CN111304679B - Device and method for preparing high-purity lithium hexafluorophosphate through electrolysis by electrochemical ion extraction method - Google Patents

Device and method for preparing high-purity lithium hexafluorophosphate through electrolysis by electrochemical ion extraction method Download PDF

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CN111304679B
CN111304679B CN202010180207.7A CN202010180207A CN111304679B CN 111304679 B CN111304679 B CN 111304679B CN 202010180207 A CN202010180207 A CN 202010180207A CN 111304679 B CN111304679 B CN 111304679B
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CN111304679A (en
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曹余良
赵阿龙
艾新平
杨汉西
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Shenzhen Jana Energy Technology Co ltd
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Wuhan University WHU
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Abstract

The invention belongs to the field of materials and energy, and particularly relates to a device and a method for preparing high-purity lithium hexafluorophosphate through electrolysis based on an electrochemical ion extraction method. Comprises an electrolytic bath A and an electrolytic bath B; the electrolytic bath A is composed of electrodes of materials capable of releasing and inserting anions and cations, and the two electrolyte solutions can be isolated by an ion exchange membrane; the electrolytic bath B consists of two electrodes of the electrolytic bath A, electrochemical ions of the extracted anions and cations are respectively released through the two electrodes in a corresponding electrolyte system to form a target salt solution, and the corresponding electrolyte salt is obtained through a solvent treatment method. The method effectively avoids impurity pollution possibly introduced in the traditional electrolyte salt preparation process, can prepare salts which are difficult to synthesize by the traditional method, and provides a feasible method for improving the quality of the electrolyte salt and developing the preparation of new electrolyte salt.

Description

Device and method for preparing high-purity lithium hexafluorophosphate through electrolysis by electrochemical ion extraction method
Technical Field
The invention belongs to the field of materials and energy, and particularly relates to a device and a method for preparing high-purity lithium hexafluorophosphate serving as an electrolyte salt of an ion battery through electrolysis based on an electrochemical ion extraction method.
Background
The wide popularization of new energy electric vehicles and smart power grids drives the continuous development of power batteries, and LiPF is an important component of the batteries6The electrolyte salt is irreplaceable in lithium batteries due to the comprehensive properties of excellent electrochemical stability, oxidation resistance, high conductivity, capability of passivating a positive current collector, benefit for the generation of a negative electrode SEI, environmental friendliness and the like, and the quality of the electrolyte salt determines the charge and discharge performance, cycle life and safety of the batteries. However, production of high quality LiPF6The purity requirements of LiF and HF which are needed raw materials are extremely high, the solvent is highly toxic and corrosive, the impurity content of the product is high, the LiPF is restricted by high and low temperature, anhydrous and dust-free operation and the like in the production process6The rapid development of the industry.
LiPF6The production techniques of (a) can be summarized in three types: gas-solid reaction, hydrofluoric acid solvent method and organic solvent method. The gas-solid reaction method is to use gaseous PF5Preparation of LiPF by direct reaction with solid LiF6Product LiPF6The coating on the surface of LiF prevents the reaction from continuing. The operation method is relatively simple, but the raw materials are not sufficiently reacted, and the later separation is difficult. Hydrofluoric acid solvent processLiF is dissolved in anhydrous HF to form LiHF2Solution, is introduced into PF5Gas reaction to form LiPF6Filtering and washing the product to obtain LiPF6. The method is carried out in a liquid phase, has fast reaction and high conversion rate, and is a commonly used technology in industry at present. However, the HF solvent has high corrosivity and high requirements on a reaction device, and a small amount of residual HF in the product is difficult to remove, so that the product quality is influenced. The organic solvent method comprises suspending LiF particles in an organic solvent (such as EC, DEC, DMC, EMC), and introducing high-purity PF5Gas reaction to form LiPF6. The method effectively avoids the introduction of HF, and has mild and controllable reaction conditions and high product conversion rate. But PF is present during the reaction5Easily react with organic solvent to generate a large amount of impurities, and simultaneously LiPF6Difficult to separate.
For the above conventional LiPF6Problems in the production technique to further realize high purity LiPF6The invention provides a method for preparing high-purity LiPF by electrolysis based on an electrochemical ion extraction method6A method and apparatus therefor.
Disclosure of Invention
The invention aims to solve the technical problem of providing a device and a method for preparing high-purity lithium hexafluorophosphate through electrolysis based on an electrochemical ion extraction method, effectively avoiding the introduction of impurity ions and ensuring the LiPF product6Has ultrahigh purity, does not need to use harmful materials and solvents, and can effectively reduce environmental pollution.
The technical scheme of the invention can be realized by the following technical measures:
an apparatus for preparing high-purity lithium hexafluorophosphate by electrolysis based on an electrochemical ion extraction method, comprising: an electrolytic cell A for ion extraction and an electrolytic cell B for ion release;
the electrolytic tank A is divided into an anode area and a cathode area by a cation exchange membrane, and the anode area comprises reversible de-intercalation PF6 -Anode made of compound and KPF6An electrolyte, the cathode region including reversibly deintercalated Li+Cathode made of compound and lithium-containing solution；
The electrolytic cell B consists of an anode, an electrolyte and a cathode, wherein the anode and the cathode are respectively made of reversible Li extraction obtained after the electrolytic cell A is fully discharged+Compound and reversible deintercalation PF6 -Compound, the electrolyte is LiPF6And (3) solution.
Reversible deintercalation PF in the cells A and B6 -The reduced anode and the oxidized cathode of the compound are different reaction states of the same electrode, and PF is generated through oxidation-reduction reaction6 -Is inserted and removed, thereby completing the PF6 -Transfer from cell a to cell B; reversible Li deintercalation in cells A and B+The cathode in the oxidized state and the anode in the reduced state of the compound are different reaction states of the same electrode, and Li is generated through oxidation and reduction+Thereby completing Li+Transfer from cell a to cell B.
Preferably, the electrodes of the cell A are made of a corresponding reversible deintercalating PF6 -Compounds or reversible deintercalation of Li+Respectively mixing the compound with a conductive agent and a binder, pressing the mixture into a film, drying the film, and pressing the film on the surface of a current collector to prepare a corresponding reversible disintercalation compound electrode; or will reversibly de-intercalate the PF6 -Compounds or reversible deintercalation of Li+The compound is respectively mixed with a conductive agent and a binder to prepare slurry to be coated on the surface of a current collector, and the corresponding reversible deintercalation compound electrode is prepared.
Preferably, the reversible de-intercalation PF6 -The compound comprises: polyaniline, polypyrrole, polythiophene, polyparaphenylene, polytriphenylamine, or a carbon material; the reversible deintercalation of Li+The compound comprises: lithium manganate, lithium iron phosphate, lithium titanate, lithium cobaltate and nickel cobalt manganese ternary materials.
Preferably, the current collector is an inert conductor, the conductive agent comprises acetylene black, conductive carbon black and Super P, and the binder is PTFE or PVDF.
Preferably, the cation exchange membrane is a monovalent selective cation exchange membrane.
Another object of the present invention is to provide a method for preparing high-purity lithium hexafluorophosphate by electrolysis based on an electrochemical ion extraction method, comprising the following steps:
(1) in the electrolytic tank A, a cation exchange membrane is adopted to be divided into an anode area and a cathode area, and the anode area is reversibly inserted into PF6 -Compound as anode, KPF6For the anolyte, the cathodic region is used for reversible Li extraction+The compound is used as a cathode, a lithium-containing solution is used as a catholyte, and the system is subjected to discharge treatment to enable the anode to reversibly remove and embed PF6 -PF for loss of electron capture by compound6 -Cathodic reversible deintercalation of Li+Obtaining of electron Capture Li from the Compound+，KPF6K in solution+The charge balance is maintained by the migration of the cation exchange membrane from the anode region to the cathode region, thus completing the PF6 -And Li+Extracting;
(2) in the electrolytic cell B, the anode and the cathode of the electrolytic cell A obtained in the step (1) are respectively used as the cathode and the anode, and LiPF is used6The solution is used as electrolyte, and the system is charged to reversibly insert and remove Li+Loss of electrons in compounds to release Li+Reversible de-intercalation PF6 -Compound to obtain electron release PF6 -To complete LiPF6Generating;
(3) the steps (1) and (2) are alternately and circularly carried out to realize LiPF6The continuous preparation of (2).
Compared with the prior art, the invention has the following beneficial effects:
the device for preparing high-purity lithium hexafluorophosphate through electrolysis based on the electrochemical ion extraction method adopts reversible de-intercalation PF6 -Compound electrodes or reversible deintercalation of Li+The compound electrode is used as the electrode material of the two electrolytic tanks, is environment-friendly, has ultrahigh cycle stability and can be repeatedly utilized.
The device for preparing the high-purity lithium hexafluorophosphate through electrolysis based on the electrochemical ion extraction method does not need high and low temperature reaction conditions, and can effectively reduce the production cost.
The invention relates to an electrochemical ion extraction method based electrolytic preparation method of high-purity sodium niobateA lithium hexafluorophosphate apparatus for preparing high-purity LiPF based on ion extraction method6The preparation of the LiPF adopts two independent electrolytic baths, effectively avoids the introduction of impurity ions, the use of harmful materials and solvents and harsh reaction conditions of high and low temperature, and ensures the LiPF product6Has ultrahigh purity, reduces production cost and reduces environmental pollution.
Drawings
The invention is further illustrated by means of the attached drawings, the examples of which are not to be construed as limiting the invention in any way.
FIG. 1 is a schematic diagram of a two-bath method experiment of an apparatus for preparing high-purity lithium hexafluorophosphate by electrolysis based on an electrochemical ion extraction method according to the present invention;
FIG. 2 is a graph showing the variation of voltage with capacity in example 1 of the present invention.
Detailed Description
In order that the invention may be more readily understood, specific embodiments thereof will be described further below.
Example 1
As shown in fig. 1, the electrodes of both electrolytic cells are configured, and the composition of the electrolyte and the charging and discharging modes are as follows:
an electrolytic cell A: reversible deintercalation PF made of Polyaniline (PANI)6 -Compound reduced anode-KPF6The aqueous solution is electrolyte-Nafion 117 proton exchange membrane-LiCl solution-lithium manganate (Li)1-xMnO4) For reversible deintercalation of Li+Compound oxidation state cathode; taking the above electrode pieces 5cm each2At 5mA · cm2The constant current is discharged until the voltage is less than 0V, and the anode PANI loses electron capture PF6 -Formation of PANI+PF6 -Cathode Li1-xMnO4Obtaining electron-trapping Li+Formation of LiMn2O4The discharge voltage-capacity relationship is shown in fig. 2, and it can be seen from fig. 2 that the average discharge voltage is 0.49V.
An electrolytic cell B: by LiMnO4For reversible deintercalation of Li+Compound reduced anode-LiPF6The solution is electrolyte-PANI+PF6 -For reversibly de-intercalation of PF6 -Compound oxidation state cathode; the anode and cathode plates are taken from the electrolytic bath A after reaction and are measured at 5 mA-cm2Is charged to a voltage of more than 1.25V by constant current, and the anode is LiMnO4Loss of electrons to release Li+Generation of Li1- xMn2O4Cathode PANI+PF6 -Obtaining electron emission PF6 -PANI is generated, the relation curve between the charging voltage and the capacity is shown in fig. 2, and the charging average voltage is 0.63V and the current efficiency is 99.5% as can be seen from fig. 2. Analysis of the electrolyte in cell B revealed that it contained Li+、PF6 -And K+The amounts of (A) were 0.483, 0.496 and 0.015mmol, respectively, corresponding to LiPF6The purity is as high as 99.21%.
Example 2
As shown in fig. 1, the electrodes of both electrolytic cells are configured, and the composition of the electrolyte and the charging and discharging modes are as follows:
an electrolytic cell A: reversible deintercalation PF made of polyaniline (PPy)6 -Compound reduced anode-KPF6The aqueous solution is electrolyte-Nafion 117 proton exchange membrane-brine-lithium iron phosphate (Li)1-xFePO4) For reversible deintercalation of Li+Compound oxidation state cathode; taking the above electrode pieces each 10cm2At 10mA · cm2Is discharged until the voltage is less than 0V, the anode PPy loses electron capture PF6 -Formation of PPy+PF6 -Cathode Li1-xFePO4Obtaining electron-trapping Li+Formation of LiFePO4The average discharge voltage was 0.12V.
An electrolytic cell B: from LiFePO4For reversible deintercalation of Li+The anode of the reduced compound-LiPF 6 solution is electrolyte-PPy+PF6 -For reversibly de-intercalation of PF6 -Compound oxidation state cathode; the anode and cathode plates are taken from the electrolytic bath A after reaction and are mixed at a rate of 10 mA-cm2Is charged to a voltage of more than 0.5V and the anode LiFePO4Loss of electrons to release Li+Generation of Li1- xFePO4Cathode PPy+PF6 -Obtaining electron emission PF6 -PPy was generated with a charge average voltage of 0.23V and a current efficiency of 99.5%. Analysis of the electrolyte in cell B revealed that it contained Li+、PF6 -And K+The amounts of (A) were 0.502, 0.511 and 0.010mmol, respectively, of the corresponding LiPF6The purity is as high as 99.49%.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (5)

1. The utility model provides a device based on high-purity lithium hexafluorophosphate is prepared in electrolysis of electrochemistry ion extraction method which characterized in that: the method comprises the following steps: an electrolytic bath A and an electrolytic bath B;
the electrolytic tank A is divided into an anode area and a cathode area by a cation exchange membrane, and the anode area comprises reversible de-intercalation PF6 -Anode made of compound and KPF6An electrolyte, the cathode region including reversibly deintercalated Li+A cathode composed of a compound and a lithium-containing solution;
the electrolytic cell B consists of an anode, an electrolyte and a cathode, wherein the anode and the cathode are respectively made of reversible Li extraction obtained after the electrolytic cell A is fully discharged+Compound and reversible deintercalation PF6 -Compound, the electrolyte is LiPF6And (3) solution.
2. The apparatus of claim 1, wherein: the electrode of the electrolytic cell A is reversibly inserted into and extracted from the corresponding PF6 -Compounds or reversible deintercalation of Li+The compound is respectively mixed with a conductive agent and a binder and then pressed into a film, and the film is pressed on the surface of a current collector after being dried to prepare a pairA corresponding reversible deintercalating compound electrode; or will reversibly de-intercalate the PF6 -Compounds or reversible deintercalation of Li+The compound is respectively mixed with a conductive agent and a binder to prepare slurry to be coated on the surface of a current collector, and the corresponding reversible deintercalation compound electrode is prepared.
3. The apparatus of claim 1, wherein: the reversible de-intercalation PF6 -The compound comprises: polyaniline, polypyrrole, polythiophene, polyparaphenylene, polytriphenylamine, or a carbon material; the reversible deintercalation of Li+The compound comprises: lithium manganate, lithium iron phosphate, lithium titanate, lithium cobaltate and nickel cobalt manganese ternary materials.
4. The apparatus of claim 1, wherein: the cation exchange membrane is a monovalent selective cation exchange membrane.
5. A method for preparing high-purity lithium hexafluorophosphate through electrolysis based on an electrochemical ion extraction method is characterized by comprising the following steps:
(1) in the electrolytic tank A, a cation exchange membrane is adopted to be divided into an anode area and a cathode area, and the anode area is reversibly inserted into PF6 -Compound as anode, KPF6For the anolyte, the cathodic region is used for reversible Li extraction+The compound is used as a cathode, a lithium-containing solution is used as a catholyte, and the system is subjected to discharge treatment to enable the PF to be reversibly deintercalated6 -PF for loss of electron capture by compound6 -Reversible deintercalation of Li+Obtaining of electron Capture Li from the Compound+，KPF6K in solution+The charge balance is maintained by the migration of the cation exchange membrane from the anode region to the cathode region, thus completing the PF6 -And Li+Extracting;
(2) in the electrolytic cell B, the anode and the cathode of the electrolytic cell A obtained in the step (1) are respectively used as the cathode and the anode, and LiPF is used6The solution is used as electrolyte, and the system is charged to reversibly insert and remove Li+Loss of electrons in compounds to release Li+Is reversibleDe-intercalation PF6 -Compound to obtain electron release PF6 -To complete LiPF6Generating;
(3) the steps (1) and (2) are alternately and circularly carried out to realize LiPF6The continuous preparation of (2).
CN202010180207.7A 2020-03-16 2020-03-16 Device and method for preparing high-purity lithium hexafluorophosphate through electrolysis by electrochemical ion extraction method Active CN111304679B (en)

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