CN112234238B - Method for preparing iron-chromium redox battery electrolyte - Google Patents

Method for preparing iron-chromium redox battery electrolyte Download PDF

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CN112234238B
CN112234238B CN202011490257.1A CN202011490257A CN112234238B CN 112234238 B CN112234238 B CN 112234238B CN 202011490257 A CN202011490257 A CN 202011490257A CN 112234238 B CN112234238 B CN 112234238B
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iron
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chromium
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Zhonghai Energy Storage Technology Beijing Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/18—Regenerative fuel cells, e.g. redox flow batteries or secondary fuel cells
    • H01M8/184—Regeneration by electrochemical means
    • H01M8/188—Regeneration by electrochemical means by recharging of redox couples containing fluids; Redox flow type batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0002—Aqueous electrolytes
    • H01M2300/0005—Acid electrolytes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Abstract

The invention provides a method for preparing an electrolyte of a ferro-chromium redox battery, which comprises the following operations: 1) dissolving an iron-containing material in hydrochloric acid, wherein the concentration of the hydrochloric acid is 0.1-0.5 mol/L, inserting an electrode into the solution, setting the electrode as a negative electrode, and introducing current for electrolysis; 2) adding chromium chloride and hydrochloric acid into a reaction container under the condition of isolating air, and starting stirring in the process of adding chromium chloride; 3) after the chromium chloride is completely dissolved, mixing the negative electrode solution obtained by the electrolysis in the step 1) with the solution obtained in the step 2). The preparation method of the iron-chromium redox battery electrolyte provided by the invention can utilize industrial wastes as raw materials for electrolysis, such as red mud and the like, and remove impurities which cannot be dissolved in the electrolyte from the red mud through constant current electrolysis, thereby not only digesting the industrial wastes, but also obtaining the cheap electrolyte.

Description

Method for preparing iron-chromium redox battery electrolyte
Technical Field
The invention belongs to the technical field of energy storage, and particularly relates to a preparation method and a preparation system of an electrolyte of a flow battery.
Background
When the concept of the liquid flow energy storage battery is put forward for the first time, Cr is utilized3+/Cr2+Electric centering of Cr2+Reducing property and Fe3+/Fe2 +Electric centering of Fe3+In acidic Cr separated by a proton exchange membrane3+Electrolyte and acidic Fe2+Carrying out electrochemical oxidation-reduction reaction in the electrolyte. With the increasing progress of flow battery technology, researchers have realized that the positive electrode Fe3+/Fe2+Cr for electric pair and negative electrode3+/Cr2+The couple is difficult to be completely separated, the diaphragm cannot completely isolate the permeation of iron ions, iron can be diffused to the negative electrode, if ferric iron exists, the deposited catalyst can be oxidized and dissolved in the solution, so that the resistance of the battery is increased, and even the capacity of the battery is lost. Therefore, in the technology developed in recent years, the iron salt and the chromium salt are mostly dissolved together in the electrolyte of the iron-chromium battery, so that the problem of cross contamination of the electrolyte is solved.
Patent CN201810213408.5 proposes an iron-chromium flow battery, an electrolyte solution, a preparation device and a preparation method thereof, wherein hydrochloric acid (with the concentration of 1-4M) is dissolved, EDTA and CrCl are added3(concentration 0-1.6M) and ammonium sulfate at 80-90 deg.C, dissolving, and adding another half of hydrochloric acid and FeCl2(concentration 0-2M). The patent CN201911169592.9 discloses an iron-chromium flow battery electrolyte and a technology provided by the application thereof, which is an electrolyte prepared by directly preparing Fe0.5-2M, Cl ions of 1.5-12M and 0.5M NaCL. Patent CN201911169625.X proposes an iron-chromium flow battery electrolyte containing a composite additive and application thereof, wherein lead and bismuth are used as the composite additive. The above-mentioned techniques are all directly prepared from iron salt and chromium salt, and their cost is still high, although they have the advantages of convenient operation and high product purity.
In nature, iron exists in the forms of ferric oxide, ferroferric oxide and the like, and some iron is industrial waste. The ferric salt in the form is very stable and low in price, and should be brought into the category of raw materials of the iron-chromium battery electrolyte, so that the cost of the electrolyte is reduced.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the preparation method of the iron-chromium redox flow battery electrolyte with simple flow, high efficiency, environmental protection and low cost, and the battery performance and capacity of the iron-chromium redox flow battery are improved.
A second object of the present invention is to provide a system for preparing an electrolyte for a ferrochrome redox cell.
The technical scheme for realizing the above purpose of the invention is as follows:
a method of making an iron-chromium redox cell electrolyte comprising the acts of:
1) dissolving an iron-containing material in hydrochloric acid, wherein the concentration of the hydrochloric acid is 0.1-0.5 mol/L, inserting an electrode into the solution, setting the electrode as a negative electrode, and introducing current for electrolysis;
2) adding chromium chloride and hydrochloric acid into a reaction container under the condition of isolating air, and starting stirring in the process of adding chromium chloride;
3) after the chromium chloride is completely dissolved, mixing the negative electrode solution obtained by the electrolysis in the step 1) with the solution obtained in the step 2).
Wherein in the step 1), the iron-containing material is ferric oxide, ferroferric oxide, ferric hydroxide, ferrous hydroxide, red mud and FeCl3One or more of; and/or
The electrode is an iron sheet electrode.
In the step 1), the electrolytic anode solution is 0.1-0.5 mol/L hydrochloric acid, and the anode electrode is iron; an electrode was inserted into the solution and the open circuit voltage was measured, and the energization time was determined based on the open circuit voltage.
Preferably, in the step 1), 0.1-0.5 mol/L sodium chloride is further added into the electrolyzed positive electrode solution. And/or
The iron-containing material is ferroferric oxide or a combination of the ferroferric oxide and red mud 5 (0.1-3).
Through electrolysis tests, it is found that sufficient iron ion concentration cannot be obtained by completely using the red mud, and the ferroferric oxide and the red mud are preferably used together.
The invention adopts a preferable technical scheme that the step 1) adopts constant current electrolysis, and the current density is set to be 0.1-0.5A/cm2And (4) when the voltage of the cell is electrified to be-0.2 to-0.4V, using the negative electrode solution in the step 3).
The time of electrolysis is necessarily predetermined by calculation. If the open-circuit voltage is 0.77V, the power-on time is
T=
Figure DEST_PATH_IMAGE001
(hours) (1)
Wherein C is the concentration mol/L of iron ions in the cathode electrolyte, V is the volume (L) of the cathode electrolyte, and I is the current density A/cm2A is the electrode area cm2。
If the iron ions in the raw material are not completely trivalent, the electrifying time is reduced in proportion. For example, when the open circuit voltage is 0.4V, the energization time is T (0.77-0.4)/0.77 hours.
Further, filtering the negative electrode solution obtained by electrolysis, and mixing the negative electrode solution with the solution obtained in the step 2); the filtration is carried out under the gas protection condition, and the filter screen is a wire mesh.
Wherein, the concentration of the hydrochloric acid in the step 2) is 2-4 mol/L, and the chromium chloride is added to ensure that the concentration of the chromium chloride is 1.2-2.0 mol/L.
The method for preparing the iron-chromium redox battery electrolyte adopts a system comprising an electrolytic bath, a filter and a reaction kettle,
the electrolytic cell comprises an anode chamber and a cathode chamber, the anode chamber and the cathode chamber are separated by an ion selective membrane, the anode and the cathode are both iron sheet electrodes, and the distance between the iron sheet electrodes and the bottom of the electrolytic cell is 1/2-1/3 of the height of the electrolytic cell;
the negative electrode chamber is connected with a filter through a pipeline, the filter is connected with a buffer tank through a pipeline, and the buffer tank is connected with the reaction kettle.
Because the electrolytic bath contains more solid slag, the electrode plates are at a certain height from the bottom.
Further, a slag outlet is formed at the bottom of the negative electrode chamber; and/or
Protective gas is introduced into the filter and the buffer tank, and the protective gas is one or more of nitrogen, argon and carbon dioxide.
More preferably, the bottom of the negative chamber is inclined to the slag outlet.
The system has the preferred scheme that the distance between the anode and the cathode is 1-10 cm.
The invention has the beneficial effects that:
the preparation method of the iron-chromium redox battery electrolyte provided by the invention can utilize industrial wastes as raw materials for electrolysis, such as red mud and the like, and remove impurities which cannot be dissolved in the electrolyte from the red mud through constant current electrolysis, thereby not only digesting the industrial wastes, but also obtaining the cheap electrolyte.
The system for preparing the iron-chromium redox battery electrolyte adopts conventional industrial facilities, takes iron as an electrode, and does not introduce other metal ions; and a waste residue outlet and a filtering device are arranged, so that the purity of the electrolyte is ensured.
Drawings
Fig. 1 is a system for preparing an electrolyte for a ferrochrome redox cell of the present invention.
In the figure, 1 is a reaction vessel, 2 is an electrolyte storage tank, 3 is a filter, 4 is a buffer tank, 5 is an electrolytic bath, 501 is a slag outlet, 502 is a negative electrode, and 503 is a positive electrode.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the examples, the technical means used are all the technical means existing in the field, unless otherwise specified.
Example 1
Referring to fig. 1, the present embodiment provides a system for preparing an electrolyte of an iron-chromium redox cell, comprising an electrolytic cell 5, a filter 3, a reaction kettle 1,
the electrolytic cell 5 comprises a positive electrode chamber and a negative electrode chamber, the positive electrode chamber and the negative electrode chamber are separated by an ion selective membrane, the positive electrode 503 and the negative electrode 502 are both iron sheet electrodes, and the distance between the iron sheet electrodes and the bottom is 1/3 height of the electrolytic cell;
the negative electrode chamber is connected with a filter 3 through a pipeline, the filter 3 is connected with a buffer tank 4 through a pipeline, and the buffer tank 4 is connected with the reaction kettle 1. The reaction kettle 1 is connected with an electrolyte storage tank 2.
A slag outlet 501 is arranged at the bottom of the negative electrode chamber; the bottom of the negative electrode chamber is an inclined plane which is inclined to the direction of the slag outlet. In this embodiment, the outlet for the negative electrolyte is located at the level of the bottom of the electrode (i.e. at the level of 1/3 of the cell) to avoid the discharge of solid sludge.
And nitrogen is introduced into the filter and the buffer tank. The outlet pipeline of the filter is provided with a backflow branch, and secondary filtration is carried out when the quality of the filtrate does not reach the standard.
In this example, the distance between the positive electrode and the negative electrode was 5 cm.
Test example 1
The embodiment provides a preparation method of an iron-chromium redox battery electrolyte, which comprises the steps of adopting an electrolytic cell in the system in the embodiment 1, putting alumina red mud into a negative electrode chamber, wherein the mass ratio of the red mud to 0.2mol/L hydrochloric acid is about 1:1, and putting 0.2mol/L hydrochloric acid and 0.1mol/L sodium chloride into a positive electrode chamber to improve the conductivity; the electrode was inserted and connected to an electrochemical workstation, at which time the open circuit voltage was 0.77V.
Setting the current density to 0.2A/cm2And (4) carrying out constant current electrolysis until gas escapes from the negative electrode, stopping electrolysis, and detecting the concentration of iron ions in the electrolyte of the negative electrode by a titration method, wherein the concentration of the iron ions is 0.2 mol/L.
Test example 2
By adopting the method of test example 1, alumina red mud and ferroferric oxide are put into a negative electrode chamber, the mass ratio of the total mass of the red mud and the ferroferric oxide to 0.2mol/L hydrochloric acid is about 1:1, the mass ratio of the red mud to the ferroferric oxide is 5:3, and 0.2mol/L hydrochloric acid and 0.1mol/L sodium chloride are put into a positive electrode chamber to improve the conductivity type; the electrode was inserted and connected to an electrochemical workstation, at which time the open circuit voltage was 0.77V.
Setting the current density to 0.2A/cm2And (4) carrying out constant current electrolysis until gas escapes from the negative electrode, stopping electrolysis, and detecting the concentration of iron ions in the electrolyte of the negative electrode by a titration method, wherein the concentration of the iron ions is 3.1 mol/L.
According to the results of test example 2, C in the formula (1) was 3.1 mol/L.
Example 2:
a method of preparing an iron-chromium redox cell electrolyte using the system of example 1 comprising the acts of:
1) dissolving an iron-containing material in hydrochloric acid, wherein the concentration of the hydrochloric acid is 0.2mol/L, inserting an electrode into the solution, setting the electrode as a negative electrode, and introducing current for electrolysis; the iron-containing material is ferroferric oxide and red mud, the mass ratio of the ferroferric oxide to the red mud is 5:3, the mass ratio of the total mass of the red mud and the ferroferric oxide to 0.2mol/L hydrochloric acid is about 1:1,
the electrolytic anode solution is 0.2mol/L hydrochloric acid and 0.1mol/L sodium chloride;
the electrode is an iron electrode. Constant current electrolysis is adopted, and the current density is set to be 0.2A/cm2The energization time was calculated according to the equation (1) and the energization was stopped until the cell voltage was about-0.4V.
And after the negative electrode electrolyte is discharged, discharging waste residues from the slag outlet.
2) Adding chromium chloride and hydrochloric acid into a reaction container under the condition of isolating air, and starting stirring in the process of adding chromium chloride; wherein the concentration of the hydrochloric acid is 4mol/L, and the chromium chloride is added to ensure that the concentration of the chromium chloride is 3.0 mol/L.
3) After the chromium chloride is completely dissolved, mixing the negative electrode solution obtained by the electrolysis in the step 1) with the solution obtained in the step 2) in equal volume.
Filtering the negative electrode solution obtained by electrolysis, and mixing the negative electrode solution with the solution obtained in the step 2); the filtration is carried out under the gas protection condition, and the filter screen is a wire mesh.
Through detection, the concentrations of iron ions and Cr ions in the electrolyte prepared in the embodiment are both 1.5 mol/L, and no detectable impurities exist in the electrolyte.
Example 3
This example presents a method for preparing an electrolyte for a ferrochrome redox cell using the system of example 1, comprising the operations of:
1) dissolving an iron-containing material in hydrochloric acid, wherein the concentration of the hydrochloric acid is 0.2mol/L, inserting an electrode into the solution, setting the electrode as a negative electrode, and introducing current for electrolysis; the material containing iron is ferroferric oxide, the mass ratio of the ferroferric oxide to 0.2mol/L hydrochloric acid is about 30:100,
the electrolytic anode solution is 0.2mol/L hydrochloric acid and 0.1mol/L sodium chloride;
the electrode is an iron electrode. Constant current electrolysis is adopted, and the current density is set to be 0.2A/cm2The energization time was calculated according to the equation (1) and the energization was stopped until the cell voltage was about-0.4V.
2) Adding chromium chloride and hydrochloric acid into a reaction container under the condition of isolating air, and starting stirring in the process of adding chromium chloride; wherein the concentration of the hydrochloric acid is 4mol/L, and the chromium chloride is added to ensure that the concentration of the chromium chloride is 3.0 mol/L.
3) After the chromium chloride is completely dissolved, mixing the negative electrode solution obtained by the electrolysis in the step 1) with the solution obtained in the step 2) in equal volume.
Filtering the negative electrode solution obtained by electrolysis, and mixing the negative electrode solution with the solution obtained in the step 2); the filtration is carried out under the gas protection condition, and the filter screen is a wire mesh.
Through detection, in the electrolyte prepared in the embodiment, the concentration of iron ions is 1.5 mol/L, the concentration of Cr ions is 1.5 mol/L, and no detectable impurity exists in the electrolyte.
Example 4
This example presents a method for preparing an electrolyte for a ferrochrome redox cell using the system of example 1, comprising the operations of:
1) dissolving an iron-containing material in hydrochloric acid, wherein the concentration of the hydrochloric acid is 0.2mol/L, inserting an electrode into the solution, setting the electrode as a negative electrode, and introducing current for electrolysis; the iron-containing material is ferroferric oxide and red mud, the mass ratio of the ferroferric oxide to the red mud is 5:2, and the mass ratio of the total mass of the red mud and the ferroferric oxide to 0.2mol/L hydrochloric acid is about 1: 1.2;
the electrolytic anode solution is 0.2mol/L hydrochloric acid and 0.1mol/L sodium chloride;
the electrode is an iron electrode. Constant current electrolysis is adopted, and the current density is set to be 0.2A/cm2The energization time was calculated according to the equation (1) and the energization was stopped until the cell voltage was about-0.4V.
2) Adding chromium chloride and hydrochloric acid into a reaction container under the condition of isolating air, and starting stirring in the process of adding chromium chloride; wherein the concentration of the hydrochloric acid is 4mol/L, and the chromium chloride is added to ensure that the concentration of the chromium chloride is 3.0 mol/L.
3) After the chromium chloride is completely dissolved, mixing the negative electrode solution obtained by the electrolysis in the step 1) with the solution obtained in the step 2) in equal volume.
Filtering the negative electrode solution obtained by electrolysis, and mixing the negative electrode solution with the solution obtained in the step 2); the filtration is carried out under the gas protection condition, and the filter screen is a wire mesh.
Through detection, the electrolyte prepared in the embodiment has the concentration of iron ions of 1.6 mol/L and the concentration of Cr ions of 1.5 mol/L, and has no detectable impurities.
Although the present invention has been described in the foregoing by way of examples, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.

Claims (7)

1. A method of preparing an electrolyte for an iron-chromium redox cell, comprising the acts of:
1) dissolving an iron-containing material in hydrochloric acid, wherein the concentration of the hydrochloric acid is 0.1-0.5 mol/L, inserting an electrode into the solution, setting the electrode as a negative electrode, and introducing current for electrolysis; 0.1-0.5 mol/L sodium chloride is also added into the electrolytic anode solution; the iron-containing material is ferroferric oxide or a combination of the ferroferric oxide and red mud 5 (0.1-3);
2) adding chromium chloride and hydrochloric acid into a reaction container under the condition of isolating air, and starting stirring in the process of adding chromium chloride;
3) after the chromium chloride is completely dissolved, mixing the negative electrode solution obtained by the electrolysis in the step 1) with the solution obtained in the step 2);
the system for preparing the iron-chromium redox battery electrolyte comprises an electrolytic bath, a filter and a reaction kettle,
the electrolytic cell comprises an anode chamber and a cathode chamber, the anode chamber and the cathode chamber are separated by an ion selective membrane, the anode and the cathode are both iron sheet electrodes, and the distance between the iron sheet electrodes and the bottom of the electrolytic cell is 1/2-1/3 of the height of the electrolytic cell;
the negative electrode chamber is connected with a filter through a pipeline, the filter is connected with a buffer tank through a pipeline, and the buffer tank is connected with the reaction kettle.
2. The method for preparing the electrolyte of the iron-chromium redox battery according to claim 1, wherein in the step 1), the electrolytic solution of the positive electrode is 0.1-0.5 mol/L hydrochloric acid, and the electrode of the positive electrode is iron; an electrode was inserted into the solution and the open circuit voltage was measured, and the energization time was determined based on the open circuit voltage.
3. The method for preparing the electrolyte of the iron-chromium redox battery according to claim 1, wherein the step 1) adopts constant current electrolysis, and the current density is set to be 0.1-0.5A/cm2And (4) when the voltage of the cell is electrified to be-0.2 to-0.4V, using the negative electrode solution in the step 3).
4. The method for preparing the electrolyte of the iron-chromium redox battery according to any one of claims 1 to 3, wherein the solution of the negative electrode obtained by electrolysis is filtered and then mixed with the solution obtained in the step 2); the filtration is carried out under the gas protection condition, and the filter screen is a wire mesh.
5. A method for preparing an iron-chromium redox battery electrolyte as claimed in any one of claims 1 to 3 wherein the hydrochloric acid concentration in step 2) is 2 to 4mol/L and chromium chloride is added to give a chromium chloride concentration of 1.2 to 2.0 mol/L.
6. The method of claim 1 wherein the cathode compartment has a tap hole at the bottom; and/or
Protective gas is introduced into the filter and the buffer tank, and the protective gas is one or more of nitrogen, argon and carbon dioxide.
7. The method of claim 1 or 6, wherein the distance between the positive electrode and the negative electrode is 1-10 cm, and/or
The anode chamber and/or the cathode chamber are/is connected with an external cathode liquid tank or an external anode liquid tank.
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