CN110078102A - The recoverying and utilizing method of salt lake bittern lithium liquor - Google Patents
The recoverying and utilizing method of salt lake bittern lithium liquor Download PDFInfo
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- CN110078102A CN110078102A CN201910292796.5A CN201910292796A CN110078102A CN 110078102 A CN110078102 A CN 110078102A CN 201910292796 A CN201910292796 A CN 201910292796A CN 110078102 A CN110078102 A CN 110078102A
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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
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
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Abstract
The invention discloses a kind of recoverying and utilizing methods of salt lake bittern lithium liquor, it is comprising steps of S1, into salt lake bittern lithium liquor be added dropwise aluminum salt solution and sodium hydroxide solution simultaneously, three is set to carry out coprecipitation reaction at 25 DEG C~70 DEG C, and keeping the pH of system is 8~13, obtains the nucleating systems with lithium aluminum hydrotalcite nucleus；Wherein, in the salt lake bittern lithium liquor, Li+Concentration be 1g/L~2g/L, CO3 2Concentration be 10g/L~30g/L, OH‑Concentration be 5g/L~25g/L；S2, it is separated by solid-liquid separation after nucleating systems are aged 6h~48h at 50 DEG C~150 DEG C, obtains lithium aluminum hydrotalcite filter cake；S3, by lithium aluminum hydrotalcite Washing of Filter Cake, drying, obtain lithium aluminum hydrotalcite.The salt lake bittern lithium liquor for containing lithium carbonate is prepared lithium aluminum hydrotalcite as raw material by recoverying and utilizing method according to the present invention, is made full use of lithium resource and carbonate therein, hydroxyl etc., is improved the level of resources utilization.
Description
Technical field
The invention belongs to salt lake resources technical field of comprehensive utilization, it relates in particular to a kind of salt lake bittern lithium liquor
Recoverying and utilizing method.
Background technique
Lithium is the most light metallic element of nature, silvery white, has high specific heat, high conductivity and chemical activity strong etc. unique
Physicochemical characteristics, have extensive purposes.Currently, lithium metal and its compound glass ceramics, electrolytic aluminium, lubricating grease,
Sustainable growth is applied in the traditional industries such as air conditioner refrigerating and organic synthesis, metallurgy, chemical industry, medicine and reagent field, is closed in aluminium lithium
The application in the fields such as the energy, military project, aerospace, the nuclear industry such as gold, lithium battery and nuclear fusion is also swift and violent to be expanded, therefore is known as
" industrial monosodium glutamate ", is also considered as important strategic materials by many countries；Again because of its application in terms of lithium battery, it is known as " pushing away
The energy metal of dynamic world's progress ".In nature, the main preservation of lithium resource is in solid mineral and liquid brine.Brine lithium money
Critical role of the source in the exploitation of world's lithium resource has established nearly 30 years, it has caused in terms of applying and extracting lithium compound
The attention of lithium resource exploitation industry.The trend of lithium salts production is to be mentioned with salt lake based on lithium in the world, and ore method mentions supplemented by lithium；And I
State has many advantages, such as that stock number is big, at low cost since salt lake bittern mentions lithium, and as solid lithium ore resources are increasingly depleted, salt lake halogen
Water has been increasingly becoming the main source of lithium resource.The prevailing technology for proposing lithium technology for high Mg/Li ratio salt lake at present, specifically includes that
The processing steps such as salt field process, separating magnesium and lithium, lithium-containing solution removal of impurities, the precipitating conversion of lithium carbonate；Wherein, the precipitating of lithium carbonate turns
Change is added to sodium carbonate liquor in rich lithium solution, prepares lithium carbonate by precipitation reaction, while generating carbon after being separated by solid-liquid separation
Sour lithium mother liquor, as salt lake bittern lithium liquor, the content of lithium still can reach 1g/L~2g/L in this part lithium carbonate mother liquor, be
A kind of important lithium resource, up for recycling and reusing.
For above-mentioned lithium carbonate mother liquor, the technique of its recycling and reusing is usually first removed using hydrochloric acid at present therein
Carbonate, then plus alkali adjust its pH；In this way, one complex process, secondly need to expend soda acid, it is at high cost, and carbon therein
Acid group is not utilized rationally, waste of resource.Therefore, for this part lithium carbonate mother liquor, it is necessary to explore completely new recycling
Reuse method.
Summary of the invention
To solve the above-mentioned problems of the prior art, the present invention provides a kind of recycling of salt lake bittern lithium liquor benefits
With method, which prepares lithium aluminum hydrotalcite as raw material for the salt lake bittern lithium liquor for containing lithium carbonate, fills
Divide and utilize lithium resource therein and carbonate, hydroxyl etc., improves the level of resources utilization.
In order to achieve the above object of the invention, present invention employs the following technical solutions:
A kind of recoverying and utilizing method of salt lake bittern lithium liquor comprising step:
S1, into salt lake bittern lithium liquor simultaneously aluminum salt solution and sodium hydroxide solution is added dropwise, make three 25 DEG C~
Coprecipitation reaction is carried out at 70 DEG C, and keeping the pH of system is 8~13, acquisition is with lithium aluminum hydrotalcite nucleus at nucleome
System；Wherein, in the salt lake bittern lithium liquor, Li+Concentration be 1g/L~2g/L, CO3 2-Concentration be 10g/L~
30g/L, OH-Concentration be 5g/L~25g/L；
S2, it is separated by solid-liquid separation after the nucleating systems are aged 6h~48h at 50 DEG C~150 DEG C, obtains lithium aluminum water
Talcum filter cake；
S3, by the lithium aluminum hydrotalcite Washing of Filter Cake, drying, obtain lithium aluminum hydrotalcite.
Further, in the step S1, Al in the aluminum salt solution3+With Li in the salt lake bittern lithium liquor+
The ratio between the amount of substance be 1:1~5:1；OH in the sodium hydroxide solution-With OH in the salt lake bittern lithium liquor-Object
The sum of amount of matter and Li in the salt lake bittern lithium liquor+The ratio between the amount of substance be 4:1~10:1.
Further, in the step S1, Al in the aluminum salt solution3+With Li in the salt lake bittern lithium liquor+
The ratio between the amount of substance be 1.5:1~3.5:1；OH in the sodium hydroxide solution-With OH in the salt lake bittern lithium liquor-
The sum of the amount of substance described in Li in salt lake bittern lithium liquor+The ratio between the amount of substance be 5:1~8:1.
Further, in the step S1, it is 9~11 that the pH of system is kept during coprecipitation reaction.
Further, in the step S1, the salt lake bittern lithium liquor and the aluminum salt solution and the hydrogen-oxygen
Change sodium solution three and carries out coprecipitation reaction at 30 DEG C~50 DEG C.
Further, in the salt lake bittern lithium liquor, Li+Concentration be 1.3g/L~1.7g/L, CO3 2-It is dense
Degree is 15g/L~25g/L, OH-Concentration be 10g/L~20g/L.
Further, the aluminum salt solution is any one in aluminum nitrate solution, aluminum sulfate solution or liquor alumini chloridi.
Further, in the step S2, the nucleating systems are aged by hydro-thermal method or circumfluence method.
Further, in the step S3, the lithium aluminum hydrotalcite filter cake after washing is done at 60 DEG C~120 DEG C
Dry 12h~48h obtains the lithium aluminum hydrotalcite.
Further, in the step S1, by the aluminum salt solution and the sodium hydroxide solution according to 1mL/min
The speed of~5mL/min is added drop-wise in the salt lake bittern lithium liquor.
The present invention is using salt lake bittern lithium liquor as raw material, using coprecipitation separation and Extraction lithium resource therein,
And wherein carbonate and hydroxyl are made full use of, it converts lithium, carbonate and hydroxyl to sliding with widely applied lithium aluminum water
Stone functional material combines so that the comprehensive utilization of salt lake resources is utilized with functionalization, improves the level of resources utilization.
Specific embodiment
Hereinafter, detailed description of the present invention embodiment in future.However, it is possible to implement this hair in many different forms
It is bright, and the present invention should not be construed as limited to the specific embodiment illustrated here.On the contrary, provide these embodiments be for
Explanation the principle of the present invention and its practical application, to make others skilled in the art it will be appreciated that of the invention is various
Embodiment and the various modifications for being suitable for specific intended application.
The present invention is for waste of resource, technique present in the general processing method for salt lake bittern lithium liquor at present
Complicated, consumption soda acid leads to high expensive, and provides the recycling benefit of another completely new salt lake bittern lithium liquor
With method, which takes full advantage of lithium resource and carbonate, hydroxyl in the salt lake bittern lithium liquor
Deng improving the level of resources utilization.
Specifically, the recoverying and utilizing method of the salt lake bittern lithium liquor includes the following steps:
In step sl, aluminum salt solution and sodium hydroxide solution is added dropwise simultaneously into salt lake bittern lithium liquor, makes three
Coprecipitation reaction is carried out at 25 DEG C~70 DEG C, preferably 30 DEG C~50 DEG C, and keeping the pH of system is 8~13, preferably 9
~11, obtain the nucleating systems with lithium aluminum hydrotalcite nucleus.
Specifically, it as the salt lake bittern lithium liquor of raw material, basic composition is: Li+Concentration be 1g/L~2g/
It L, is preferably 1.3g/L~1.7g/L, CO3 2-Concentration be 10g/L~30g/L, preferably 15g/L~25g/L, OH-Concentration
For 5g/L~25g/L, preferably 10g/L~20g/L.
More specifically, aluminum salt solution is any one in aluminum nitrate solution, aluminum sulfate solution or liquor alumini chloridi.
Further, Al in aluminum salt solution is controlled3+With Li in salt lake bittern lithium liquor+The ratio between the amount of substance be 1:1
~5:1, preferably 1.5:1~3.5:1；Meanwhile controlling OH in sodium hydroxide solution-With OH in salt lake bittern lithium liquor-Object
The sum of amount of matter and Li in salt lake bittern lithium liquor+The ratio between the amount of substance be 4:1~10:1, preferably 5:1~8:1.
Preferably, the aluminum salt solution and sodium hydroxide solution isometric with salt lake bittern lithium liquor can be prepared in advance, and
And Al in control aluminum salt solution3+Substance withdrawl syndrome be salt lake bittern lithium liquor in Li+Substance withdrawl syndrome 1~5
Again, preferably 1.5~3.5 times, while controlling OH in sodium hydroxide solution-With OH in salt lake bittern lithium liquor-Substance amount
The sum of for Li in salt lake bittern lithium liquor+4~10 times of amount, preferably 5~8 times of substance.Then, preferably by aluminium
The speed that both salting liquid and sodium hydroxide solution are all made of 1mL/min~5mL/min is added drop-wise in salt lake bittern lithium liquor,
To carry out the coprecipitation reaction of three.
In this way, passing through being total between salt lake bittern lithium liquor and the aluminum salt solution and sodium hydroxide solution that add simultaneously
Precipitation reaction, completes the nucleation process of pre-prepared lithium aluminum hydrotalcite, wherein the lithium aluminum hydrotalcite nucleus formed can be used as
The basis of subsequent lithium aluminum hydrotalcite growth.
In step s 2, it is separated by solid-liquid separation after nucleating systems being aged 6h~48h at 50 DEG C~150 DEG C, obtains lithium
Aluminum hydrotalcite filter cake.
Above-mentioned ageing can be carried out by hydro-thermal method or circumfluence method carries out.
In step s3, by lithium aluminum hydrotalcite Washing of Filter Cake, drying, lithium aluminum hydrotalcite is obtained.
Preferably, the lithium aluminum hydrotalcite filter cake after washing is dried to 12h~48h at 60 DEG C~120 DEG C, can be obtained lithium
Aluminum hydrotalcite.
Lithium aluminum hydrotalcite is a kind of double-metal hydroxide with layer structure, and metallic element is alternately arranged on laminate
Anion can be inserted in cloth, interlayer, has in fields such as high dispersive catalysis, selective absorption, function additive, biological medicines and answers extensively
With.
In this way, i.e. using salt lake bittern lithium liquor as raw material, using coprecipitation separation and Extraction lithium resource therein, and
Carbonate and hydroxyl therein are taken full advantage of, converts lithium, carbonate and hydroxyl to widely applied lithium aluminum water
Talcum functional material combines so that the comprehensive utilization of salt lake resources is utilized with functionalization, improves the level of resources utilization.
It will illustrate the recycling side of above-mentioned salt lake bittern lithium liquor of the invention by specific embodiment below
Method, still, following embodiments are only the specific examples of recoverying and utilizing method of the invention, are not used in and limit its whole.
Embodiment 1
The salt lake bittern lithium liquor that the present embodiment uses generates after preparing lithium carbonate from the brine in Qinghai salt lake
Mother liquor；Wherein, Li+Concentration be 1.3g/L, CO3 2-Concentration be 15g/L, OH-Concentration be 5g/L.
Firstly, weighing 67.8g Aluminum Chloride Hexahydrate configuration 1L aluminum salt solution, then weigh 18.30g sodium hydroxide configuration 1L hydrogen-oxygen
Change sodium solution.
Then, while according to the speed of 5mL/min by above-mentioned prepared aluminum salt solution and sodium hydroxide solution it is added dropwise to
In the above-mentioned salt lake bittern lithium liquor of 1L, under 70 DEG C, pH=11 coprecipitation reaction occurs for three, obtains brilliant with lithium aluminum hydrotalcite
The nucleating systems of core.
Again, by the nucleating systems of above-mentioned acquisition, hydro-thermal method is aged 48h at 150 DEG C, is then filtered, and obtains lithium aluminium
Hydrotalcite filter cake.
Finally, by the lithium aluminum hydrotalcite Washing of Filter Cake to weakly acidic pH, and dry 48h under the conditions of 120 DEG C, i.e. acquisition lithium aluminium
Hydrotalcite.
Embodiment 2
The salt lake bittern lithium liquor that the present embodiment uses generates after preparing lithium carbonate from the brine in Qinghai salt lake
Mother liquor；Wherein, Li+Concentration be 2g/L, CO3 2-Concentration be 10g/L, OH-Concentration be 20g/L.
Firstly, weighing nine water aluminum nitrate of 540.4g configuration 1L aluminum salt solution, then weigh 10.8g sodium hydroxide configuration 1L hydrogen-oxygen
Change sodium solution.
Then, while according to the speed of 1mL/min by above-mentioned prepared aluminum salt solution and sodium hydroxide solution it is added dropwise to
In the above-mentioned salt lake bittern lithium liquor of 1L, under 50 DEG C, pH=8 coprecipitation reaction occurs for three, obtains brilliant with lithium aluminum hydrotalcite
The nucleating systems of core.
Again, by the nucleating systems of above-mentioned acquisition, circumfluence method is aged 68h at 50 DEG C, is then filtered, and obtains lithium aluminium
Hydrotalcite filter cake.
Finally, by the lithium aluminum hydrotalcite Washing of Filter Cake to weakly acidic pH, and dry 30h under the conditions of 60 DEG C, i.e. acquisition lithium aluminium
Hydrotalcite.
Embodiment 3
The salt lake bittern lithium liquor that the present embodiment uses generates after preparing lithium carbonate from the brine in Qinghai salt lake
Mother liquor；Wherein, Li+Concentration be 1.7g/L, CO3 2-Concentration be 30g/L, OH-Concentration be 25g/L.
Firstly, weighing 146.7g aluminum sulfate configuration 1L aluminum salt solution, then weigh 19.8g sodium hydroxide configuration 1L sodium hydroxide
Solution.
Then, while according to the speed of 3mL/min by above-mentioned prepared aluminum salt solution and sodium hydroxide solution it is added dropwise to
In the above-mentioned salt lake bittern lithium liquor of 1L, under 30 DEG C, pH=13 coprecipitation reaction occurs for three, obtains brilliant with lithium aluminum hydrotalcite
The nucleating systems of core.
Again, by the nucleating systems of above-mentioned acquisition, hydro-thermal method ageing for 24 hours, is then filtered at 80 DEG C, obtains lithium aluminium
Hydrotalcite filter cake.
Finally, by the lithium aluminum hydrotalcite Washing of Filter Cake to weakly acidic pH, and dry 20h under the conditions of 80 DEG C, i.e. acquisition lithium aluminium
Hydrotalcite.
Embodiment 4
The salt lake bittern lithium liquor that the present embodiment uses generates after preparing lithium carbonate from the brine in Qinghai salt lake
Mother liquor；Wherein, Li+Concentration be 1g/L, CO3 2-Concentration be 25g/L, OH-Concentration be 10g/L.
Firstly, weighing 34.791g Aluminum Chloride Hexahydrate configuration 1L aluminum salt solution, then weigh 34.1g sodium hydroxide configuration 1L hydrogen
Sodium hydroxide solution.
Then, while according to the speed of 4mL/min by above-mentioned prepared aluminum salt solution and sodium hydroxide solution it is added dropwise to
In the above-mentioned salt lake bittern lithium liquor of 1L, under 25 DEG C, pH=9 coprecipitation reaction occurs for three, obtains brilliant with lithium aluminum hydrotalcite
The nucleating systems of core.
Again, by the nucleating systems of above-mentioned acquisition, hydro-thermal method is aged 12h at 100 DEG C, is then filtered, and obtains lithium aluminium
Hydrotalcite filter cake.
Although the present invention has shown and described referring to specific embodiment, it should be appreciated by those skilled in the art that:
In the case where not departing from the spirit and scope of the present invention being defined by the claims and their equivalents, can carry out herein form and
Various change in details.
Claims (10)
1. a kind of recoverying and utilizing method of salt lake bittern lithium liquor, which is characterized in that comprising steps of
S1, aluminum salt solution and sodium hydroxide solution is added dropwise simultaneously into salt lake bittern lithium liquor, makes three at 25 DEG C~70 DEG C
Lower carry out coprecipitation reaction, and keeping the pH of system is 8~13, obtains the nucleating systems with lithium aluminum hydrotalcite nucleus；Its
In, in the salt lake bittern lithium liquor, Li+Concentration be 1g/L~2g/L, CO3 2-Concentration be 10g/L~30g/L, OH-
Concentration be 5g/L~25g/L；
S2, it is separated by solid-liquid separation after the nucleating systems are aged 6h~48h at 50 DEG C~150 DEG C, obtains lithium aluminum hydrotalcite
Filter cake；
S3, by the lithium aluminum hydrotalcite Washing of Filter Cake, drying, obtain lithium aluminum hydrotalcite.
2. recoverying and utilizing method according to claim 1, which is characterized in that in the step S1, the aluminum salt solution
Middle Al3+With Li in the salt lake bittern lithium liquor+The ratio between the amount of substance be 1:1~5:1；In the sodium hydroxide solution
OH-With OH in the salt lake bittern lithium liquor-The sum of the amount of substance and Li in the salt lake bittern lithium liquor+Substance
The ratio between amount be 4:1~10:1.
3. recoverying and utilizing method according to claim 2, which is characterized in that in the step S1, the aluminum salt solution
Middle Al3+With Li in the salt lake bittern lithium liquor+The ratio between the amount of substance be 1.5:1~3.5:1；The sodium hydroxide solution
Middle OH-With OH in the salt lake bittern lithium liquor-The sum of the amount of substance and Li in the salt lake bittern lithium liquor+Object
The ratio between amount of matter is 5:1~8:1.
4. recoverying and utilizing method according to claim 1, which is characterized in that in the step S1, coprecipitation reaction mistake
It is 9~11 that the pH of system is kept in journey.
5. recoverying and utilizing method according to claim 1, which is characterized in that in the step S1, the salt lake bittern
Lithium liquor and the aluminum salt solution and the sodium hydroxide solution three carry out coprecipitation reaction at 30 DEG C~50 DEG C.
6. -5 any recoverying and utilizing method according to claim 1, which is characterized in that in the salt lake bittern lithium liquor
In, Li+Concentration be 1.3g/L~1.7g/L, CO3 2-Concentration be 15g/L~25g/L, OH-Concentration be 10g/L~20g/L.
7. -5 any recoverying and utilizing method according to claim 1, which is characterized in that the aluminum salt solution is that aluminum nitrate is molten
Any one in liquid, aluminum sulfate solution or liquor alumini chloridi.
8. -5 any recoverying and utilizing method according to claim 1, which is characterized in that in the step S2, it is described at
Nuclear system is aged by hydro-thermal method or circumfluence method.
9. -5 any recoverying and utilizing method according to claim 1, which is characterized in that in the step S3, will wash
Dry 12h~the 48h at 60 DEG C~120 DEG C of the lithium aluminum hydrotalcite filter cake afterwards, obtains the lithium aluminum hydrotalcite.
10. -5 any recoverying and utilizing method according to claim 1, which is characterized in that in the step S1, will be described
Aluminum salt solution and the sodium hydroxide solution are added drop-wise to the salt lake bittern according to the speed of 1mL/min~5mL/min and mention lithium
In mother liquor.
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| CN115739004A (en) * | 2022-11-25 | 2023-03-07 | 中国科学院青海盐湖研究所 | Lithium-aluminum adsorption material prepared from salt lake brine with high magnesium-lithium ratio and method thereof |
| CN115739002A (en) * | 2022-11-25 | 2023-03-07 | 中国科学院青海盐湖研究所 | Lithium-aluminum adsorbent prepared from carbonate type salt lake original brine and preparation method and application thereof |
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| CN115739004A (en) * | 2022-11-25 | 2023-03-07 | 中国科学院青海盐湖研究所 | Lithium-aluminum adsorption material prepared from salt lake brine with high magnesium-lithium ratio and method thereof |
| CN115739002A (en) * | 2022-11-25 | 2023-03-07 | 中国科学院青海盐湖研究所 | Lithium-aluminum adsorbent prepared from carbonate type salt lake original brine and preparation method and application thereof |
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| CN116282111A (en) * | 2023-03-02 | 2023-06-23 | 武汉理工大学 | Compound, preparation method thereof and application of compound as eluting-deactivation-resistant lithium extraction adsorbent |
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Application publication date: 20190802 |