and adds water progress heating stirring, obtain the leaching containing lithium
Go out liquid；
(5) purification and impurity removal：To removing the impurity such as aluminium or calcium in the solution of leaching in step (4)；
(6) it is concentrated by evaporation：Solution after the completion of being reacted in step (5) is evaporated concentration, obtains lithium sulfate solution
It is levigate to the raw material in amblygonite to 100~200 mesh in step (1) as preferred.
As preferred, temperature control is calcined at 500 DEG C~800 DEG C in step (3), and the constant temperature calcining time is 20
~60 minutes.
It is after material cooling that clinker is levigate to 100~200 mesh after step (4) medium roasting as preferred.
As preferred, in step (4), in step (4)) middle leaching liquid-solid ratio 3~5：1.
It is used as preferred, extraction temperature room temperature (about 20 DEG C), 20~150 DEG C, constant temperature extraction time 0.5~2 hour.
Further, in step (5), the leachate that step (4) is obtained adjusts PH to 7~8 with solid sodium hydroxide, plus
Hot solution is to 80~90 DEG C and isothermal reaction 10~15 minutes；To neutralize the acid in solution and remove the impurity such as the aluminium in solution.
Further, in step (5), to neutralize the acid in solution and remove after the impurity such as the aluminium in solution, by aluminium
Filtered after the completion of reaction；Then repeated hydrogenation sodium oxide molybdena adjusts PH to 14, to remove magnesium in solution and the impurity such as partial calcium.
Further, it is heavy in the saturated solution of sodium carbonate of addition amount of calculation excessive 10% or production in step (5)
Heated solution is filtered to 80~90 DEG C of simultaneously isothermal reaction 10~15 minutes, filterings after the completion of question response in lithium mother liquor, course of reaction
Clear liquid afterwards adjusts PH to 6.5~7.5 with sulfuric acid again, and calcium impurities therein are removed with depth.
As preferred, in step (6), when aoxidizing lithium concentration when being concentrated in solution for 45g/l or so, stop adding
Heat.
The advantage of the invention is that：
1 there is provided the technique that a kind of initiative amblygonite extracts lithium sulfate；It is by the way that raw material is levigate, dispensing, roasting
Burn, the steps such as leaching, purification and impurity removal, evaporation and concentration of sizing mixing extract lithium sulfate solution；
2, proportioning of the material provided in the present invention, time etc. of reaction can with its raw material of the extraction and application of economy, with
Meet the commercial value of the exploitation to the raw material, further to improve its competitiveness of product in market；
3, the scheme of experiment is reliable, and impurity is few, and process route is simple, and can be further to the mother liquor in process
Utilize.
Brief description of the drawings：
Accompanying drawing 1 extracts the process chart of lithium sulfate for the acidization of embodiment from amblygonite.
Embodiment：
Embodiment 1：The technique that a kind of acidization extracts lithium sulfate from amblygonite, it is characterised in that：Including following step
Suddenly：
(1) raw material is levigate：Raw material in amblygonite is carried out levigate；
(2) dispensing：By amblygonite of the step (1) after levigate and the concentrated sulfuric acid using weight ratio as 1:0.25~0.37 is carried out
Mixing；The concentrated sulfuric acid is 98% concentrated sulfuric acid solution.
(3) it is calcined：Step (2) mixed material is calcined in Muffle furnace；For can in industrial processes
To be calcined in calcining kiln, clinker is obtained；
(4) size mixing leaching：Step (3) clinker is placed in reactor and adds water progress heating stirring；It is preferred that, it can adopt
It is stirred with electric mixer, it can preferably use distilled water, its reactor can preferably use autoclave
Or stainless steel reaction pot, the leachate containing lithium is obtained after reaction.
(5) purification and impurity removal：To removing the impurity such as aluminium or calcium in the solution of leaching in step (4)；
(6) it is concentrated by evaporation：Solution after the completion of being reacted in step (5) is evaporated concentration.
It is preferred that, it is levigate to the raw material in amblygonite to 100~200 mesh in step (1).
As preferred, temperature control is calcined at 500 DEG C~800 DEG C in step (3), and roasting time is 10~60
Minute.
It is after material cooling that clinker is levigate to 100~200 mesh after step (4) medium roasting as preferred.
As preferred, in step (4)) middle leaching liquid-solid ratio 3~5：1,20 DEG C~150 DEG C of extraction temperature, constant temperature is leached
0.5~2 hour time.
Further, in step (5), the leachate that step (4) is obtained adjusts PH to 7~8 with solid sodium hydroxide, plus
Hot solution is to 80~90 DEG C and isothermal reaction 10~15 minutes；To neutralize the acid in solution and remove the impurity such as the aluminium in solution.
Further, in step (5), to neutralize the acid in solution and remove after the impurity such as the aluminium in solution, by aluminium
Filtered after the completion of reaction；Then repeated hydrogenation sodium oxide molybdena adjusts PH to 14, it is preferred that the sodium hydroxide of addition is solid sodium hydroxide,
To remove magnesium in solution and the impurity such as partial calcium, its reactive chemistry equation is as follows：
Al3++OH-→Al(OH)3↓
Mg2++OH-→Mg(OH)2↓
Ca2++OH-→Ca(OH)2↓
Further, it is heavy in the saturated solution of sodium carbonate of addition amount of calculation excessive 10% or production in step (5)
Heated solution is filtered to 80~90 DEG C of simultaneously isothermal reaction 10~15 minutes, filterings after the completion of question response in lithium mother liquor, course of reaction
Clear liquid afterwards adjusts PH to 6.5~7.5 with sulfuric acid again, and calcium impurities therein are removed with depth, and its reactive chemistry equation is as follows：
Ca2++CO3 2-→CaCO3↓。
As preferred, in step (6), when aoxidizing lithium concentration when being concentrated in solution for 45g/l or so, stop adding
Heat.
As preferred, it can be entered in the levigate technique in step (1), step (4) using levigate machine or ball mill
Processing that row is levigate.
Details are as follows for the dominating process route and technical characteristic of the present invention：
1st, raw material is levigate and dispensing
Raw material is levigate and mixed in dispensing and be conducive to being smoothed out for solid phase reaction, dispensing be in order to add can and lithium
Peganite ore deposit is reacted and lithium is at utmost converted into water-soluble lithium compound, so as to be conducive to subsequent handling to extract lithium.
1.1st, then weigh amblygonite ore deposit is levigate, be put into a porcelain crucible, manual mixing is uniform to 180 mesh.Then
The concentrated sulfuric acid is proportionally added into, then carries out manual mixing, untill well mixed.
The proportioning of amblygonite and sulfuric acid is：Amblygonite：Sulfuric acid=1：0.25~~0.37
Formula be have passed through after pre-selection, and several groups of main formulas are listed.
Specific test recipe such as table 3 below：
| Numbering | 1 | 2 | 3 | 4 |
| Formula | 1:0.25 | 1:0.30 | 1:0.35 | 1:0.37 |
2nd, it is calcined
By roasting, water insoluble lithium is converted into water-soluble lithium compound in material.
The material prepared is put into Muffle furnace the roasting that heats up, sintering temperature control is in 500~800 DEG C of (each sample settings
Different sintering temperatures), constant temperature calcining time control is 30 minutes.
Sintering temperature is determined by testing, and the constant temperature calcining time is then with calcining kiln high temperature section general in industrial production
About half an hour passage time is foundation.By taking 4 formulas in table as an example, the lithium conversion ratio such as following table under its different sintering temperature：
Table 4
Sintering temperature is determined by testing, and the constant temperature calcining time is then with calcining kiln high temperature section general in industrial production
About half an hour passage time is foundation.By taking 4 formulas in table as an example, the lithium conversion ratio such as following table under its different sintering temperature：
Table 4-1 is (with amblygonite：Sulfuric acid=1:Exemplified by the roasting of 0.37 proportioning)
Table 4-2 is (with amblygonite：Sulfuric acid=1:Exemplified by 0.37 proportioning and 30 minutes constant temperature calcinings)
| Levigate fineness (mesh) | 500℃ | 600℃ | 650℃ | 700℃ | 800℃ |
| 100 | 32.49% | 35.26% | 45.25% | 56.28% | 63.63% |
| 180 | 79.65% | 86.96% | 95.11% | 97.48% | 97.69% |
| 200 | 81.52% | 87.32% | 95.45% | 97.62% | 97.96% |
3rd, size mixing leaching
Roasting clinker is levigate to 180 mesh, then weigh a certain amount (general 2.5~~10 grams) and add reactor
In, then measure 100ml distilled water and add reactor, reactor is installed, heating is opened and stirs, set reaction temperature as 95~
150 DEG C, the reaction time 1~~2 hours, reaction closes heating after terminating, and continues to stir and cool, then filters, filtrate
Sampling analysis, leached mud adds 50ml water heating stirring to wash, and filtering, slag adds 50ml water wash twice, baking oven is put into after filtering again
Interior drying, weighs and sampling analysis slag oxide containing lithium amount after cooling.Slag washing water, which is returned, (to be measured and divides during due to experiment for leaching
Analysis reason does not return to leaching).
In order to obtain higher concentration and large volume of lithium solution, 200~400 grams of roasting clinkers are weighed every time with liquid-solid ratio
3~5:1 ratio is leached in stainless steel reaction pot, and electric furnace is then used in heating, and uses electric stirring.Same reaction temperature is
95~150 DEG C, the reaction time 1~~2 hours.Natural cooling after the completion of reaction, is then filtered, using buchner funnel and filter flask and
Vavuum pump is filtered by vacuum, and leached mud is taken out after being filtered dry with liquid-solid ratio 3：1 adds water and heating stirring washing, and the heat time 10~
20 minutes, 80 DEG C or so of heating-up temperature, then suction filtration again, adds water elution twice after draining, and elution liquid-solid ratio is every time
0.5：1, take out to be put into after drying in oven, cooling after suction filtration is dry and weighs and sampling analysis slag oxide containing lithium amount, slag washing water can be with
Return for leaching and (being measured during due to experiment and analysis reason does not return to leaching).(1#, 2# are corresponding for leachate analysis result
Formula is 1 respectively:0.35 and 1:0.37)
Table 5 (mg/l)
Note：1#2# is to use result of the reactor in high liquid-solid ratio, and 3# is to use result of the reaction pot in low liquid-solid ratio.
The influence of different extraction temperatures and different extraction times to leaching rate is as follows
Table 6
Leached mud analysis result is as follows：
Table 7 (%)
4th, purification and impurity removal
The leachate that 3rd step is obtained adjusts PH to 7~8, heated solution to 80~90 DEG C and constant temperature with solid sodium hydroxide
Reaction 10~15 minutes, to neutralize the acid in solution and remove the impurity such as the aluminium in solution, is filtered after the completion of reaction.Then add again
Solid sodium hydroxide adjusts PH to 14, to remove magnesium in solution and the impurity such as partial calcium.In order to which depth removes calcium therein, also
Adding the saturated solution of sodium carbonate of amount of calculation excessive 10% (can be replaced with sinker mother liquor in production, utilize carbonic acid therein
Root).Answer heated solution to 80~90 DEG C and isothermal reaction 10~15 minutes in course of reaction, filtered after the completion of question response.Filtering
Clear liquid afterwards adjusts PH to 6.5~7.5 with sulfuric acid again.
The main chemical reactions of purification and impurity removal are as follows：
Al3++OH-→Al(OH)3↓
Mg2++OH-→Mg(OH)2↓
Ca2++OH-→Ca(OH)2↓
Ca2++CO3 2-→CaCO3↓
5th, it is concentrated by evaporation
The solution obtained after the completion of 4th step is added in beaker or stainless steel reaction pot, heating on electric furnace is placed in and is steamed
Hair concentration, when aoxidizing lithium concentration when being concentrated in solution for 45g/l or so, stops heating, suction filtration is removed in evaporation process and analysed
Some impurity (impurity such as calcium and magnesium that mainly supersaturation is separated out) gone out, obtain limpid lithium sulfate concentrate, solution composition is such as
Under：(g/l)
Table 8
Embodiment 2:
(1) raw material is levigate and dispensing:
It is first that amblygonite ore deposit is levigate to 180 mesh.A porcelain crucible is taken, drying is cleaned, weighs, then by levigate lithium phosphorus aluminium
Stone flour is added weighs in porcelain crucible, weighs weight for 400 grams, then weighs 140 grams of concentrated sulfuric acids with a plastic beaker, dense by what is weighed up
Sulfuric acid is added to be mixed in porcelain crucible with amblygonite, and manual mixing is uniform.Formula and proportioning now be：Amblygonite：Sulfuric acid
=1：0.35.
(2) it is calcined:
The material that 1st step is prepared is installed with two porcelain crucibles, is put into Muffle furnace, opens heating, and setting maximum temperature is
700℃.After Muffle in-furnace temperature is raised to 700 DEG C, constant temperature calcining 30 minutes, to the time after closing switch stop heating.Then
Take out and put in drier after furnace temperature lowers, be cooled to room temperature, weigh.Then it is its is levigate to 180 mesh sieves excessively.
(3-1) is leached：
The 2nd step is weighed into 400 grams through the levigate clinker to after 180 mesh to add in stainless steel reaction pot, according to liquid-solid ratio 5:1
Ratio with graduated cylinder measure 2000ml distilled water add stainless steel reaction pot in, reaction pot is placed on electric furnace, electric mixing is loaded onto
Mix, cover lid, open heating and stir, in 95 DEG C or so isothermal reactions 1 hour.After the completion of reaction, hot solution is filtered.This
Place carries out suction filtration using bottle,suction, obtains filtrate 1827ml, sampling analysis, analysis result is as follows：(g/l)
Leached mud is with liquid-solid ratio about 3:1 ratio add water heating stirring washing, then elute again.Wet slag weighs 427 grams, consumption
Cylinder measures 1000ml distilled water and added in stainless steel reaction pot, and reaction pot is placed on electric furnace, loads onto electric stirring, is then turned on adding
Heat and stirring, stir at a temperature of 70~80 DEG C and wash 15 minutes, be then filtered by vacuum with bottle,suction, and add water elution twice, every time
Added water 100ml, is filtered dry, and washed wet slag is installed with enamel tray to be put into baking oven, is dried, is weighed after cooling at a temperature of 105 DEG C,
And sampling analysis, analysis result is as follows：(%)
(3-2) is leached：
Clinker of 2nd step after levigate is levigate to 200 mesh, weigh 400 grams and add in stainless steel reaction pot, it is solid according to liquid
Than 4:1 ratio measures 1600ml distilled water with graduated cylinder and added in stainless steel reaction pot, and reaction pot is placed on electric furnace, electricity is loaded onto
Dynamic stirring, covered lid, opens heating and stirs, in 95 DEG C or so isothermal reactions 1 hour.After the completion of reaction, by hot solution mistake
Filter.Suction filtration is carried out using bottle,suction herein, filtrate 1455ml is obtained, sampling analysis, analysis result is as follows：(g/l)
Leached mud is with liquid-solid ratio about 3:1 ratio add water heating stirring washing, then elute again.Wet slag weighs 410 grams, consumption
Cylinder measures 1000ml distilled water and added in stainless steel reaction pot, and reaction pot is placed on electric furnace, loads onto electric stirring, is then turned on adding
Heat and stirring, stir at a temperature of 70~80 DEG C and wash 15 minutes, be then filtered by vacuum with bottle,suction, and add water elution twice, every time
Added water 100ml, is filtered dry, and washed wet slag is installed with enamel tray to be put into baking oven, is dried, is weighed after cooling at a temperature of 105 DEG C,
And sampling analysis, analysis result is as follows：(%)
(3-3) is leached：
Clinker of 2nd step after levigate is levigate to 100 mesh, weigh 400 grams and add in stainless steel reaction pot, it is solid according to liquid
Than 3:1 ratio measures 1200ml distilled water with graduated cylinder and added in stainless steel reaction pot, and reaction pot is placed on electric furnace, electricity is loaded onto
Dynamic stirring, covered lid, opens heating and stirs, in 95 DEG C or so isothermal reactions 1 hour.After the completion of reaction, by hot solution mistake
Filter.Suction filtration is carried out using bottle,suction herein, filtrate 1056ml is obtained, sampling analysis, analysis result is as follows：(g/l)
Leached mud is with liquid-solid ratio about 3:1 ratio add water heating stirring washing, then elute again.Wet slag weighs 413 grams, consumption
Cylinder measures 1000ml distilled water and added in stainless steel reaction pot, and reaction pot is placed on electric furnace, loads onto electric stirring, is then turned on adding
Heat and stirring, stir at a temperature of 70~80 DEG C and wash 15 minutes, be then filtered by vacuum with bottle,suction, and add water elution twice, every time
Added water 100ml, is filtered dry, and washed wet slag is installed with enamel tray to be put into baking oven, is dried, is weighed after cooling at a temperature of 105 DEG C,
And sampling analysis, analysis result is as follows：(%)
(4) purification and impurity removal
3-1 is walked to obtained leachate and adjusts PH to 7~8 with solid sodium hydroxide, heated solution is to 80~90 DEG C and permanent
Temperature reaction 10~15 minutes, to neutralize the acid in solution and remove the impurity such as the aluminium in solution, is filtered after the completion of reaction.Then again
Reinforcing body sodium hydroxide adjusts PH to 14, to remove magnesium in solution and the impurity such as partial calcium.In order to which depth removes calcium therein,
Also to add the saturated solution of sodium carbonate of amount of calculation excessive 10% (can be replaced with sinker mother liquor in production, utilize carbon therein
Acid group).Answer heated solution to 80~90 DEG C and isothermal reaction 10~15 minutes in course of reaction, filtered after the completion of question response.Cross
Clear liquid after filter adjusts PH to 6.5~7.5 with sulfuric acid again.
It is concentrated by evaporation：
The solution 1794ml obtained after the completion of 4th step is added in beaker, heating on electric furnace is placed in and is evaporated concentration, etc.
To when being concentrated to solution about 550ml, stop heating, stand cooling, then suction filtration removes some impurity separated out in evaporation process
(impurity such as calcium and magnesium that mainly supersaturation is separated out), obtains limpid lithium sulfate concentrate 541ml, solution composition is as follows：(g/l)
| Solution composition | Li2O | Na | K | Ca | Mg | Fe | SO4 |
| Testing result | 46.74 | 9.63 | 0.54 | 0.055 | 0.003 | 0.003 | 169.26 |
Certainly, better embodiment of the present invention is these are only, the use scope of the present invention is not limited with this, therefore, it is every
Equivalent change is made in the principle of the invention to should be included within the scope of the present invention.
Claims (10)
1. the technique that a kind of acidization extracts lithium sulfate from amblygonite, it is characterised in that：Comprise the following steps：
(1) raw material is levigate：Raw material in amblygonite is carried out levigate；
(2) dispensing：By amblygonite of the step (1) after levigate and the concentrated sulfuric acid using weight ratio as 1:0.25~0.37 is mixed
Close；
(3) it is calcined：Step (2) mixed material is calcined, clinker is obtained；
(4) size mixing leaching：Step (3) clinker is placed in reactor and adds water progress heating stirring, obtain the leachate containing lithium；
(5) purification and impurity removal：To removing the impurity such as aluminium or calcium in the solution of leaching in step (4)；
(6) it is concentrated by evaporation：Solution after the completion of being reacted in step (5) is evaporated concentration, obtains lithium sulfate solution.
2. the technique that a kind of acidization according to claim 1 extracts lithium sulfate from amblygonite, it is characterised in that：
Step (1) is levigate to the raw material in amblygonite to 100~200 mesh.
3. the technique that a kind of acidization according to claim 1 extracts lithium sulfate from amblygonite, it is characterised in that：
Temperature control is calcined at 500 DEG C~800 DEG C in step (3), and roasting time is 20~60 minutes.
4. the technique that a kind of acidization according to claim 1 extracts lithium sulfate from amblygonite, it is characterised in that：
It is after material cooling that clinker is levigate to 100~200 mesh after step (4) medium roasting.
5. the technique that a kind of acidization according to claim 1 extracts lithium sulfate from amblygonite, it is characterised in that：
Step (4)) middle leaching liquid-solid ratio 3~5：1.
6. the technique that a kind of acidization according to claim 1 extracts lithium sulfate from amblygonite, it is characterised in that：Leaching
Go out 20 DEG C~150 DEG C of temperature, constant temperature extraction time 0.5~2 hour.
7. a kind of acidization according to claim any one of 1-6 extracts the technique of lithium sulfate from amblygonite, it is special
Levy and be：In step (5), the leachate that step (4) is obtained adjusts PH to 7~8, heated solution to 80 with solid sodium hydroxide
~90 DEG C and isothermal reaction 10~15 minutes；To neutralize the acid in solution and remove the impurity such as the aluminium in solution.
8. the technique that a kind of acidization according to claim 7 extracts lithium sulfate from amblygonite, it is characterised in that：
In step (5), to neutralize the acid in solution and remove after the impurity such as the aluminium in solution, it will be filtered after the completion of reactive aluminum；Then again
It is hydrogenated with sodium oxide molybdena and adjusts PH to 14, removes magnesium in solution and the impurity such as partial calcium.
9. the technique that a kind of acidization according to claim 8 extracts lithium sulfate from amblygonite, it is characterised in that：
In step (5), add amount of calculation excessive 10% saturated solution of sodium carbonate or production in sinker mother liquor, heat in course of reaction
Solution is to 80~90 DEG C of simultaneously isothermal reaction 10~15 minutes, filterings after the completion of question response, and the clear liquid after filtering is again with sulfuric acid tune PH
To 6.5~7.5, calcium impurities therein are removed with depth.
10. a kind of acidization according to claim any one of 1-6 extracts the technique of lithium sulfate from amblygonite, it is special
Levy and be：In step (6), when aoxidizing lithium concentration when being concentrated in solution for 45g/l or so, stop heating.
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| CN201710577804.1A CN107188205A (en) | 2017-07-15 | 2017-07-15 | The technique that a kind of acidization extracts lithium sulfate from amblygonite |
| PCT/CN2017/098776 WO2019015012A1 (en) | 2017-07-15 | 2017-08-24 | Process for extraction of lithium sulfate from amblygonite by acidification method |
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| CN201710577804.1A CN107188205A (en) | 2017-07-15 | 2017-07-15 | The technique that a kind of acidization extracts lithium sulfate from amblygonite |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108862227A (en) * | 2018-09-21 | 2018-11-23 | 深圳市德方纳米科技股份有限公司 | One kind extracting lithium from amblygonite and prepares iron-containing phosphatic method |
| CN108910851A (en) * | 2018-09-21 | 2018-11-30 | 深圳市德方纳米科技股份有限公司 | A method of lithium-containing compound is prepared by amblygonite |
| CN109354046A (en) * | 2018-11-08 | 2019-02-19 | 中国神华能源股份有限公司 | A method of lithium carbonate is prepared using dirty mother liquor is steamed |
| WO2019227158A1 (en) * | 2018-05-30 | 2019-12-05 | Lithium Australia Nl | Process for recovering lithium phosphate and lithium sulfate from lithium-bearing silicates |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103114211A (en) * | 2013-02-19 | 2013-05-22 | 宁波莲华环保科技股份有限公司 | Method for extracting lithium from primary lithium extraction solution of lithium ore |
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| WO2019227158A1 (en) * | 2018-05-30 | 2019-12-05 | Lithium Australia Nl | Process for recovering lithium phosphate and lithium sulfate from lithium-bearing silicates |
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| CN108910851A (en) * | 2018-09-21 | 2018-11-30 | 深圳市德方纳米科技股份有限公司 | A method of lithium-containing compound is prepared by amblygonite |
| CN108910851B (en) * | 2018-09-21 | 2021-12-31 | 深圳市德方纳米科技股份有限公司 | Method for preparing lithium-containing compound from lithium-phosphorus-aluminum |
| CN108862227B (en) * | 2018-09-21 | 2022-11-11 | 深圳市德方纳米科技股份有限公司 | Method for extracting lithium from lithium-phosphorus-aluminum and preparing iron-containing phosphate |
| CN109354046A (en) * | 2018-11-08 | 2019-02-19 | 中国神华能源股份有限公司 | A method of lithium carbonate is prepared using dirty mother liquor is steamed |
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