CN114335649A - Method for preparing all-vanadium redox flow battery electrolyte and/or vanadyl sulfate crystal and triple-effect evaporation device - Google Patents
Method for preparing all-vanadium redox flow battery electrolyte and/or vanadyl sulfate crystal and triple-effect evaporation device Download PDFInfo
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Abstract
The invention belongs to the technical field of vanadium batteries, and particularly discloses a method for preparing electrolyte and/or vanadyl sulfate crystals of an all-vanadium redox flow battery and a triple-effect evaporation device, wherein the method comprises the following steps: the method comprises the following steps of sequentially carrying out extraction and back extraction on a tetravalent vanadium solution, and additionally arranging triple-effect evaporation concentration in at least one of the two stages before the extraction and after the back extraction, wherein the triple-effect evaporation concentration comprises the following steps: and (3) sequentially carrying out one-effect evaporation, two-effect evaporation and three-effect evaporation on the solution to be concentrated, and adjusting the flow rate, the steam consumption and the evaporation temperature of each stage of evaporation to finally obtain the vanadium battery electrolyte and/or vanadyl sulfate crystal, wherein the concentration of vanadium ions in the electrolyte is 1-7 mol/L. According to the method, the concentration of the electrolyte of the vanadium battery is high by combining the traditional extraction method with triple-effect evaporation, the prepared vanadyl sulfate crystal can be directly used for preparing the electrolyte of the vanadium battery, and the method is high in concentration efficiency, energy-saving, consumption-reducing and suitable for popularization and application.
Description
Technical Field
The invention belongs to the technical field of vanadium batteries, and particularly relates to a method for preparing electrolyte and/or vanadyl sulfate crystals of an all-vanadium redox flow battery and a triple-effect evaporation device.
Background
The energy storage is a key technology for improving the stable operation and consumption capability of new energy and realizing the targets of carbon peak reaching and carbon neutralization and double carbon. The all-vanadium redox flow battery energy storage system is developed for power grid level energy storage application, has the advantages of simple management, good monomer consistency, safe operation, independent design of power and capacity, long service life and the like, and has wide application prospects in the fields of new energy access, smart power grid construction and the like. The electrolyte is one of the key technologies of the all-vanadium redox flow battery, is a vanadium ion multivalent system, is an active substance for electrochemical reaction in the all-vanadium redox flow battery, and realizes the storage and release of energy.
At present, the methods for preparing the electrolyte for the all-vanadium redox flow battery mainly comprise a chemical reduction method, an electrolysis method and an extraction method. The chemical reduction method comprises dissolving vanadium oxide or compound in dilute sulfuric acid under heating, adding reducing agent such as oxalic acid and sulfur dioxide, heating under stirring to prepare VOSO4And (3) solution. The electrolytic method is to put the vanadium oxide or compound dissolved in dilute sulphuric acid into the cathode of an electrolytic cell, the anode is dilute sulphuric acid or sulphate solution, and direct current is applied to the anode and the cathode of the electrolytic cell to prepare the vanadium battery electrolyte through electrolysis. The raw material for producing the electrolyte by the chemical reduction method and the electrolytic method is high-purity vanadium pentoxide, the low-purity vanadium pentoxide can be prepared into the vanadium pentoxide with the purity of 99.9% by processes of vanadium precipitation purification or chlorination purification and the like, and the production process is high in energy consumption, medicament consumption and complex in process. The extraction method is characterized in that vanadium-containing solution is directly used for preparing vanadium battery electrolyte, various vanadium-containing solutions are used for removing impurities of the solutions through extraction, and then vanadium enrichment solution is obtained, but the vanadium enrichment solution has a difference relative to the concentration of the electrolyte for the all-vanadium redox flow battery, and further concentration and treatment are needed to obtain the electrolyte suitable for the all-vanadium redox flow battery and vanadyl sulfate crystals.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing all-vanadium redox flow battery electrolyte and/or vanadyl sulfate crystals and a triple-effect evaporation device, and aims to solve the problem that vanadium ions in a vanadium-enriched liquid obtained by the conventional extraction method are low in concentration and cannot be directly used as the all-vanadium redox flow battery electrolyte.
In order to achieve the above object, the present invention provides a method for preparing electrolyte of an all-vanadium flow battery and/or vanadyl sulfate crystals, comprising subjecting a tetravalent vanadium solution to an extraction process and a back-extraction process in sequence, and adding a triple-effect evaporation concentration process in at least one of the two stages before the extraction process and after the back-extraction process, wherein the triple-effect evaporation concentration process comprises the following steps:
and sequentially carrying out one-effect evaporation, two-effect evaporation and three-effect evaporation on the solution to be concentrated, and adjusting at least one parameter of the flow rate of the liquid entering each stage of evaporation, the steam consumption during each stage of evaporation and the evaporation temperature to finally obtain the electrolyte of the all-vanadium redox flow battery and/or vanadyl sulfate crystal, wherein the concentration of vanadium ions in the electrolyte of the all-vanadium redox flow battery is 1-7 mol/L.
Preferably, the tetravalent vanadium solution is directly obtained from a vanadium-containing raw material through a sulfation roasting-water leaching process, or is obtained through a sulfation roasting-water leaching process and chemical reduction sequentially.
Preferably, the triple-effect evaporation concentration process is arranged after the back extraction process, and in the solution to be concentrated, the concentration of vanadium ions is 0.1-2 mol/L, the concentration of sulfate ions is 0.1-5 mol/L, and the concentration of single impurity elements is less than or equal to 5 ppm.
Preferably, the impurities comprise at least one of aluminum, arsenic, calcium, chromium, magnesium, copper, iron, potassium, sodium, manganese, molybdenum, nickel, silicon, titanium, phosphorus, iridium, cobalt, platinum, lead, and nitrogen.
Preferably, the flow speed of the liquid to be concentrated when entering the single-effect evaporation is controlled to be 3m3/h～10m3The temperature is 10-50 ℃.
Preferably, the electrolyte is used for preparing the all-vanadium redox flow battery electrolyte, in the solution to be concentrated, the concentration of vanadium ions is 0.1-1 mol/L, and the concentration of sulfate ions is 0.1-1 mol/L;
the concentration of the concentrated solution after the first-effect evaporation is 1-3 mol/L, the concentration of the concentrated solution after the second-effect evaporation is 3-4 mol/L, and the concentration of the concentrated solution after the third-effect evaporation is 4-5 mol/L by respectively adjusting the steam dosage and temperature of the first-effect evaporation, the steam dosage and temperature of the second-effect evaporation, the steam dosage and temperature of the third-effect evaporation and the flow rate of the solution to be concentrated.
Preferably, the method is used for preparing vanadyl sulfate crystals, wherein in the solution to be concentrated, the concentration of vanadium ions is 0.1-2 mol/L, and the concentration of sulfate ions is 0.1-5 mol/L;
the concentration of the concentrated solution after the first-effect evaporation is 2-5 mol/L, the concentration of the concentrated solution after the second-effect evaporation is 5-7 mol/L, and the product after the third-effect evaporation is vanadyl sulfate crystal.
Preferably, the method is used for preparing the electrolyte of the all-vanadium redox flow battery and the vanadyl sulfate crystal, wherein in the solution to be concentrated, the concentration of vanadium ions is 0.1-1 mol/L, and the concentration of sulfate ions is 0.1-1 mol/L;
the concentration of the concentrated solution after the first-effect evaporation is 1-5 mol/L, the concentration of the concentrated solution after the second-effect evaporation is 5-7 mol/L, and the product after the third-effect evaporation is vanadyl sulfate crystal.
According to another aspect of the invention, the invention also provides a triple-effect evaporation device based on the method, which comprises a first-effect evaporator, a second-effect evaporator and a triple-effect evaporator which are connected in sequence, wherein discharge ports of the first-effect evaporator and the second-effect evaporator are respectively provided with a multi-channel interface for changing the flow direction of liquid after evaporation and concentration so as to prepare products with different specification concentrations.
Preferably, feed inlets of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are respectively connected with a flow peristaltic pump, and steam inlets of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are respectively connected with a control valve.
Generally, compared with the prior art, the above technical solution conceived by the present invention has the following beneficial effects:
(1) in the existing process for preparing the vanadium battery electrolyte by using the extraction method, a triple-effect evaporation concentration process is added in certain links of the process to improve the concentration of vanadium ions in the concentrated solution, so that an electrolyte product or vanadyl sulfate crystal meeting the requirements of the vanadium battery electrolyte is obtained, and the concentration efficiency is high.
(2) The vanadium enrichment solution obtained by the extraction and back extraction processes has high vanadium ion concentration and few impurities, and is subjected to triple-effect evaporation concentration, so that the obtained product can directly meet the requirements of the electrolyte required by the all-vanadium redox flow battery, the production efficiency is high, and the energy consumption is low.
(3) The invention is used for preparing the triple-effect evaporation device of the electrolyte of the all-vanadium redox flow battery and/or the vanadyl sulfate crystal, the interface of the discharge port is a multi-channel interface, the flow direction of the evaporated liquid can be freely changed according to the requirement, and products with different specifications can be prepared at the same time.
(4) The invention can independently adjust the steam dosage, temperature and liquid inlet flow rate of each stage of evaporator of the triple-effect evaporation device from the aspects of energy saving and product requirements, and can also perform combined adjustment of two stages of evaporators or three stages of evaporators, and the adjustment and control are more accurate and flexible.
Drawings
Fig. 1 is a flow chart of a preparation process of an electrolyte and vanadyl sulfate crystals of an all-vanadium redox flow battery provided by an embodiment of the invention.
Fig. 2 is a schematic structural diagram of a triple-effect evaporation device for preparing an electrolyte and/or vanadyl sulfate crystals of an all-vanadium flow battery according to an embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a method for preparing electrolyte of an all-vanadium redox flow battery and/or vanadyl sulfate crystals, which comprises the steps of sequentially carrying out an extraction process and a back extraction process on a tetravalent vanadium solution, and additionally arranging a triple-effect evaporation concentration process in at least one stage of the two stages before the extraction process and after the back extraction process, wherein the triple-effect evaporation concentration process comprises the following steps:
and sequentially carrying out one-effect evaporation, two-effect evaporation and three-effect evaporation on the solution to be concentrated, and adjusting at least one parameter of the flow rate of the liquid entering each stage of evaporation, the steam consumption during each stage of evaporation and the evaporation temperature to finally obtain the electrolyte of the all-vanadium redox flow battery and/or vanadyl sulfate crystals, wherein the concentration of vanadium ions in the electrolyte of the all-vanadium redox flow battery reaches 1-7 mol/L.
In some embodiments, the tetravalent vanadium solution may be a leaching solution containing tetravalent vanadium directly obtained after sulfating roasting-water leaching process of a vanadium-containing raw material; or the vanadium-containing raw material is subjected to sulfating roasting-water leaching process to obtain a leaching solution containing the pentavalent vanadium, and then the leaching solution containing the pentavalent vanadium is subjected to chemical reduction to obtain the vanadium-containing leaching solution.
Because the vanadium ion concentration in the tetravalent vanadium solution obtained by the traditional vanadium-containing raw material through a sulfating roasting-water leaching process or sequentially through the sulfating roasting-water leaching process and chemical reduction is low and impurities are more, the situation of 'mud and sand' easily occurs in the evaporation concentration process, so that the quality of an evaporation concentration product is influenced, the time and the energy consumption are long, in order to improve the concentration efficiency, improve the product quality, simplify the preparation flow and reduce the energy consumption, the triple-effect evaporation concentration process is arranged after the extraction and back-extraction process, in the to-be-concentrated solution to be subjected to triple-effect evaporation, the vanadium ion concentration should reach 0.1 mol/L-2 mol/L, the sulfate ion concentration should reach 0.1 mol/L-5 mol/L, and the concentration of a single impurity element is less than or equal to 5 ppm; the impurities may include any one or a combination of any several of aluminum, arsenic, calcium, chromium, magnesium, copper, iron, potassium, sodium, manganese, molybdenum, nickel, silicon, titanium, phosphorus, iron, cobalt, platinum, lead, and nitrogen. As shown in fig. 1, the concentration of vanadium ions, sulfate ions and impurity concentration in the vanadium-enriched liquid obtained after the back extraction are detected, and when the concentration of vanadium ions is 0.1-2 mol/L, the concentration of sulfate ions is 0.1-5 mol/L, and the concentration of a single impurity element is less than or equal to 5ppm, the vanadium-enriched liquid can be used as the liquid to be concentrated to carry out a triple-effect evaporation concentration process; if the conditions are not met, the extraction and back extraction processes are repeated until the concentration of vanadium ions and the concentration of impurities in the vanadium enrichment solution meet the conditions.
Specifically, when the all-vanadium redox flow battery electrolyte is prepared, the concentration of vanadium ions in a solution to be concentrated is 0.1-1 mol/L, the concentration of sulfate ions is 0.1-1 mol/L, and the concentration of a single impurity element is less than or equal to 5 ppm;
controlling the flow rate of qualified liquid to be concentrated to be 3m when the liquid enters the single-effect evaporation3/h～10m3The temperature is 10-50 ℃, and the amount of the introduced raw steam is 100-500 kg/h; the concentration of the concentrated solution after the first-effect evaporation is 1-3 mol/L, the concentration of the concentrated solution after the second-effect evaporation is 3-4 mol/L, and the concentration of the concentrated solution after the third-effect evaporation is 4-5 mol/L by respectively adjusting the steam dosage and temperature of the first-effect evaporation, the steam dosage and temperature of the second-effect evaporation, the steam dosage and temperature of the third-effect evaporation and the flow rate of the solution to be concentrated.
When vanadyl sulfate crystals are prepared, in a solution to be concentrated, the concentration of vanadium ions should reach 0.1-2 mol/L, the concentration of sulfate ions should reach 0.1-5 mol/L, and the concentration of a single impurity element is less than or equal to 5 ppm;
controlling the flow rate of qualified liquid to be concentrated to be 3m when the liquid enters the single-effect evaporation3/h～10m3The temperature is 10-50 ℃, and the amount of the introduced raw steam is 300-1000 kg/h; the concentrated solution after the first-effect evaporation is enabled to be obtained by respectively adjusting the steam dosage and temperature of the first-effect evaporation, the steam dosage and temperature of the second-effect evaporation, the steam dosage and temperature of the third-effect evaporation and the flow rate of the solution to be concentratedThe concentration is 2-5 mol/L, the concentration of the concentrated solution after the two-effect evaporation is 5-7 mol/L, and the product after the three-effect evaporation is vanadyl sulfate crystal.
When the electrolyte of the all-vanadium redox flow battery and the vanadyl sulfate crystal are prepared, in a solution to be concentrated, the concentration of vanadium ions should reach 0.1-1 mol/L, the concentration of sulfate ions should reach 0.1-1 mol/L, and the concentration of a single impurity element is less than or equal to 5 ppm;
referring to FIG. 1, the flow rate of qualified liquid to be concentrated is controlled to be 3m when entering the single-effect evaporation3/h～10m3The temperature is 10-50 ℃, and the amount of the introduced raw steam is 300-1000 kg/h; the concentration of the concentrated solution after the first-effect evaporation is 1-5 mol/L, the concentration of the concentrated solution after the second-effect evaporation is 5-7 mol/L, and the product after the third-effect evaporation is vanadyl sulfate crystal.
The vanadyl sulfate crystal prepared by the method is dissolved in water, can also be used for preparing all-vanadium redox flow battery electrolyte, and has high purity and low impurity content.
As shown in fig. 2, the invention also provides a triple-effect evaporation device based on the method for preparing the electrolyte of the all-vanadium redox flow battery and/or the vanadyl sulfate crystal, which comprises a first-effect evaporator, a second-effect evaporator and a triple-effect evaporator which are sequentially connected, wherein each stage of evaporator is provided with a feeding hole, a discharging hole, a steam inlet and a steam outlet. The feed inlet of the first-effect evaporator is communicated with a to-be-concentrated liquid conveying pipeline; the feed inlet of the second-effect evaporator is communicated with the discharge outlet of the first-effect evaporator through a pipeline and is also communicated with a to-be-concentrated liquid conveying pipeline; the feed inlet of the triple-effect evaporator is communicated with the discharge outlet of the double-effect evaporator through a pipeline and is also communicated with a to-be-concentrated liquid conveying pipeline. The steam inlet of the first-effect evaporator is used for introducing raw steam or recycled secondary steam, the steam outlet of the first-effect evaporator is communicated with the steam inlet of the second-effect evaporator, the steam outlet of the second-effect evaporator is communicated with the steam inlet of the third-effect evaporator, and the secondary steam coming out of the steam outlet of the third-effect evaporator can be recycled.
In some embodiments, the discharge ports of the first-effect evaporator and the second-effect evaporator are provided with multi-channel interfaces, that is, the discharge ports of the first-effect evaporator and the second-effect evaporator are respectively communicated with a plurality of pipelines, and the multi-channel interfaces can be specifically multi-channel flanges and used for changing the flow direction of the liquid after evaporation and concentration so as to prepare products with different specification concentrations. Specifically, a discharge port of the first-effect evaporator is communicated with a feed port of the second-effect evaporator and a first-effect product outlet through a multi-channel flange; the discharge hole of the second-effect evaporator is communicated with the feed hole of the third-effect evaporator and the outlet of the second-effect product through a multi-channel flange; the discharge port of the triple-effect evaporator is the outlet of the triple-effect product.
In some embodiments, the front ends of the feed inlets of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are respectively connected with a flow peristaltic pump for independently adjusting the liquid inlet flow rate of each stage of evaporator. Control valves are arranged on the liquid conveying pipeline to be concentrated, which is communicated with the feed inlet of the second-effect evaporator, and the liquid conveying pipeline to be concentrated, which is communicated with the feed inlet of the third-effect evaporator, and are used for respectively adjusting the adding amount of the liquid to be concentrated in the second-effect evaporator and the third-effect evaporator. The front ends of the steam inlets of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are respectively connected with a control valve for independently adjusting the steam flow entering each stage of evaporator, and the temperature in each stage of evaporator can be adjusted by adjusting the steam consumption of each stage of evaporator and the proportion of raw steam and secondary steam. Preferably, each evaporator is internally provided with a thermometer, so that the evaporation temperature can be accurately adjusted.
Specifically, when the concentration of vanadium ions in the product outlet concentrated solution of a certain stage of evaporator is greater than the required electrolyte product concentration, the steam consumption of the stage of evaporator can be reduced, the evaporation temperature is reduced, the liquid flow rate entering the stage of evaporator is increased, or the original to-be-concentrated solution (aiming at the second-effect evaporator and the third-effect evaporator) is added until the concentration of the product outlet concentrated solution is adjusted to reach the required concentration. When the concentration of vanadium ions in the product outlet concentrated solution of a certain stage of evaporator is less than the required concentration of electrolyte product, the steam dosage of the stage of evaporator can be increased, the evaporation temperature is increased, or the flow rate of liquid entering the stage of evaporator is reduced until the concentration of the product outlet concentrated solution is adjusted to reach the required concentration.
Preferably, the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are made of materials resistant to corrosion of strong acid and strong base.
In conclusion, the three-effect evaporation and concentration process is introduced in the process of preparing the vanadium redox flow battery electrolyte by the extraction method, so that the concentration of the vanadium redox flow battery electrolyte is improved, the production efficiency is high, and the energy is saved and the consumption is reduced.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A method for preparing electrolyte and/or vanadyl sulfate crystals of an all-vanadium flow battery is characterized by comprising the steps of sequentially carrying out an extraction process and a back-extraction process on a tetravalent vanadium solution, and additionally arranging a triple-effect evaporation concentration process in at least one of the two stages before the extraction process and after the back-extraction process, wherein the triple-effect evaporation concentration process comprises the following steps:
and sequentially carrying out one-effect evaporation, two-effect evaporation and three-effect evaporation on the solution to be concentrated, and adjusting at least one parameter of the flow rate of the liquid entering each stage of evaporation, the steam consumption during each stage of evaporation and the evaporation temperature to finally obtain the electrolyte of the all-vanadium redox flow battery and/or vanadyl sulfate crystal, wherein the concentration of vanadium ions in the electrolyte of the all-vanadium redox flow battery is 1-7 mol/L.
2. The method of claim 1, wherein: the tetravalent vanadium solution is directly obtained by a vanadium-containing raw material through a sulfating roasting-water leaching process, or is obtained through the sulfating roasting-water leaching process and chemical reduction in sequence.
3. The method of claim 1, wherein: the triple-effect evaporation concentration process is arranged after the back extraction process, and in the solution to be concentrated, the concentration of vanadium ions is 0.1-2 mol/L, the concentration of sulfate ions is 0.1-5 mol/L, and the concentration of a single impurity element is less than or equal to 5 ppm.
4. The method of claim 3, wherein: the impurities include at least one of aluminum, arsenic, calcium, chromium, magnesium, copper, iron, potassium, sodium, manganese, molybdenum, nickel, silicon, titanium, phosphorus, iron, cobalt, platinum, lead, and nitrogen.
5. The method of claim 3, wherein: controlling the flow speed of the solution to be concentrated to be 3m when the solution enters the one-effect evaporation3/h～10m3The temperature is 10-50 ℃.
6. The method of claim 5, wherein: the electrolyte is used for preparing the all-vanadium redox flow battery electrolyte, and in the solution to be concentrated, the concentration of vanadium ions is 0.1-1 mol/L, and the concentration of sulfate ions is 0.1-1 mol/L;
the concentration of the concentrated solution after the first-effect evaporation is 1-3 mol/L, the concentration of the concentrated solution after the second-effect evaporation is 3-4 mol/L, and the concentration of the concentrated solution after the third-effect evaporation is 4-5 mol/L by respectively adjusting the steam dosage and temperature of the first-effect evaporation, the steam dosage and temperature of the second-effect evaporation, the steam dosage and temperature of the third-effect evaporation and the flow rate of the solution to be concentrated.
7. The method of claim 5, wherein: the method is used for preparing vanadyl sulfate crystals, and in the solution to be concentrated, the concentration of vanadium ions is 0.1-2 mol/L, and the concentration of sulfate ions is 0.1-5 mol/L;
the concentration of the concentrated solution after the first-effect evaporation is 2-5 mol/L, the concentration of the concentrated solution after the second-effect evaporation is 5-7 mol/L, and the product after the third-effect evaporation is vanadyl sulfate crystal.
8. The method of claim 5, wherein: the method is used for preparing all-vanadium redox flow battery electrolyte and vanadyl sulfate crystals, wherein in the solution to be concentrated, the concentration of vanadium ions is 0.1-1 mol/L, and the concentration of sulfate ions is 0.1-1 mol/L;
the concentration of the concentrated solution after the first-effect evaporation is 1-5 mol/L, the concentration of the concentrated solution after the second-effect evaporation is 5-7 mol/L, and the product after the third-effect evaporation is vanadyl sulfate crystal.
9. A triple effect evaporation plant based on the method according to any one of claims 1 to 8, characterized in that: the device comprises a first-effect evaporator, a second-effect evaporator and a third-effect evaporator which are sequentially connected, wherein a discharge hole of the first-effect evaporator and a discharge hole of the second-effect evaporator are respectively provided with a multi-channel interface for changing the flow direction of liquid after evaporation concentration so as to prepare products with different specification concentrations.
10. A triple effect evaporation device according to claim 9, wherein: the feed inlets of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are respectively connected with a flow peristaltic pump, and the steam inlets of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are respectively connected with a control valve.
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