CN107344724A - A kind of method that simple and efficient reduces content of magnesium in salt lake bittern - Google Patents
A kind of method that simple and efficient reduces content of magnesium in salt lake bittern Download PDFInfo
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- CN107344724A CN107344724A CN201610293802.5A CN201610293802A CN107344724A CN 107344724 A CN107344724 A CN 107344724A CN 201610293802 A CN201610293802 A CN 201610293802A CN 107344724 A CN107344724 A CN 107344724A
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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
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- 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
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/22—Magnesium hydroxide from magnesium compounds with alkali hydroxides or alkaline- earth oxides or hydroxides
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Abstract
The invention discloses a kind of method that simple and efficient reduces content of magnesium in salt lake bittern, including the excessive addition water soluble hydroxide into salt lake bittern, the mole hydroxy of introducing is precipitation Mg completely2+At least 1.5 times of theoretical amount, stir；Separation of solid and liquid is carried out after staticly settling, filtrate is the bittern of low content of magnesium.The method handling process of the present invention is simple and convenient to operate, and can significantly reduce cost of transportation in salt lake field conduct；Excessive allogene will not be introduced in Salt Lake Area, accessory substance magnesium hydroxide is also valuable resource, environmentally friendly.Demagging efficiency high, lithium loss is low, and the filtrate after separation of solid and liquid can be directly used for the preparation of lithium carbonate, especially suitable for the extensive mass separating magnesium and lithium in plateau salt lake.
Description
Technical field
The present invention relates to a kind of method for reducing content of magnesium in salt lake bittern, content of magnesium particularly in lake bittern water containing lithium salts
Method.
Background technology
Lithium is the minimum metallic element of atomic weight, have current potential is most negative, electrochemical equivalent is maximum, high specific heat, high conductivity and
The properties such as chemism is strong, are the ideals for manufacturing disposable battery, charging dynamics battery, aerospace structural material etc.
Metal material.As the whole world substitutes traditional ore source to new energy（Oil, coal, shale gas etc.）Requirement it is more and more urgent,
Lithium battery act as generation of electricity by new energy, power transmission and transformation, the hinge of storing up electricity and core roles.The confession of global lithium raw material-lithium carbonate simultaneously
It should not ask, cause the transaction value of lithium carbonate in 2015 short 1 year, 40,000 yuan have increased to RMB 16 by RMB
Wan Yuan.
Lithium resource is the strategic resources of typical oligopoly, and the overwhelming majority is distributed in Chile, China, the U.S., A Gen
The court of a feudal ruler and Bolivia, China have verified lithium resource reserves and have occupied the whole world second.Lithium is primarily present in salt lake bittern in nature,
It is present on a small quantity in spodumene and lepidolite.The saline lake lithium resource reserves of China account for more than the 85% of Chinese industrial reserves.
In putting forward the method for lithium in various traditional salt lakes, because the magnesium elements and elemental lithium of universal symbiosis are located at the periodic table of elements
Diagonally, extremely close physics and chemical characteristic are possessed, the separation of magnesium lithium is the various core difficult points for putting forward lithium technique.Traditional magnesium lithium
In the method for separation, ionic adsorption method requires high to adsorbent, is granulated difficulty, and permeance property is poor, in absorption and the process of desorption
In, adsorbent is easy to be lost, and the waste of lithium is more than 50%；Calcination method is because running temperature is high, and high energy consumption, caking is serious, and equipment is rotten
Erosion is serious；The extraction of extraction and stripping process long flow path, reagent consumption amount is big, and toxicity is big, unfriendly to environment；Therefore, to the greatest extent
Pipe China, which sits, gathers around advantage saline lake lithium resource, but ripe industrialization salt lake puies forward lithium technology still in small-scale scope or stops so far
Stagnant state, in this context, the vertical industry chain of lithium are seriously restricted, Chinese New Energy Industry such as battery, automobile etc., no
Not be forced to bear raw material and increase crazily pain.
How economically the content of magnesium in salt lake bittern to be reduced, be a key factor for reducing lithium extraction cost.So
And existing technology for removal of magnesium from phosphorous, it is substantially the small-scale demagging operation of laboratory level.Water soluble carbonate（Such as
CN103864249A）And water soluble hydroxide（Such as CN101538057A）It is public to be used for salt lake bittern demagging as magnesium precipitation agent
Recognize more environmental protection and energy saving and cost is relatively low, the relatively simple method of technique.
But water soluble carbonate is in precipitation Mg2+During, it can also be co-precipitated and separate out Li2CO3, the Li rate of recovery is significantly
Reduce.Inventor's test result indicates that, work as Mg2+For concentration in 3g/L or so, excessive water soluble carbonate causes Li except Mg
Loss 15% or so, still receive；But with Mg2+The raising of concentration, Li losses caused by carbonic acid magnesium precipitate also increase therewith
Add.Work as Mg2+Concentration reaches more than 50%, loses the meaning of demagging substantially in 6g/L or so, Li loss.Actually salt lake
Content of magnesium in bittern is generally far above the content of lithium, after being concentrated into and meeting industrial brewed brine condition, Mg2+Concentration generally compared with
Height, cause its use range by very serious limitation.
Soluble hydroxide is in precipitation Mg2+When, hydroxyl is very high for the selectivity of magnesium ion, will not produce LiOH and sink
Form sediment, but magnesium hydrate precipitate is gel, it is difficult to which sedimentation and filtering, magnesium hydroxide gels are to Li+There is stronger suction-operated, lead
Cause Li loss amount excessive.To reduce Li loss, someone take the extra additive of addition surfactant etc. aiding in or
Promote magnesium hydroxide.Such as CN101538057A to this kind of colloid using addition odium stearate, enuatrol, DBSA
Sodium, polyacrylamide, bodied ferric sulfate, a kind of superficiality for improving sediment as surfactant in polyaluminium sulfate
Matter, then add hydrochloric acid octadecylamine, hydroxy chloride amine, ammonium carbonate, ammonium hydrogen carbonate, ammonium chloride, ammonium sulfate, one kind or more of ammoniacal liquor
Kind promotes magnesium hydrate precipitate as crystal accelerator.In CN105152189A, by substituted aniline, natrium nitrosum, sulfuric acid, benzene
Aids precipitation agent is made to improve sediment structure through diazotising and coupling in phenol, in CN105253903A, with the dilute acid amides of polyphenyl,
Polyvinyl alcohol, polyacrylic acid, polyethylene glycol.A variety of and HLB in HPMA, polyvinylpyrrolidone is more than 9 surface
Activating agent and magnesium salts crystal seed improve Mg (OH)2The crystal structure of precipitation.The use of these additives no doubt contributes to improve Mg
(OH)2Precipitation status, but its technological process is relative complex, and the chemical industry medicament categories used are various, unfriendly to environment, non-
Often it is easily destroyed the extremely fragile ecological environment in plateau Salt Lake Area, it is difficult to practice on a large scale.A large amount of uses of additive,
Also transport burden has been aggravated, production cost can also remain high.
Developing a kind of more simple, more friendly to environment salt lake bittern technology for removal of magnesium from phosphorous has very actual meaning
Justice.
The content of the invention
It is an object of the invention to provide a kind of method that content of magnesium salt lake bittern is reduced suitable for industrialization.
The technical solution used in the present invention is：
The method of content of magnesium, comprises the following steps in a kind of reduction salt lake bittern：
1) the excessive addition water soluble hydroxide into salt lake bittern, the mole hydroxy of introducing is precipitation Mg completely2+Reason
By at least 1.5 times of dosage, stir；
2) separation of solid and liquid is carried out after staticly settling, filtrate is the bittern of low content of magnesium.
Preferably, the mole hydroxy of introducing is precipitation Mg completely2+1.5~2 times of theoretical amount.
As the further improvement of the above method, appropriate salt lake bittern is added in filtrate, is made unreacted in filtrate
Mole hydroxy is newly introduced into Mg in salt lake bittern for precipitation completely2+At least 1.5 times of theoretical amount, stir, and stand
Isolated filtrate after precipitation.Further, repeat to introduce new salt lake bittern in filtrate 1~3 time, to consume in filtrate
Excessive hydroxyl, while ensure Mg therein2+It can be precipitated with most fast speed.
As the further improvement of the above method, repeat to add the excessive hydroxyl in salt lake bittern consumption part in filtrate
Afterwards, appropriate salt lake bittern is introduced for the last time, the remaining hydroxyl of filtrate is introduced the complete reaction precipitation of salt lake bittern with new.
As the further improvement of the above method, in salt lake bittern, the concentration of magnesium ion is not less than 3g/L.
As the further improvement of the above method, the temperature staticly settled is 0~50 DEG C.
As the further improvement of the above method, the time staticly settled is at least 6 hours.
As the further improvement of the above method, water soluble hydroxide is NaOH or KOH.
As the further improvement of the above method, first water soluble hydroxide is dissolved in appropriate bittern, then again with
Salt lake bittern mixes；Or water soluble hydroxide solid is added in salt lake bittern by way of stream adds
The beneficial effects of the invention are as follows：
Inventor is had been surprisingly found that in research process, and the amount hydroxy that water soluble hydroxide introduces is added in salt lake bittern
During to precipitate the desired amount of 1.5 times of magnesium ion or more completely, nearly 99.9% magnesium ion, while the hydrogen generated can be not only removed
Magnesia can be with rapid precipitation, and its sinking speed is significantly faster than that hydroxyl is slightly excessive（Less than 1.2 times）, significantly reduce solid-liquid point
From difficulty so that the loss of lithium is greatly reduced, and the waste of lithium is controllable to be no more than 10%.
The inventive method will not introduce excessive allogene in Salt Lake Area, and accessory substance magnesium hydroxide is also valuable
Resource, it is environmentally friendly, cost of transportation can be significantly reduced in salt lake field conduct.
The method handling process of the present invention is simple and convenient to operate, is environmentally friendly, suitable for the extensive batch in plateau salt lake
Change separating magnesium and lithium.Demagging efficiency high of the present invention, lithium loss is low, and the filtrate after separation of solid and liquid can be directly used for the preparation of lithium carbonate.
By further adding salt lake bittern in filtrate, hydroxyl excessive in filtrate can be effectively consumed, it is final complete
Excessive hydroxyl is consumed, avoiding it may endanger to caused by environment.
Brief description of the drawings
Fig. 1 is Mg (OH) in the different lower bittern of NaOH dosages effect2Effect of settling；
Fig. 2 is Mg (OH) under different time of repose2Effect of settling.
Embodiment
The method of content of magnesium, comprises the following steps in a kind of reduction salt lake bittern：
1) the excessive addition water soluble hydroxide into salt lake bittern, the mole hydroxy of introducing is precipitation Mg completely2+Reason
By at least 1.5 times of dosage, stir；
2) separation of solid and liquid is carried out after staticly settling, filtrate is the bittern of low content of magnesium.
The security risk brought for reduction excess hydroxyl is preferable, and the mole hydroxy of introducing is precipitation completely
Mg2+1.5~2 times of theoretical amount.It so can both ensure the Mg (OH) of generation2Can be with rapid subsidence, remaining unreacted hydrogen
Oxygen root is also easier to remove.
As the further improvement of the above method, appropriate salt lake bittern is added in filtrate, is made unreacted in filtrate
Mole hydroxy is newly introduced into Mg in salt lake bittern for precipitation completely2+At least 1.5 times of theoretical amount, stir, and stand
Isolated filtrate after precipitation.Further, repeat to introduce new salt lake bittern in filtrate 1~3 time, to consume in filtrate
Excessive hydroxyl, while ensure Mg therein2+It can be precipitated with most fast speed.
As the further improvement of the above method, repeat to add the excessive hydroxyl in salt lake bittern consumption part in filtrate
Afterwards, appropriate salt lake bittern is introduced for the last time, the remaining hydroxyl of filtrate is introduced the complete reaction precipitation of salt lake bittern with new.
As the further improvement of the above method, in salt lake bittern, the concentration of magnesium ion is not less than 3g/L.Such operation
Can be more economical.The concentration of magnesium ion can be removed in below 60g using this method.
As the further improvement of the above method, the temperature staticly settled is 0~50 DEG C.More economical it can so go
Except the magnesium ion in bittern.Be advantageous to accelerate Mg (OH) although temperature is higher2Sedimentation, but its to equipment, place etc. require
Also greatly improve, it is relatively not economical enough.
Test result indicates that standing can remove more than 99% magnesium ion for 6 hours, enter one as the above method
Step is improved, and the time staticly settled is at least 6 hours.In this case, can be by Mg (OH)2At precipitation increase press filtration
Reason, to reduce Mg (OH)2The volume of precipitation, improve the Li rate of recovery.
As the further improvement of the above method, water soluble hydroxide is NaOH or KOH.
As the further improvement of the above method, first water soluble hydroxide is dissolved in appropriate bittern, then again with
Salt lake bittern mixes；Or water soluble hydroxide solid is added in salt lake bittern by way of stream adds
With reference to experiment, technical scheme is further illustrated.
In following examples, unless otherwise instructed, the main component of used concentrated brine is：Mg2+：4.90g/L and
Li+：6.70g/L.
Influence of the different hydroxyl additions to magnesium ion sinking speed and the Li rate of recovery
Take 400mL bittern some, separately take and remove 1 times of NaOH mass needed for Mg in theory（6.53g）, 1.2 times（7.84g）, 1.5 times
（9.80g）With 2 times（13.07g）Solid be dissolved separately in 50mL hot water, bittern and NaOH solution are mixed, stirring
15min, it is statically placed in 50 DEG C of insulating box, is separated after 3 days with 750AB filter-cloth filterings, collect filtrate, tests and analyzes such as the institute of table 1
Show.
The influence of table 1, NaOH dosage to Mg contents in reduction bittern
Note：The Li rate of recovery=Li+Concentration × filtrate volume ÷（Original bittern volume × Li+Concentration）.
Fig. 1 is Mg (OH) in bittern after different NaOH dosages act on lower 3 days2Effect of settling.Can be with from Fig. 1 and table 1
Find out, NaOH dosages are bigger, Mg (OH)2Effect of settling it is more obvious.With reference to table 1 it is recognised that with the increase of NaOH dosages,
Li in filtrate+Concentration slightly reduce, but the filtrate volume obtained by being separated by filtration gradually increases, from 1 times of dosage when
190mL rises to 400mL during 1.5 times of dosages；The Li rate of recovery improves rapidly.Particularly NaOH is excessively than being more than 1.5：When 1,
The rate of recovery that filtrate volume can reach more than 90%, Li of volume after solution mixes reaches 89.2%, and it is slightly excessive to be far longer than NaOH
Than when 45%.Dosage only by increasing NaOH, so that it may dramatically speed up Mg (OH)2Sedimentation, improve Mg clearance, reduce
Li loss, the effective separating magnesium and lithium for carrying out salt lake bittern, has unexpected effect.
Different time of repose reduce the influence of Mg contents in bittern to NaOH
Take 400mL bittern some, take 9.80gNaOH solids are some to be dissolved separately in 50mL hot water, bittern and NaOH is molten
Liquid mixes, and stirs 15min, is statically placed in 50 DEG C of insulating box, 750AB is used after 3h, 6h, 12h, 24h, 36h, 48h, 72h, 120h
Filter-cloth filtering separates, and collects filtrate, and detection and analysis are as shown in table 2.
2 different time of repose of table reduce the influence of Mg contents in bittern to NaOH
Note：The Li rate of recovery=Li+Concentration × filtrate volume ÷（Original bittern volume × Li+Concentration）.
Fig. 2 is Mg (OH) under different time of repose2Effect of settling, in Fig. 2, gelatinous precipitate volume is：A31,
400mL；A31,330mL；A33,220mL；A34,150mL；A35,130mL；A36,100mL;A37,90mL;A38,80mL.
From table 2 and Fig. 2 it can be found that with reaction and the extension of time of repose, Mg in solution2+And Li+Change not
Substantially, except the early stage reacted and stood（Within 6h）Mg2+And Li+It is slightly higher outer.But Mg (OH)2The effect of settling of colloid with
The extension for reaction time of repose significantly improves, and the volume of colloidal mixture is deposited to 48h 100mL, filtrate from 3h 400mL
Volume 48h 405mL, Li are risen to from 3h 210mL+The rate of recovery bring up to the 91.3% of 48h from the 49.1% of 3h.
After standing 48h, then extend the time, Mg (OH)2The Volume Changes unobvious of colloidal mixture, preferable 24~72h,
More preferably 36~48 hours.
Temperature reduces the influence of Mg contents in bittern to NaOH
Take 400mL bittern some, take 7.84g and 9.80gNaOH solids are some to be dissolved separately in 50mL hot water, by bittern and
NaOH solution mixes, and stirs 15min, is statically placed in 50 DEG C, 35 DEG C, 20 DEG C and 5 DEG C of insulating box, is filtered after 3 days with 750AB respectively
Cloth natural filtration separates, and collects filtrate, and detection and analysis are as shown in table 3.
The temperature of table 3 reduces the influence of Mg contents in bittern to NaOH
Note：The Li rate of recovery=Li+Concentration × filtrate volume ÷（Original bittern volume × Li+Concentration）.
Table 3 is it can be found that under low temperature（5℃）, NaOH is except Mg effect slightly reduction, Mg (OH)2Effect of settling it is slightly worse,
Separation is slightly difficult, and filtrate volume is few, and the Li rate of recovery is low.With the rise of temperature, NaOH is except Mg effect increase, Li recovery
Rate increases.Temperature reaches high temperature（50℃）When, beneficial effect is more obvious.Particularly NaOH is excessively than being 1.5：When 1,
High temperature（50℃）Under the Li rate of recovery low compare low temperature（50℃）It is lower high by 10% or so, reach 89.2%, difference is obvious.Reaction temperature
Degree is to Mg (OH)2Settlement influence it is smaller, but at 20 DEG C and more than, separating magnesium and lithium can be more effectively carried out.
It is contemplated that the feelings of 1.5 times of hydroxyl or more needed for precipitation magnesium ion are added in the bittern of more high Mg/Li ratio
Under condition, there is more preferably removal efficiency to magnesium, obtain actually available low Mg/Li ratio bittern, meet other lithium carbonates preparation technology's
Need.
Industrialize in large-scale production process, can to allow water soluble hydroxide to be mixed with bittern with being more uniformly distributed
First water soluble hydroxide is dissolved in the bittern of part, is then added to afterwards in bittern.Or flowed back to while bittern is introduced
Water soluble hydroxide solid, allows it uniformly to mix.
Excessive NaOH removal in filtrate
Appropriate bittern is added in filtrate, the first new hydroxyl for introducing magnesium ion consumption is hydroxy no more than remaining in bittern
2/3, to obtain faster Mg (OH)2Effect of settling.After circulate operation 1~3 time, remaining hydroxyl concentration is very low in filtrate
.In this case, it can introduce and consume remaining hydroxyl completely just, to remove remaining hydroxyl completely, while to whole
The Mg (OH) of body2Effect of settling is substantially without influence.
Claims (10)
1. a kind of method for reducing content of magnesium in salt lake bittern, comprises the following steps：
The excessive addition water soluble hydroxide into salt lake bittern, the mole hydroxy of introducing is precipitation Mg completely2+It is theoretical
At least 1.5 times of dosage, stir；
Separation of solid and liquid is carried out after staticly settling, filtrate is the bittern of low content of magnesium.
2. according to the method for claim 1, it is characterised in that：The mole hydroxy introduced is precipitation Mg completely2+Reason
By 1.5~2 times of dosage.
3. according to the method for claim 1, it is characterised in that：Appropriate salt lake bittern is added in filtrate, is made in filtrate not
The mole hydroxy of reaction is newly introduced into Mg in salt lake bittern for precipitation completely2+At least 1.5 times of theoretical amount, stirring are equal
It is even, staticly settle rear isolated filtrate.
4. according to the method for claim 3, it is characterised in that：The operation of repetition claim 3 1~3 time, to consume filtrate
Middle excessive hydroxyl.
5. the method according to claim 3 or 4, it is characterised in that：Repeat to add salt lake bittern consumption part in filtrate
After excessive hydroxyl, appropriate salt lake bittern is introduced for the last time, makes the remaining hydroxyl of filtrate and new introducing salt lake bittern complete
Full response precipitates.
6. according to the method for claim 1, it is characterised in that：In salt lake bittern, the concentration of magnesium ion is not less than 3g/L.
7. according to the method for claim 1, it is characterised in that：The temperature staticly settled is 0~50 DEG C.
8. the method according to claim 1 or 7, it is characterised in that：The time staticly settled is at least 6 hours.
9. according to the method for claim 1, it is characterised in that：Water soluble hydroxide is NaOH or KOH.
10. according to the method for claim 1, it is characterised in that：First water soluble hydroxide is dissolved in appropriate bittern,
Then mixed again with salt lake bittern；Or water soluble hydroxide solid is added in salt lake bittern by way of stream adds.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110862101A (en) * | 2019-12-25 | 2020-03-06 | 安徽胜达化工科技有限公司 | Preparation method of potassium nitrate |
| CN111468301A (en) * | 2020-04-17 | 2020-07-31 | 中南大学 | Method for recovering salt lake magnesium resource by fractional precipitation flotation |
| CN114671492A (en) * | 2022-03-09 | 2022-06-28 | 大连理工大学 | Bipolar membrane system for efficiently removing magnesium ions in salt lake brine in-situ alkali preparation |
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| CN110862101A (en) * | 2019-12-25 | 2020-03-06 | 安徽胜达化工科技有限公司 | Preparation method of potassium nitrate |
| CN111468301A (en) * | 2020-04-17 | 2020-07-31 | 中南大学 | Method for recovering salt lake magnesium resource by fractional precipitation flotation |
| CN114671492A (en) * | 2022-03-09 | 2022-06-28 | 大连理工大学 | Bipolar membrane system for efficiently removing magnesium ions in salt lake brine in-situ alkali preparation |
| CN114671492B (en) * | 2022-03-09 | 2023-08-18 | 大连理工大学 | Bipolar membrane system for efficiently removing magnesium ions in salt lake brine by in-situ alkali preparation |
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