CN106756106B - A kind of preparation method of zinc-base lithium ion extraction material - Google Patents
A kind of preparation method of zinc-base lithium ion extraction material Download PDFInfo
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- CN106756106B CN106756106B CN201710005190.XA CN201710005190A CN106756106B CN 106756106 B CN106756106 B CN 106756106B CN 201710005190 A CN201710005190 A CN 201710005190A CN 106756106 B CN106756106 B CN 106756106B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
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Abstract
The present invention provides a kind of preparation methods of lithium ion exchanged type zinc-base lithium ion extraction material comprising following steps: after analysis pure cerium hydroxide lithium, zinc hydroxide and ammonium dihydrogen phosphate are mixed in proportion, being fully ground to form abrasive material under room temperature;It is zinc-based compounds that abrasive material obtained is transferred to the solid obtained after being sintered and cooled in high temperature furnace;Zinc-based compounds obtained are ground into graininess, is placed in aqueous solution of nitric acid, shakes at a constant temperature, form particulate matter after isolating supernatant;By particulate matter filtration drying obtained, zinc-base lithium ion extraction material is obtained.Have the characteristics that high stability, synthesis are simple and selectivity is good by zinc-base lithium ion extraction material made from this method.
Description
Technical field
The present invention relates to the preparation methods of zinc-base lithium ion extraction material.
Background technique
Inorganic ion exchanger has high temperature resistant, anti-radiation, synthesis simple and good selective and it is useless in core
Object processing, the enrichment of metal ion and the good characteristic for separating, being shown in the application of chromatography etc., in relation to it
Basic research and application study are strengthened again.
With the growth of lithium consumption figure, non-renewable lithium ore resources are depleted at last, therefore various countries attach great importance to naturally
The research of the valuable elements extracting method such as lithium in salt water resources.The technology that exploitation mentions lithium from natural salt water has important strategy
Meaning.The method that this method uses high temperature solid state reaction, synthesizes a series of zinc-base exchange materials, is replaced in previous with zinc
Magnesium reduces the dissolution rate of ion-exchanger, improves stability.The results show, the ion sieve hold the exchange of lithium ion
Amount is big, and selectivity is good, mentions lithium at low concentrations with preferable effect, application prospect is good.
Summary of the invention
It is an object of the invention to provide a kind of preparation methods of zinc-base lithium ion extraction material, by zinc system made from this method
Lithium ion extraction material has the characteristics that high stability, synthesis are simple and selectivity is good.
For achieving the above object, the preparation method of zinc-base lithium ion extraction material provided by the present invention includes following
Step:
(1) will analysis pure cerium hydroxide lithium, zinc hydroxide and ammonium dihydrogen phosphate in molar ratio (0.6~1.4)/(0.8~
1.2) it after ratio mixing/1, is fully ground to form abrasive material under room temperature;
(2) abrasive material obtained in step (1) is transferred in high temperature furnace, be warming up to 700~800 DEG C be sintered and cooled after
The solid arrived is the zinc-based compounds of lithium;
(3) zinc-based compounds obtained in step (2) are ground into graininess, being placed in concentration is 0.5~1.21mol/L's
It in aqueous solution of nitric acid, is shaken under 25 DEG C of constant temperature, the lithium ion in compound is precipitated is transferred in supernatant completely, isolates
Particulate matter is formed after supernatant;
(4) particulate matter filtration drying obtained in step (3) is obtained into lithium ion extraction material.
In the step (1), dispersing agent is added and has into the mixture of lithium hydroxide, zinc hydroxide and ammonium dihydrogen phosphate
Solvent is simultaneously mixed into slurry and is ground, and dispersing agent is stearic acid, accounts for the 0.18%~0.22% of said mixture gross mass,
Organic solvent is ethyl alcohol, accounts for the 9%~11% of said mixture gross mass.
In the step (3), the zinc-based compounds of granular lithium intermittent oscillation 2d, phase in 25 DEG C of water bath with thermostatic control
Between, the aqueous solution of nitric acid for being separated off supernatant while more renewing, at least 2 times repeatedly.
Drying temperature in step (4) is 80~140 DEG C.
In above-mentioned steps (3), formed after lithium ion is precipitated in the hydrogen ion filling zinc-based compounds in aqueous solution of nitric acid
Hole, repeatedly gap oscillation can guarantee hydrionic be sufficient filling with.
The method of zinc-base lithium ion extraction material provided by the present invention is a kind of completely new zinc-base lithium ion extraction material
Preparation method prepares the Zr-based materials of the lithium with rock-steady structure first, i.e., by analysis pure cerium hydroxide lithium, the hydrogen after above-mentioned grinding
Zinc oxide and ammonium dihydrogen phosphate are allowed to form above-mentioned Zr-based materials through sintering process, and above-mentioned Zr-based materials use lithium ion therein
Ore Leaching (holding of material skeleton is basically unchanged).It is that there is stable structural bone first by the lithium ion material so handled
Frame ensure that its stability, secondly because have passed through ion exchange process, make lithium ion movement should be more smooth and be easy to elute,
Lithium ion exchanged procedure structure is not easily susceptible to destroy, and considerably increases the exchange times of exchanger.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of the zinc-based compounds of lithium.
Specific embodiment
The preparation method of zinc-base lithium ion extraction material of the present invention, these embodiments are further illustrated by the following examples
It is merely to illustrate the present invention, and there is no limit to the present invention.
Embodiment 1
Pure LiOH, Zn (OH) will be analyzed2、NH4H2PO40.6/1.2/1 is mixed after weighing in molar ratio, and stearic acid is added and makees
It is mixed into slurry as organic solvent and said mixture for dispersing agent and ethyl alcohol, stearic acid accounts for said mixture gross mass
0.18%, ethyl alcohol accounts for the 9% of said mixture gross mass, is put into planetary ball mill and is fully ground 8 hours, is formed and is ground after grinding
Grind object, abrasive material is transferred in high temperature furnace by the particle of abrasive material in 1000-2000 mesh, be warming up to 700 DEG C be sintered and cooled after
The solid arrived is the zinc-based compounds of lithium, and the granular size and sintering temperature of above-mentioned abrasive material make the zinc-based compounds generated
Material skeleton have rock-steady structure, weigh zinc-based compounds 5g, it be ground into graininess by pulverizer, addition
The aqueous solution of nitric acid 500ml of 0.5mol/L, in 25 DEG C of water bath with thermostatic control during which intermittent oscillation 2d is separated off supernatant
The aqueous solution of nitric acid more renewed simultaneously, 2 times repeatedly, forms particulate matter after being finally recovered out supernatant, is washed out, and dries
It is dry, zinc-base lithium ion extraction material can be obtained, the drying temperature of above-mentioned precipitating particulate matter is 80 DEG C.Experimental result shows, this
Zinc-base lithium ion extraction material reaches 2.4mgg to the saturation exchange capacity of Li ion-1。
Embodiment 2
Pure LiOH, Zn (OH) will be analyzed2、NH4H2PO41.2/0.9/1 is mixed after weighing in molar ratio, and stearic acid is added and makees
It is mixed into slurry as organic solvent and said mixture for dispersing agent and ethyl alcohol, stearic acid accounts for said mixture gross mass
0.18%, ethyl alcohol accounts for the 9% of said mixture gross mass, is put into planetary ball mill and is fully ground 8 hours, is formed and is ground after grinding
Grind object, abrasive material is transferred in high temperature furnace by the particle of abrasive material in 1000-2000 mesh, be warming up to 725 DEG C be sintered and cooled after
The solid arrived is the zinc-based compounds of lithium, and the granular size and sintering temperature of above-mentioned abrasive material make the zinc-based compounds generated
Material skeleton have rock-steady structure, weigh zinc-based compounds 5g, it be ground into graininess by pulverizer, addition
The aqueous solution of nitric acid 500ml of 0.5mol/L, in 25 DEG C of water bath with thermostatic control during which intermittent oscillation 2d is separated off supernatant
The aqueous solution of nitric acid more renewed simultaneously, 2 times repeatedly, forms particulate matter after being finally recovered out supernatant, is washed out, and dries
It is dry, zinc-base lithium ion extraction material can be obtained, the drying temperature of above-mentioned precipitating particulate matter is 80 DEG C.Experimental result shows, this
Zinc-base lithium ion extraction material reaches 5.1mgg to the saturation exchange capacity of Li ion-1。
Embodiment 3
Pure LiOH, Zn (OH) will be analyzed2、NH4H2PO41.4/0.8/1 is mixed after weighing in molar ratio, and stearic acid is added and makees
It is mixed into slurry as organic solvent and said mixture for dispersing agent and ethyl alcohol, stearic acid accounts for said mixture gross mass
0.18%, ethyl alcohol accounts for the 9% of said mixture gross mass, is put into planetary ball mill and is fully ground 8 hours, is formed and is ground after grinding
Grind object, abrasive material is transferred in high temperature furnace by the particle of abrasive material in 1000-2000 mesh, be warming up to 750 DEG C be sintered and cooled after
The solid arrived is the zinc-based compounds (as shown in Figure 1) of lithium, and the granular size and sintering temperature of above-mentioned abrasive material make generation
The material skeleton of zinc-based compounds has rock-steady structure, weighs zinc-based compounds 5g, it is ground into graininess by pulverizer,
The aqueous solution of nitric acid 500ml of 0.5mol/L is added, in 25 DEG C of water bath with thermostatic control during which intermittent oscillation 2d is separated off supernatant
The aqueous solution of nitric acid more renewed while night 2 times repeatedly, forms particulate matter after being finally recovered out supernatant, is washed out,
Drying, can be obtained zinc-base lithium ion extraction material, and the drying temperature of above-mentioned precipitating particulate matter is 80 DEG C.Experimental result shows,
This zinc-base lithium ion extraction material reaches 5.8mgg to the saturation exchange capacity of Li ion-1。
Embodiment 4
Pure LiOH, Zn (OH) will be analyzed2、NH4H2PO40.8/1.1/1 is mixed after weighing in molar ratio, and stearic acid is added and makees
It is mixed into slurry as organic solvent and said mixture for dispersing agent and ethyl alcohol, stearic acid accounts for said mixture gross mass
0.18%, ethyl alcohol accounts for the 9% of said mixture gross mass, is put into planetary ball mill and is fully ground 8 hours, is formed and is ground after grinding
Grind object, abrasive material is transferred in high temperature furnace by the particle of abrasive material in 1000-2000 mesh, be warming up to 775 DEG C be sintered and cooled after
The solid arrived is the zinc-based compounds of lithium, and the granular size and sintering temperature of above-mentioned abrasive material make the zinc-based compounds generated
Material skeleton have rock-steady structure, weigh zinc-based compounds 5g, it be ground into graininess by pulverizer, addition
The aqueous solution of nitric acid 500ml of 0.5mol/L, in 25 DEG C of water bath with thermostatic control during which intermittent oscillation 2d is separated off supernatant
The aqueous solution of nitric acid more renewed simultaneously, 2 times repeatedly, forms particulate matter after being finally recovered out supernatant, is washed out, and dries
It is dry, zinc-base lithium ion extraction material can be obtained, the drying temperature of above-mentioned precipitating particulate matter is 80 DEG C.Experimental result shows, this
Zinc-base lithium ion extraction material reaches 2.7mgg to the saturation exchange capacity of Li ion-1。
Embodiment 5
Pure LiOH, Zn (OH) will be analyzed2、NH4H2PO4It is mixed after 1/1/1 weighing in molar ratio, stearic acid is added and is used as and divides
Powder and ethyl alcohol are mixed into slurry as organic solvent and said mixture, and stearic acid accounts for said mixture gross mass
0.18%, ethyl alcohol accounts for the 9% of said mixture gross mass, is put into planetary ball mill and is fully ground 8 hours, is formed and is ground after grinding
Grind object, abrasive material is transferred in high temperature furnace by the particle of abrasive material in 1000-2000 mesh, be warming up to 800 DEG C be sintered and cooled after
The solid arrived is the zinc-based compounds of lithium, and the granular size and sintering temperature of above-mentioned abrasive material make the zinc-based compounds generated
Material skeleton have rock-steady structure, weigh zinc-based compounds 5g, it be ground into graininess by pulverizer, addition
The aqueous solution of nitric acid 500ml of 0.5mol/L, in 25 DEG C of water bath with thermostatic control during which intermittent oscillation 2d is separated off supernatant
The aqueous solution of nitric acid more renewed simultaneously, 2 times repeatedly, forms particulate matter after being finally recovered out supernatant, is washed out, and dries
It is dry, zinc-base lithium ion extraction material can be obtained, the drying temperature of above-mentioned precipitating particulate matter is 80 DEG C.Experimental result shows, this
Zinc-base lithium ion extraction material reaches 4.6mgg to the saturation exchange capacity of Li ion-1。
Basic principles and main features and advantages of the present invention of the invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (1)
1. a kind of preparation method of zinc-base lithium ion extraction material, it is characterised in that the following steps are included:
(1) pure cerium hydroxide lithium, zinc hydroxide and ammonium dihydrogen phosphate (0.6~1.4)/(0.8~1.2)/1 in molar ratio will be analyzed
After ratio mixing, it is fully ground to form abrasive material under room temperature;
(2) abrasive material obtained in step (1) is transferred in high temperature furnace, being warming up to the solid that 700 DEG C obtain after being sintered and cooled is
The zinc-based compounds of lithium;
(3) compound powder obtained in step (2) is broken into graininess, it is water-soluble is placed in the nitric acid that concentration is 0.5~1.21mol/L
It in liquid, is shaken under 25 DEG C of constant temperature, the lithium ion in compound is precipitated is transferred in supernatant completely, after isolating supernatant
Form particulate matter;
(4) particulate matter filtration drying obtained in step (3) is obtained into lithium ion extraction material;
In the step (1), into the mixture of lithium hydroxide, zinc hydroxide and ammonium dihydrogen phosphate be added dispersing agent with it is organic molten
Agent is simultaneously mixed into slurry and is ground, and dispersing agent is stearic acid, accounts for the 0.18%~0.22% of said mixture gross mass, organic
Solvent is ethyl alcohol, accounts for the 9%~11% of said mixture gross mass;
In the step (3), during which granular compound intermittent oscillation 2d in 25 DEG C of water bath with thermostatic control is separated off
The aqueous solution of nitric acid that clear liquid more renews simultaneously, at least 2 times repeatedly;
Drying temperature in step (4) is 80~140 DEG C.
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