CN103227326B - Synthesis method of lithium hexafluorozirconate and new application thereof - Google Patents

Synthesis method of lithium hexafluorozirconate and new application thereof Download PDF

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CN103227326B
CN103227326B CN201310127955.9A CN201310127955A CN103227326B CN 103227326 B CN103227326 B CN 103227326B CN 201310127955 A CN201310127955 A CN 201310127955A CN 103227326 B CN103227326 B CN 103227326B
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lithium
suspension
turbid liquid
hexafluoro
pure water
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CN103227326A (en
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石世昆
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Jiangxi Shi Lei Fluorine Material Co., Ltd.
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BEIJING SHILEI QIANKUN FLUORINATED NEW MATERIALS RESEARCH INSTITUTE Co Ltd
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    • Y02E60/10—Energy storage using batteries

Abstract

The invention provides a synthesis method of lithium hexafluorozirconate and its new application. The synthesis method comprises the steps of: firstly, preparing a transparent fluorozirconic acid solution; secondly, preparing lithium fluoride into a 20-30% lithium fluoride suspension liquid by using pure water; thirdly, adding the lithium fluoride suspension liquid obtained in the second step into the transparent fluorozirconic acid solution prepared in the first step in a dropwise manner, thus obtaining a white and turbid lithium hexafluorozirconate suspension liquid; and fourthly, stirring and heating the lithium hexafluorozirconate suspension liquid prepared in the third step to make water in the lithium hexafluorozirconate suspension liquid evaporated and make the suspension liquid concentrated, when the suspension liquid becomes fully white and turbid, conducting filtering, washing a filter cake by pure water and performing crystallization, then placing crystals on a PTFE board, implementing heating and drying, naturally cooling the crystals, and carrying out grinding and crushing, thus obtaining lithium hexafluorozirconate powder. The synthesized lithium hexafluorozirconate has high purity, and when it is applied to a lithium battery electrolyte solution containing lithium hexafluorophosphate, conductivity of the lithium battery electrolyte solution is significantly enhanced, so that the lithium battery performance can be improved.

Description

The synthetic method of hexafluoro zirconate lithium and novelty teabag thereof
Technical field
The invention belongs to Study on Li-ion batteries technical field, be specifically related to a kind of synthetic method and novelty teabag thereof of hexafluoro zirconate lithium.
Background technology
Lithium ion battery has the features such as energy density ratio is large, carrying capacity of environment is little, therefore, is widely used in portable electric appts, in the future large-scale application in electric automobile, the fields such as energy-accumulating power station.
Electrolyte, as one of the important component part of lithium ion battery, has been the indispensable part of electrochemical reaction.In prior art, the main lithium hexafluoro phosphate that adopts is as electrolyte, and its conductive capability is still limited, thus can reduce the performance of lithium ion battery.
In prior art, disclose and a kind of lithium hydroxide or lithium chloride or Lithium carbonate solution or suspension-turbid liquid to be added drop-wise in the hexafluoro zirconate lithium solution be mixed with, thus prepare hexafluoro zirconate lithium.But the purity of this kind of method preparation-obtained hexafluoro zirconate lithium is lower.And adopt preparation method provided by the invention, the hexafluoro zirconate lithium that purity is very high can be obtained.The test of X-ray powder diffraction is carried out to the final products that the present invention prepares, by the collection of illustrative plates of Fig. 1 gained, demonstrates final products and be hexafluoro zirconate lithium.Its purity is 97.8%.
The present invention second object is the novelty teabag of the hexafluoro zirconate lithium providing a kind of said method to prepare, and adds in the lithium battery electrolytes containing lithium hexafluoro phosphate by described hexafluoro zirconate lithium; Wherein, described lithium hexafluoro phosphate is main electrolyte, and described hexafluoro zirconate lithium is assisted electrolysis matter.
Preferably, in described lithium battery electrolytes, the mol ratio of lithium hexafluoro phosphate and hexafluoro zirconate lithium is 10: 1-10: 2.
Preferably, the mol ratio of lithium hexafluoro phosphate and hexafluoro zirconate lithium is 10: 1.5.
Preferably, in lithium battery electrolytes, organic solvent is one or more in ethylene carbonate EC, diethyl carbonate DEC, dimethyl carbonate DMC, propene carbonate PC and methyl ethyl carbonate MEC.
The present inventor is devoted for years to the research in lithium battery electrolytes, after many experiments, unexpected to find, when to when adding a certain proportion of hexafluoro zirconate lithium in containing the lithium battery electrolytes of lithium hexafluoro phosphate, the conductivity of lithium battery electrolytes can be significantly improved, thus improve the performance of lithium battery.Follow-up comparative example 2 demonstrates this conclusion.
Summary of the invention
For the defect that prior art exists, the invention provides a kind of synthetic method and novelty teabag thereof of hexafluoro zirconate lithium, the purity of synthesized hexafluoro zirconate lithium is high, when applying it in the lithium battery electrolytes containing lithium hexafluoro phosphate, the conductivity of obvious enhancing lithium battery electrolytes, thus the performance improving lithium battery.
The technical solution used in the present invention is as follows:
The present invention first object is the synthetic method providing a kind of hexafluoro zirconate lithium, comprises the following steps:
The first step, with pure water by zirconium dioxide ZrO 2powder is formulated as the suspension-turbid liquid of 15-25%, stirs this suspension-turbid liquid, drips the hydrofluoric acid of 60-70% in suspension-turbid liquid, obtained transparent fluorine zirconic acid H 2zrF 6solution;
Second step, is formulated as the lithium carbonate suspension-turbid liquid of 20-30%, stirs this suspension-turbid liquid, drip the hydrofluoric acid of 60-70% in suspension-turbid liquid by lithium carbonate powder with pure water, obtained lithium fluoride suspension-turbid liquid; Filter lithium fluoride suspension-turbid liquid, after filter cake pure water, get filter cake and lithium fluoride, with pure water, lithium fluoride is formulated as the lithium fluoride suspension-turbid liquid of 20-30%;
3rd step, prepares the lithium fluoride suspension-turbid liquid obtained by second step, be added drop-wise to the first step and prepare in the transparent fluorine zirconic acid solution obtained, and preparation obtains the hexafluoro zirconate lithium suspension-turbid liquid of gonorrhoea;
4th step, the hexafluoro zirconate lithium suspension-turbid liquid that agitating heating the 3rd step is obtained, make the moisture evaporation and concentration in hexafluoro zirconate lithium suspension-turbid liquid, filter after the abundant gonorrhoea of suspension-turbid liquid, with the crystallization of pure water filter cake, then crystallization is positioned over heating, drying on PTFE plate, naturally grinds after cooling, namely obtain hexafluoro zirconate lithium powder.
Preferably, the crystallization of described filter cake pure water is specially:
Filter cake is placed in centrifuge tube, in centrifuge tube, adds pure water; 25 DEG C of centrifugal 0.5-1h, leave standstill 5-8 hour, crystallization; Wherein, the mass ratio of filter cake and pure water is 10: 1-15: 1.
Preferably, in the 4th step, heating, drying condition is: be first heated to 60 degree and dry 2 hours, and then is heated to 110 degree and dries 2 hours.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction pattern of the hexafluoro zirconate lithium that the present invention prepares.
Embodiment
Hexafluoro zirconate lithium prepares embodiment one
The first step, with pure water by zirconium dioxide ZrO 2powder is formulated as the suspension-turbid liquid of 20%, stirs this suspension-turbid liquid, drips the hydrofluoric acid of 65%, obtained transparent fluorine zirconic acid H in suspension-turbid liquid 2zrF 6solution;
Second step, is formulated as the lithium carbonate suspension-turbid liquid of 25%, stirs this suspension-turbid liquid by lithium carbonate powder with pure water, drip the hydrofluoric acid of 65% in suspension-turbid liquid, obtained lithium fluoride suspension-turbid liquid; Filter lithium fluoride suspension-turbid liquid, after filter cake pure water, get filter cake and lithium fluoride, with pure water, lithium fluoride is formulated as the lithium fluoride suspension-turbid liquid of 25%;
3rd step, prepares the lithium fluoride suspension-turbid liquid obtained by second step, be added drop-wise to the first step and prepare in the transparent fluorine zirconic acid solution obtained, and preparation obtains the hexafluoro zirconate lithium suspension-turbid liquid of gonorrhoea;
4th step, the hexafluoro zirconate lithium suspension-turbid liquid that agitating heating the 3rd step is obtained, makes the moisture evaporation and concentration in hexafluoro zirconate lithium suspension-turbid liquid, filter after the abundant gonorrhoea of suspension-turbid liquid, with the crystallization of pure water filter cake, wherein, crystallization condition is: be placed into by filter cake in centrifuge tube, in centrifuge tube, add pure water; 25 DEG C of centrifugal 0.8h, leave standstill 7 hours, crystallization; Wherein, the mass ratio of filter cake and pure water is 12: 1;
Then crystallization is positioned over heating, drying on PTFE plate, wherein, heating, drying condition is: be first heated to 60 degree and dry 2 hours, and then is heated to 110 degree and dries 2 hours; Naturally grind after cooling, namely obtain hexafluoro zirconate lithium powder.
The purity of the hexafluoro zirconate lithium powder that said method prepares is 97.8%.
Hexafluoro zirconate lithium prepares embodiment two
The first step, with pure water by zirconium dioxide ZrO 2powder is formulated as the suspension-turbid liquid of 15%, stirs this suspension-turbid liquid, drips the hydrofluoric acid of 70%, obtained transparent fluorine zirconic acid H in suspension-turbid liquid 2zrF 6solution;
Second step, is formulated as the lithium carbonate suspension-turbid liquid of 30%, stirs this suspension-turbid liquid by lithium carbonate powder with pure water, drip the hydrofluoric acid of 60% in suspension-turbid liquid, obtained lithium fluoride suspension-turbid liquid; Filter lithium fluoride suspension-turbid liquid, after filter cake pure water, get filter cake and lithium fluoride, with pure water, lithium fluoride is formulated as the lithium fluoride suspension-turbid liquid of 30%;
3rd step, prepares the lithium fluoride suspension-turbid liquid obtained by second step, be added drop-wise to the first step and prepare in the transparent fluorine zirconic acid solution obtained, and preparation obtains the hexafluoro zirconate lithium suspension-turbid liquid of gonorrhoea;
4th step, the hexafluoro zirconate lithium suspension-turbid liquid that agitating heating the 3rd step is obtained, makes the moisture evaporation and concentration in hexafluoro zirconate lithium suspension-turbid liquid, filter after the abundant gonorrhoea of suspension-turbid liquid, with the crystallization of pure water filter cake, wherein, crystallization condition is: be placed into by filter cake in centrifuge tube, in centrifuge tube, add pure water; 25 DEG C of centrifugal 1h, leave standstill 5 hours, crystallization; Wherein, the mass ratio of filter cake and pure water is 10: 1;
Then crystallization is positioned over heating, drying on PTFE plate, wherein, heating, drying condition is: be first heated to 60 degree and dry 2 hours, and then is heated to 110 degree and dries 2 hours; Naturally grind after cooling, namely obtain hexafluoro zirconate lithium powder.
The purity of the hexafluoro zirconate lithium powder that said method prepares is 97.9%.
Hexafluoro zirconate lithium prepares embodiment three
The first step, with pure water by zirconium dioxide ZrO 2powder is formulated as the suspension-turbid liquid of 25%, stirs this suspension-turbid liquid, drips the hydrofluoric acid of 60%, obtained transparent fluorine zirconic acid H in suspension-turbid liquid 2zrF 6solution;
Second step, is formulated as the lithium carbonate suspension-turbid liquid of 20%, stirs this suspension-turbid liquid by lithium carbonate powder with pure water, drip the hydrofluoric acid of 70% in suspension-turbid liquid, obtained lithium fluoride suspension-turbid liquid; Filter lithium fluoride suspension-turbid liquid, after filter cake pure water, get filter cake and lithium fluoride, with pure water, lithium fluoride is formulated as the lithium fluoride suspension-turbid liquid of 20%;
3rd step, prepares the lithium fluoride suspension-turbid liquid obtained by second step, be added drop-wise to the first step and prepare in the transparent fluorine zirconic acid solution obtained, and preparation obtains the hexafluoro zirconate lithium suspension-turbid liquid of gonorrhoea;
4th step, the hexafluoro zirconate lithium suspension-turbid liquid that agitating heating the 3rd step is obtained, makes the moisture evaporation and concentration in hexafluoro zirconate lithium suspension-turbid liquid, filter after the abundant gonorrhoea of suspension-turbid liquid, with the crystallization of pure water filter cake, wherein, crystallization condition is: be placed into by filter cake in centrifuge tube, in centrifuge tube, add pure water; 25 DEG C of centrifugal 0.5h, leave standstill 8 hours, crystallization; Wherein, the mass ratio of filter cake and pure water is 15: 1;
Then crystallization is positioned over heating, drying on PTFE plate, wherein, heating, drying condition is: be first heated to 60 degree and dry 2 hours, and then is heated to 110 degree and dries 2 hours; Naturally grind after cooling, namely obtain hexafluoro zirconate lithium powder.
The purity of the hexafluoro zirconate lithium powder that said method prepares is 97.8%.
Hexafluoro zirconate lithium prepares embodiment four
The first step, with pure water by zirconium dioxide ZrO 2powder is formulated as the suspension-turbid liquid of 18%, stirs this suspension-turbid liquid, drips the hydrofluoric acid of 63%, obtained transparent fluorine zirconic acid H in suspension-turbid liquid 2zrF 6solution;
Second step, is formulated as the lithium carbonate suspension-turbid liquid of 24%, stirs this suspension-turbid liquid by lithium carbonate powder with pure water, drip the hydrofluoric acid of 67% in suspension-turbid liquid, obtained lithium fluoride suspension-turbid liquid; Filter lithium fluoride suspension-turbid liquid, after filter cake pure water, get filter cake and lithium fluoride, with pure water, lithium fluoride is formulated as the lithium fluoride suspension-turbid liquid of 28%;
3rd step, prepares the lithium fluoride suspension-turbid liquid obtained by second step, be added drop-wise to the first step and prepare in the transparent fluorine zirconic acid solution obtained, and preparation obtains the hexafluoro zirconate lithium suspension-turbid liquid of gonorrhoea;
4th step, the hexafluoro zirconate lithium suspension-turbid liquid that agitating heating the 3rd step is obtained, makes the moisture evaporation and concentration in hexafluoro zirconate lithium suspension-turbid liquid, filter after the abundant gonorrhoea of suspension-turbid liquid, with the crystallization of pure water filter cake, wherein, crystallization condition is: be placed into by filter cake in centrifuge tube, in centrifuge tube, add pure water; 25 DEG C of centrifugal 0.9h, leave standstill 6 hours, crystallization; Wherein, the mass ratio of filter cake and pure water is 14: 1;
Then crystallization is positioned over heating, drying on PTFE plate, wherein, heating, drying condition is: be first heated to 60 degree and dry 2 hours, and then is heated to 110 degree and dries 2 hours; Naturally grind after cooling, namely obtain hexafluoro zirconate lithium powder.
The purity of the hexafluoro zirconate lithium powder that said method prepares is 97.9%.
Hexafluoro zirconate lithium prepares embodiment five
The first step, with pure water by zirconium dioxide ZrO 2powder is formulated as the suspension-turbid liquid of 19%, stirs this suspension-turbid liquid, drips the hydrofluoric acid of 63%, obtained transparent fluorine zirconic acid H in suspension-turbid liquid 2zrF 6solution;
Second step, is formulated as the lithium carbonate suspension-turbid liquid of 27%, stirs this suspension-turbid liquid by lithium carbonate powder with pure water, drip the hydrofluoric acid of 62% in suspension-turbid liquid, obtained lithium fluoride suspension-turbid liquid; Filter lithium fluoride suspension-turbid liquid, after filter cake pure water, get filter cake and lithium fluoride, with pure water, lithium fluoride is formulated as the lithium fluoride suspension-turbid liquid of 26%;
3rd step, prepares the lithium fluoride suspension-turbid liquid obtained by second step, be added drop-wise to the first step and prepare in the transparent fluorine zirconic acid solution obtained, and preparation obtains the hexafluoro zirconate lithium suspension-turbid liquid of gonorrhoea;
4th step, the hexafluoro zirconate lithium suspension-turbid liquid that agitating heating the 3rd step is obtained, makes the moisture evaporation and concentration in hexafluoro zirconate lithium suspension-turbid liquid, filter after the abundant gonorrhoea of suspension-turbid liquid, with the crystallization of pure water filter cake, wherein, crystallization condition is: be placed into by filter cake in centrifuge tube, in centrifuge tube, add pure water; 25 DEG C of centrifugal 0.9h, leave standstill 7 hours, crystallization; Wherein, the mass ratio of filter cake and pure water is 11: 1;
Then crystallization is positioned over heating, drying on PTFE plate, wherein, heating, drying condition is: be first heated to 60 degree and dry 2 hours, and then is heated to 110 degree and dries 2 hours; Naturally grind after cooling, namely obtain hexafluoro zirconate lithium powder.
The purity of the hexafluoro zirconate lithium powder that said method prepares is 97.9%.
Hexafluoro zirconate lithium prepares embodiment six
The first step, with pure water by zirconium dioxide ZrO 2powder is formulated as the suspension-turbid liquid of 23%, stirs this suspension-turbid liquid, drips the hydrofluoric acid of 62%, obtained transparent fluorine zirconic acid H in suspension-turbid liquid 2zrF 6solution;
Second step, is formulated as the lithium carbonate suspension-turbid liquid of 23%, stirs this suspension-turbid liquid by lithium carbonate powder with pure water, drip the hydrofluoric acid of 66% in suspension-turbid liquid, obtained lithium fluoride suspension-turbid liquid; Filter lithium fluoride suspension-turbid liquid, after filter cake pure water, get filter cake and lithium fluoride, with pure water, lithium fluoride is formulated as the lithium fluoride suspension-turbid liquid of 28%;
3rd step, prepares the lithium fluoride suspension-turbid liquid obtained by second step, be added drop-wise to the first step and prepare in the transparent fluorine zirconic acid solution obtained, and preparation obtains the hexafluoro zirconate lithium suspension-turbid liquid of gonorrhoea;
4th step, the hexafluoro zirconate lithium suspension-turbid liquid that agitating heating the 3rd step is obtained, makes the moisture evaporation and concentration in hexafluoro zirconate lithium suspension-turbid liquid, filter after the abundant gonorrhoea of suspension-turbid liquid, with the crystallization of pure water filter cake, wherein, crystallization condition is: be placed into by filter cake in centrifuge tube, in centrifuge tube, add pure water; 25 DEG C of centrifugal 0.9h, leave standstill 6 hours, crystallization; Wherein, the mass ratio of filter cake and pure water is 11: 1;
Then crystallization is positioned over heating, drying on PTFE plate, wherein, heating, drying condition is: be first heated to 60 degree and dry 2 hours, and then is heated to 110 degree and dries 2 hours; Naturally grind after cooling, namely obtain hexafluoro zirconate lithium powder.
The purity of the hexafluoro zirconate lithium powder that said method prepares is 97.8%.
Purposes embodiment one
The hexafluoro zirconate lithium that preparation embodiment one prepares is joined in the lithium battery electrolytes containing lithium hexafluoro phosphate; Wherein, the organic solvent in lithium battery electrolytes is PC; The mol ratio of lithium hexafluoro phosphate and hexafluoro zirconate lithium is 10: 1.0, and concentration is respectively 1.0mol/l and 0.10mol/l.
Purposes embodiment two
The hexafluoro zirconate lithium that preparation embodiment three prepares is joined in the lithium battery electrolytes containing lithium hexafluoro phosphate; Wherein, the organic solvent in lithium battery electrolytes is diethyl carbonate DEC; The mol ratio of lithium hexafluoro phosphate and hexafluoro zirconate lithium is 10: 1.2, and concentration is respectively 1.0mol/l and 0.12mol/l.
Purposes embodiment three
The hexafluoro zirconate lithium that preparation embodiment six prepares is joined in the lithium battery electrolytes containing lithium hexafluoro phosphate; Wherein, the organic solvent in lithium battery electrolytes is dimethyl carbonate DMC; The mol ratio of lithium hexafluoro phosphate and hexafluoro zirconate lithium is 10: 1.8, and concentration is respectively 1.0mol/l and 0.18mol/l.
Purposes embodiment four
The hexafluoro zirconate lithium that preparation embodiment six prepares is joined in the lithium battery electrolytes containing lithium hexafluoro phosphate; Wherein, the organic solvent in lithium battery electrolytes is ethylene carbonate EC; The mol ratio of lithium hexafluoro phosphate and hexafluoro zirconate lithium is 10: 1.4, and concentration is respectively 1.0mol/l and 0.14mol/l.
Purposes embodiment five
The hexafluoro zirconate lithium that preparation embodiment six prepares is joined in the lithium battery electrolytes containing lithium hexafluoro phosphate; Wherein, the organic solvent in lithium battery electrolytes is methyl ethyl carbonate MEC; The mol ratio of lithium hexafluoro phosphate and hexafluoro zirconate lithium is 10: 1.6, and concentration is respectively 1.0mol/l and 0.16mol/l.
Test example 1
This test example, for investigating the preparation-obtained electrolyte of purposes embodiment 1-5 the molar conductivity of 20 DEG C, the results are shown in Table 1.
Table 1
Numbering Molar conductivity 0.0001Sm2/mol
Purposes embodiment one 8.5
Purposes embodiment two 8.4
Purposes embodiment three 8.4
Purposes embodiment four 8.5
Purposes embodiment five 8.6
Comparative example 1
This comparative example is for investigating hexafluoro zirconate lithium and the conductivity of lithium hexafluoro phosphate proportioning on electrolyte and the impact of molar conductivity.
As shown in table 2, the following 7 kinds of electrolyte of preparation, measure the electric conductivity of the 7 kinds of electrolyte prepared respectively at 20 DEG C respectively.Wherein, the hexafluoro zirconate lithium that uses of electrolyte 2 to 7 prepares gained for embodiment one.
Table 2
Note: molar conductivity=conductivity ÷ total electrolyte content
As can be seen from the above table, when the organic solvent of electrolyte and main electrolyte hexafluorophosphoric acid lithium content constant, only change the content of assisted electrolysis matter hexafluoro zirconate lithium, the molar conductivity of electrolyte changes greatly.Concrete, when not adding assisted electrolysis matter hexafluoro zirconate lithium in electrolyte, the molar conductivity of electrolyte is minimum; Along with the increase of hexafluoro zirconate lithium content, the molar conductivity of electrolyte increases gradually, and when hexafluoro zirconate lithium mole is 0.15 times of lithium hexafluoro phosphate mole, the molar conductivity of electrolyte is the highest; When then continuing to increase hexafluoro zirconate lithium content, the molar conductivity of electrolyte declines on the contrary.Therefore, the optimum mole ratio of hexafluoro zirconate lithium and lithium hexafluoro phosphate is 0.15: 1.
Carried out identical test to the hexafluoro zirconate lithium that other embodiments of the invention prepare, experimental result is similar.
Comparative example 2
This comparative example is used for more various electrolyte conductivity at different temperatures (mS/cm) and molar conductivity (0.0001Sm 2/ mol), wherein, numbering 1-7 is electrolyte used in comparative example 1.
Table 3
As can be seen from the above table, temperature all increases along with the increase of assisted electrolysis matter addition to conductivity value during four temperature sections of 40 degree at-20 degree.
When hexafluoro zirconate lithium mole is 0.15 times of lithium hexafluoro phosphate mole, the molar conductivity of the electrolyte of four temperature sections is all maximum.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should look protection scope of the present invention.

Claims (7)

1. a synthetic method for hexafluoro zirconate lithium, is characterized in that, comprises the following steps:
The first step, with pure water by zirconium dioxide ZrO 2powder is formulated as the suspension-turbid liquid of 15-25%, stirs this suspension-turbid liquid, drips the hydrofluoric acid of 60-70% in suspension-turbid liquid, obtained transparent fluorine zirconic acid H 2zrF 6solution;
Second step, is formulated as the lithium carbonate suspension-turbid liquid of 20-30%, stirs this suspension-turbid liquid, drip the hydrofluoric acid of 60-70% in suspension-turbid liquid by lithium carbonate powder with pure water, obtained lithium fluoride suspension-turbid liquid; Filter lithium fluoride suspension-turbid liquid, after filter cake pure water, get filter cake and lithium fluoride, with pure water, lithium fluoride is formulated as the lithium fluoride suspension-turbid liquid of 20-30%;
3rd step, prepares the lithium fluoride suspension-turbid liquid obtained by second step, be added drop-wise to the first step and prepare in the transparent fluorine zirconic acid solution obtained, and preparation obtains the hexafluoro zirconate lithium suspension-turbid liquid of gonorrhoea;
4th step, the hexafluoro zirconate lithium suspension-turbid liquid that agitating heating the 3rd step is obtained, make the moisture evaporation and concentration in hexafluoro zirconate lithium suspension-turbid liquid, filter after the abundant gonorrhoea of suspension-turbid liquid, with the crystallization of pure water filter cake, then crystallization is positioned over heating, drying on PTFE plate, naturally grinds after cooling, namely obtain hexafluoro zirconate lithium powder.
2. the synthetic method of hexafluoro zirconate lithium according to claim 1, is characterized in that, the crystallization of described filter cake pure water is specially:
Filter cake is placed in centrifuge tube, in centrifuge tube, adds pure water; 25 DEG C of centrifugal 0.5-1h, leave standstill 5-8 hour, crystallization; Wherein, the mass ratio of filter cake and pure water is 10:1-15:1.
3. the synthetic method of hexafluoro zirconate lithium according to claim 1, is characterized in that, in the 4th step, heating, drying condition is: be first heated to 60 degree and dry 2 hours, and then is heated to 110 degree and dries 2 hours.
4. the purposes of hexafluoro zirconate lithium for preparing of the synthetic method of hexafluoro zirconate lithium according to claim 1, is characterized in that, add in the lithium battery electrolytes containing lithium hexafluoro phosphate by described hexafluoro zirconate lithium; Wherein, described lithium hexafluoro phosphate is main electrolyte, and described hexafluoro zirconate lithium is assisted electrolysis matter.
5. the purposes of hexafluoro zirconate lithium according to claim 4, is characterized in that, in described lithium battery electrolytes, the mol ratio of lithium hexafluoro phosphate and hexafluoro zirconate lithium is 10:1-10:2.
6. the purposes of hexafluoro zirconate lithium according to claim 5, is characterized in that, the mol ratio of lithium hexafluoro phosphate and hexafluoro zirconate lithium is 10:1.5.
7. the purposes of hexafluoro zirconate lithium according to claim 4, is characterized in that, in lithium battery electrolytes, organic solvent is at least one in ethylene carbonate EC, diethyl carbonate DEC, dimethyl carbonate DMC, propene carbonate PC and methyl ethyl carbonate MEC.
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