CN119898815A - A method and device for preparing high-purity potassium metavanadate by short-process sodium vanadate - Google Patents
A method and device for preparing high-purity potassium metavanadate by short-process sodium vanadate Download PDFInfo
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- CN119898815A CN119898815A CN202510089671.8A CN202510089671A CN119898815A CN 119898815 A CN119898815 A CN 119898815A CN 202510089671 A CN202510089671 A CN 202510089671A CN 119898815 A CN119898815 A CN 119898815A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/16—Evaporating by spraying
- B01D1/18—Evaporating by spraying to obtain dry solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D25/00—Filters formed by clamping together several filtering elements or parts of such elements
- B01D25/12—Filter presses, i.e. of the plate or plate and frame type
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
- B01D5/006—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D9/00—Crystallisation
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- B01D9/0031—Evaporation of components of the mixture to be separated by heating
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
本发明公开了一种钒酸钠短流程制备高纯偏钒酸钾的方法及装置，包括下述步骤：1）按钾离子和钒的摩尔比为0.34～1.0将钒酸钠溶液和硫酸钾混合，加入浓硫酸至pH值为1.9～2.5，在90～100℃反应、结晶，分离，得到多钒酸钾固体；2）按钾离子和钒的摩尔比为0.5～1.0将多钒酸钾固体加入氢氧化钾溶液中，加热升温至80～100℃进行消解反应，得到偏钒酸钾溶液。本发明以钠化焙烧浸出的钒酸钠溶液为原料短流程制备偏钒酸钾，制备过程中不产生还原性气体NH3和低价钒，改变偏钒酸钾析出过程，能制备出粒度均匀，流动性好的球状偏钒酸钾固体颗粒，提高偏钒酸钾结晶过程稳定性和钒回收率，所得偏钒酸钾产品纯度大于99.5wt%、钒回收率大于99%。
The invention discloses a method and device for preparing high-purity potassium metavanadate from sodium vanadate in a short process, comprising the following steps: 1) mixing a sodium vanadate solution and potassium sulfate according to a molar ratio of potassium ions to vanadium of 0.34 to 1.0, adding concentrated sulfuric acid to a pH value of 1.9 to 2.5, reacting, crystallizing, and separating at 90 to 100°C to obtain a potassium polyvanadate solid; 2) adding a potassium polyvanadate solid to a potassium hydroxide solution according to a molar ratio of potassium ions to vanadium of 0.5 to 1.0, heating to 80 to 100°C for digestion reaction, and obtaining a potassium metavanadate solution. The invention uses a sodium vanadate solution leached by sodiumization roasting as a raw material to prepare potassium metavanadate in a short process, does not generate reducing gas NH 3 and low-valent vanadium during the preparation process, changes the precipitation process of potassium metavanadate, can prepare spherical potassium metavanadate solid particles with uniform particle size and good fluidity, improves the stability of the potassium metavanadate crystallization process and the vanadium recovery rate, and the obtained potassium metavanadate product has a purity of more than 99.5wt% and a vanadium recovery rate of more than 99%.
Description
Technical Field
The invention belongs to the technical field of fine chemical engineering, and particularly relates to a method and a device for preparing high-purity potassium metavanadate through a sodium vanadate short process.
Background
Potassium metavanadate, english name Potassium metavanadate, molecular formula KVO 3, is widely used in the fields of glaze, chemical catalyst, medical treatment, etc. At present, the production process of potassium metavanadate comprises a solid-phase melting method and an alkali dissolution crystallization method, wherein the solid-phase melting method is to mix and heat ammonium polyvanadate ((NH 4)2V6O16), ammonium metavanadate (NH 4VO3) or vanadium pentoxide (V 2O5) and potassium carbonate (K 2CO3) according to stoichiometric ratio to a molten state, cool and recrystallize in an aqueous medium system to obtain KVO 3.
In the above method, the raw material V 2O5 is mainly prepared from (NH 4)2V6O16 or NH 4VO3) through calcination deamination, and one inherent disadvantage of the method is that ammonium polyvanadate or ammonium metavanadate is decomposed to obtain NH 3 and V 2O5,NH3 as reducing agents at 550 ℃ to reduce a small amount of V 2O5 into low-valence vanadium oxide.
Similarly, (NH 4)2V6O16 or NH 4VO3 is used as a raw material, a large amount of NH 3 is decomposed in the alkali dissolution process, a small amount of NH4 + remained in the potassium metavanadate solution is combined with metavanadate, and is separated out along with potassium metavanadate crystallization, so that the nitrogen impurity content in the potassium metavanadate product exceeds the standard.
Another disadvantage is that, due to the large solubility and supersaturation of potassium metavanadate, crystal seeds are added in the cooling crystallization process to promote potassium metavanadate crystallization, and the high-concentration potassium metavanadate crystallization mother liquor is returned to the alkali dissolution tank for recycling, so that the dissolution rate of solid-phase vanadium raw materials is reduced and impurities in the potassium metavanadate solution are accumulated, and the production efficiency and the product quality are affected.
In recent years, aiming at the problems existing in the above-mentioned process, the improvement process is proposed by the domestic scientific workers. For example, publication No. CN108975398A provides a high density potassium metavanadate and a method for preparing the same, wherein H 2O2 solution is added in the process of heating and alkali dissolution, and low valence vanadium oxide reacts with H 2O2 to obtain potassium metavanadate. The feasibility study of the preparation process of potassium metavanadate [ J ] (ferroalloy, 2022,53 (01): 24-27), adding potassium carbonate into the sodium roasting leaching solution by Mu Xiaoling, regulating the pH value to 1.5-1.8 by concentrated sulfuric acid, hydrolyzing and precipitating vanadium to obtain sodium-containing potassium polyvanadate, mixing and melting the sodium-containing potassium polyvanadate with the potassium carbonate, and recrystallizing in an aqueous medium system to obtain a potassium metavanadate product, wherein the process does not produce a reducing agent NH 3, but the sodium impurity content in the product is high. Publication No. CN102531055A provides a preparation method of sodium metavanadate/potassium metavanadate, which comprises the steps of adding calcium chloride into a sodium vanadate solution to obtain calcium vanadate solid, reacting with a potassium bicarbonate solution to obtain a potassium metavanadate solution and calcium bicarbonate precipitation, generating a large amount of chlorine-containing wastewater by the system, and dissolving back the calcium vanadate, wherein Ca (HCO 3)2) has a certain solubility, so that the Ca content in the potassium metavanadate product is increased.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing high-purity potassium metavanadate through a short process of pure sodium vanadate, and also provides a device for preparing high-purity potassium metavanadate through a short process of sodium vanadate.
In order to solve the technical problems, the method adopts the technical scheme that 1) sodium vanadate solution and potassium sulfate are mixed according to the mole ratio of potassium ions to vanadium of 0.34-1.0, concentrated sulfuric acid is added to the mixture until the pH value is 1.9-2.5, and the mixture is reacted and crystallized at 90-100 ℃ to obtain potassium polyvanadate solid;
2) Adding potassium polyvanadate solid into potassium hydroxide solution according to the molar ratio of potassium ions to vanadium of 0.5-1.0, heating to 80-100 ℃ for digestion reaction, and obtaining potassium metavanadate solution.
Further, in the step 2), the pH value of the digestion reaction end point solution is 7.0-9.0.
Further, the potassium metavanadate solution obtained in the step 2) is concentrated and dried to obtain high-purity potassium metavanadate.
The device comprises a crystallization reaction kettle, a first filtering device, a digestion reaction kettle and a second filtering device, wherein the crystallization reaction kettle is provided with a sodium vanadate solution inlet, a potassium sulfate inlet and a concentrated sulfuric acid inlet, and is provided with a heating mechanism, the digestion reaction kettle is provided with a potassium polyvanadate inlet and a potassium hydroxide solution inlet, and is provided with a heating mechanism, an outlet at the bottom of the crystallization reaction kettle is communicated with an inlet of the first filtering device, a solid material outlet of the first filtering device is connected with the potassium polyvanadate inlet of the digestion reaction kettle, an outlet at the bottom of the digestion reaction kettle is communicated with an inlet of the second filtering device, and a solid material outlet of the second filtering device is connected with the potassium polyvanadate inlet of the digestion reaction kettle.
The device is characterized by further comprising an evaporation concentration device and a spray drying device, wherein a liquid outlet of the second filtering device is communicated with an inlet of the evaporation concentration device, and an outlet of the evaporation concentration device is communicated with an inlet of the spray drying device.
And the steam outlet of the evaporation concentration device is communicated with the potassium hydroxide solution inlet of the digestion reaction kettle through the condenser.
The technical scheme has the beneficial effects that the high-purity potassium polyvanadate is innovatively used as a vanadium raw material in the alkali dissolution process, and the potassium-vanadium ratio of the potassium metavanadate solution is accurately regulated and controlled by adding excessive potassium polyvanadate in the digestion reaction, so that the high-purity potassium metavanadate is obtained. According to the invention, the sodium vanadate solution leached by sodium roasting is used as a raw material to prepare the potassium metavanadate in a short process, the reducing gas NH 3 and low-valence vanadium are not generated in the preparation process, and the potassium metavanadate precipitation process is changed, so that the potassium metavanadate in the solution is completely precipitated. According to the invention, high-purity potassium polyvanadate is used as a vanadium raw material in an alkali dissolution process, so that vanadium is prevented from being reduced in a deamination process due to the introduction of ammonium salt, spherical potassium metavanadate solid particles with uniform granularity and good fluidity can be prepared, the stability in a potassium metavanadate crystallization process and the vanadium recovery rate are improved, and the purity of the obtained potassium metavanadate product is more than 99.5wt% and the vanadium recovery rate is more than 99%.
Drawings
The invention will be described in further detail with reference to the drawings and the detailed description.
Fig. 1 is a schematic view of the structure of the device of the present invention.
In the figure, a crystallization reaction kettle 1, a first filtering device 2, a digestion reaction kettle 3, a second filtering device 4, an evaporation concentration device 5, a spray drying device 6 and a condenser 7 are arranged.
Detailed Description
The method for preparing high-purity potassium metavanadate through the short process of sodium vanadate comprises the following steps of 1) mixing a sodium vanadate solution and potassium sulfate according to the molar ratio of potassium ions to vanadium of 0.34-1.0, adding concentrated sulfuric acid to a pH value of 1.9-2.5, reacting and crystallizing under stirring at a speed of 30-300 r/min at a temperature of 90-100 ℃, observing that the reaction liquid is completed when the color of the reaction liquid is changed from red to light yellow, separating to obtain a potassium polyvanadate solid, wherein the concentration of vanadium (V) in the sodium vanadate solution is 8-45 g/L, and the concentration of potassium sulfate is 85-98wt% when the potassium sulfate is added in a solid form.
2) Adding potassium polyvanadate solid into potassium hydroxide solution according to the molar ratio of potassium ions to vanadium of 0.5-1.0, heating to 80-100 ℃, stirring at the speed of 50-400 r/min, and carrying out digestion reaction for at least 1h, wherein the pH value of a digestion reaction end point solution is 7.0-9.0, so as to obtain potassium metavanadate solution, and the concentration of the KOH solution is 20-80 g/L.
3) The potassium metavanadate solution is subjected to evaporation concentration, the evaporation concentration temperature is 80-100 ℃, the concentration of the potassium metavanadate solution after the evaporation concentration is 300-400 g/L, then drying is carried out, the drying temperature is 150-350 ℃, the high-purity potassium metavanadate can be obtained, the purity of the obtained potassium metavanadate product is more than 99.5wt%, and the vanadium recovery rate is more than 99%.
The device for preparing high-purity potassium metavanadate in the short process of sodium vanadate shown in fig. 1 comprises a crystallization reaction kettle 1, a first filtering device 2, a digestion reaction kettle 3 and a second filtering device 4. The crystallization reaction kettle 1 is provided with a sodium vanadate solution inlet, a potassium sulfate inlet and a concentrated sulfuric acid inlet, wherein the sodium vanadate solution inlet is communicated with a sodium vanadate solution source, the potassium sulfate inlet is communicated with a potassium sulfate source, the concentrated sulfuric acid inlet is communicated with a concentrated sulfuric acid source, and a heating mechanism is arranged, and the heating mechanism is preferably a structure of directly introducing steam for heating or a structure of heating a jacket. The digestion reaction kettle 3 is provided with a potassium polyvanadate inlet and a potassium hydroxide solution inlet, wherein the potassium hydroxide solution inlet is communicated with a potassium hydroxide solution source, and is also provided with a heating mechanism, and the heating mechanism is preferably a jacket heating structure. The outlet at the bottom of the crystallization reaction kettle 1 is communicated with the inlet of a first filtering device 2, the solid material outlet of the first filtering device 2 is connected with the potassium polyvanadate inlet of the digestion reaction kettle 3, the outlet at the bottom of the digestion reaction kettle 3 is communicated with the inlet of a second filtering device 4, and the solid material outlet of the second filtering device 4 is connected with the potassium polyvanadate inlet of the digestion reaction kettle 3. The first filter device 2 and the second filter device 4 are preferably filter presses.
As shown in figure 1, the device for preparing high-purity potassium metavanadate in the short process of sodium vanadate is also provided with an evaporation concentration device 5 and a spray drying device 6. The liquid outlet of the second filtering device 4 is communicated with the inlet of the evaporation and concentration device 5, and the outlet of the evaporation and concentration device 5 is communicated with the inlet of the spray drying device 6. The evaporation and concentration device 5 is provided with a heating mechanism, and the heating mechanism is preferably a jacket heating structure. The spray drying device 6 preferably performs drying by directly blowing hot air.
The device for preparing high-purity potassium metavanadate in the short process of sodium vanadate is shown in fig. 1, and is further provided with a condenser 7, wherein a steam outlet of the evaporation concentration device 5 and a steam outlet of the spray drying device 6 are communicated with a potassium hydroxide solution inlet of the digestion reaction kettle 3 through the condenser 7.
The preparation process of the device for preparing high-purity potassium metavanadate by adopting the sodium vanadate short process is as follows:
1) Sequentially injecting sodium vanadate solution, potassium sulfate solid and concentrated sulfuric acid into a crystallization reaction kettle 1, heating and heating to crystallize and separate out potassium polyvanadate, and filtering the reacted solution in a first filtering device 2 to obtain potassium polyvanadate solid;
2) Adding a potassium polyvanadate solid and a potassium hydroxide solution into a digestion reaction kettle 3, heating and heating to obtain a reaction solution, and filtering the reaction solution by a No. two filtering device 4 to obtain a potassium metavanadate solution and undissolved potassium polyvanadate solid;
3) The potassium metavanadate solution is pumped into an evaporation concentration device 5 for evaporation concentration, and then enters a spray drying device 6 for drying, so that high-purity potassium metavanadate particles are obtained;
4) In the step 3), the vapor generated by the evaporation concentration device 5 and the spray drying device 6 is condensed by a condenser 7, and the condensed water returns to the digestion reaction kettle 3 for recycling.
Example 1
To the crystallization reactor were added in sequence 1L of sodium vanadate solution with a vanadium concentration of 35g/L and 59.68g of potassium sulfate solid, the molar ratio of potassium to vanadium being 1.0, 98wt% of concentrated sulfuric acid was slowly added to a solution pH of 1.9, the stirring speed was 50r/min, and the temperature was 40 ℃. After the solution is clarified, heating to 90 ℃, and when the reaction liquid is observed to change from red to light yellow, pumping the slurry into a filter press from the bottom of the reaction kettle, and filtering and washing to obtain the potassium polyvanadate solid. Adding 0.5L KOH solution with the concentration of 50.0g/L into a digestion reaction kettle, slowly adding excessive potassium polyvanadate solid, controlling the molar ratio of potassium to vanadium in the digestion reaction kettle to be 1.0, heating to 80 ℃, stirring at the stirring rate of 100r/min, reacting for 1h, pumping the potassium metavanadate solution with the pH value of 8.0 at the end point of the reaction into an evaporation concentration device, slowly pumping the concentrated 380g/L KVO 3 solution into a 250 ℃ spray dryer, and obtaining the KVO 3 solid with the purity of 99.68wt% and the vanadium recovery rate of 99.35%.
Example 2
1L of sodium vanadate solution with the vanadium concentration of 28g/L and 32.54g of potassium sulfate solid are sequentially added into a crystallization reaction kettle, wherein the molar ratio of potassium to vanadium is 0.68, 98wt% of concentrated sulfuric acid is slowly added until the pH value of the solution is 2.1, the stirring speed is 100r/min, and the temperature is 40 ℃. After the solution is clarified, heating to 93 ℃, and when the reaction liquid is observed to change from red to light yellow, pumping the slurry into a filter press from the bottom of the reaction kettle, and filtering and washing to obtain the potassium polyvanadate solid. Adding 0.5L KOH solution with the concentration of 20.0g/L into a digestion reaction kettle, slowly adding potassium polyvanadate solid, controlling the molar ratio of potassium to vanadium in the digestion reaction kettle to be 0.70, heating to 90 ℃, stirring at the stirring rate of 200r/min, reacting for 1h, filtering excessive potassium polyvanadate, returning to the digestion reaction kettle, pumping the potassium polyvanadate solution with the pH value of 7.1 into an evaporation concentration device, slowly pumping the concentrated 340g/L KVO 3 solution into a 280 ℃ spray dryer, and obtaining the KVO 3 solid with the purity of 99.52wt% and the vanadium recovery rate of 99.16%.
Example 3
To the crystallization reactor were added in sequence 1L of a sodium vanadate solution having a vanadium concentration of 35g/L (0.686 mol) and 20.67g of potassium sulfate solid, the molar ratio of potassium ions to vanadium being 0.346, and 98wt% of concentrated sulfuric acid was slowly added to a solution pH of 2.5, stirring speed of 200r/min, and temperature of 40 ℃. After the solution is clarified, heating to 100 ℃, and when the reaction liquid is observed to change from red to light yellow, pumping the slurry into a filter press from the bottom of the reaction kettle, and filtering and washing to obtain the potassium polyvanadate solid. Adding 0.5L KOH solution with the concentration of 60.0g/L into a digestion reaction kettle, slowly adding potassium polyvanadate solid, controlling the molar ratio of potassium to vanadium in the digestion reaction kettle to be 0.5, heating to 100 ℃, stirring at the stirring rate of 230r/min, reacting for 1h, and controlling the molar ratio of potassium to vanadium in the solution to be 1.0. The excessive potassium polyvanadate is filtered and returned to a digestion reaction kettle, a potassium metavanadate solution with the pH value of 8.0 is pumped into an evaporation concentration device, and 310g/L concentrated KVO 3 solution is slowly pumped into a 320 ℃ spray dryer, so that the purity of KVO 3 solid is 99.61wt% and the vanadium recovery rate is 99.28%.
Example 4
1L of sodium vanadate solution with the vanadium concentration of 33g/L and 41.36g of potassium sulfate solid are sequentially added into a crystallization reaction kettle, wherein the molar ratio of potassium to vanadium is 0.73, 98wt% of concentrated sulfuric acid is slowly added until the pH value of the solution is 2.0, the stirring speed is 50r/min, and the temperature is 40 ℃. After the solution is clarified, heating to 95 ℃, and when the reaction liquid is observed to change from red to light yellow, pumping the slurry into a filter press from the bottom of the reaction kettle, and filtering and washing to obtain the potassium polyvanadate solid. Adding 0.5L KOH solution with the concentration of 80.0g/L into a digestion reaction kettle, slowly adding excessive potassium polyvanadate solid, controlling the molar ratio of potassium to vanadium in the digestion reaction kettle to be 0.6, heating to 91 ℃, stirring at the stirring rate of 100r/min, reacting for 1h, pumping the potassium metavanadate solution with the pH value of 8.9 at the end point of the reaction into an evaporation concentration device, slowly pumping the concentrated 380g/L KVO 3 solution into a 245 ℃ spray dryer, and obtaining the KVO 3 solid with the purity of 99.65wt% and the vanadium recovery rate of 99.34%.
Claims (6)
1. The method for preparing high-purity potassium metavanadate through a short process of sodium vanadate is characterized by comprising the following steps of 1) mixing a sodium vanadate solution and potassium sulfate according to a molar ratio of potassium ions to vanadium of 0.34-1.0, adding concentrated sulfuric acid to a pH value of 1.9-2.5, reacting at 90-100 ℃, crystallizing, and separating to obtain a potassium polyvanadate solid;
2) Adding potassium polyvanadate solid into potassium hydroxide solution according to the molar ratio of potassium ions to vanadium of 0.5-1.0, heating to 80-100 ℃ for digestion reaction, and obtaining potassium metavanadate solution.
2. The method for preparing high-purity potassium metavanadate in a short process of sodium vanadate, according to claim 1, wherein in the step 2), the pH value of the digestion reaction end point solution is 7.0-9.0.
3. The method for preparing high-purity potassium metavanadate in short flow path by using sodium vanadate as claimed in claim 1, wherein in the step 2), the obtained potassium metavanadate solution is concentrated and dried to obtain high-purity potassium metavanadate.
4. A device for preparing high-purity potassium metavanadate through a sodium vanadate short process is characterized by comprising a crystallization reaction kettle (1), a first filtering device (2), a digestion reaction kettle (3) and a second filtering device (4), wherein the crystallization reaction kettle (1) is provided with a sodium vanadate solution inlet, a potassium sulfate inlet and a concentrated sulfuric acid inlet, and is provided with a heating mechanism, the digestion reaction kettle (3) is provided with a potassium polyvanadate inlet and a potassium hydroxide solution inlet, and is provided with a heating mechanism, an outlet at the bottom of the crystallization reaction kettle (1) is communicated with an inlet of the first filtering device (2), a solid material outlet of the first filtering device (2) is connected with a potassium polyvanadate inlet of the digestion reaction kettle (3), an outlet at the bottom of the digestion reaction kettle (3) is communicated with the inlet of the second filtering device (4), and a solid material outlet of the second filtering device (4) is connected with the potassium polyvanadate inlet of the digestion reaction kettle (3).
5. The device for preparing high-purity potassium metavanadate in a short process by using sodium vanadate as claimed in claim 4, wherein the device is further provided with an evaporation concentration device (5) and a spray drying device (6), the liquid outlet of the second filtering device (4) is communicated with the inlet of the evaporation concentration device (5), and the outlet of the evaporation concentration device (5) is communicated with the inlet of the spray drying device (6).
6. The device for preparing high-purity potassium metavanadate in a short process by using sodium vanadate as claimed in claim 5, wherein the device is further provided with a condenser (7), and the steam outlet of the evaporation concentration device (5) and the steam outlet of the spray drying device (6) are communicated with the potassium hydroxide solution inlet of the digestion reaction kettle (3) through the condenser (7).
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| CN202510089671.8A CN119898815A (en) | 2025-01-21 | 2025-01-21 | A method and device for preparing high-purity potassium metavanadate by short-process sodium vanadate |
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| CN202510089671.8A CN119898815A (en) | 2025-01-21 | 2025-01-21 | A method and device for preparing high-purity potassium metavanadate by short-process sodium vanadate |
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