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CN-122012952-A - Method for deep extracting vanadium from vanadium-containing mud

CN122012952ACN 122012952 ACN122012952 ACN 122012952ACN-122012952-A

Abstract

The invention relates to the technical field of extraction, in particular to a method for deeply extracting vanadium from vanadium-containing mud, which sequentially comprises the following steps of (1) microwave-mechanical coupling roasting modification, (2) composite collaborative leaching, (3) graded oxidation vanadium precipitation, (4) recycling closed-loop treatment, wherein from the view of the synergistic effect of the whole technical scheme, the microwave-mechanical coupling roasting modification provides a modified product which is easy to leach for the composite collaborative leaching, the composite collaborative leaching provides leaching liquid with high vanadium concentration and low impurities for graded oxidation vanadium precipitation, the graded oxidation vanadium precipitation provides filtrate and leaching slag which are easy to treat for the recycling closed-loop treatment, the recycling closed-loop treatment prepares the leaching slag into silicate bricks, and the filtrate is recycled to a roasting process after being concentrated by a nanofiltration membrane and intercepted by impurities, so that the recycling of resources is realized, and meanwhile, the solid waste and the wastewater emission are reduced, and the environmental pollution is reduced.

Inventors

  • Shu Guipeng
  • LIU ZHANMING
  • YU XIAOCHEN

Assignees

  • 攀枝花市阳润科技有限公司

Dates

Publication Date
20260512
Application Date
20260317

Claims (10)

  1. 1. The method for deeply extracting vanadium from the vanadium-containing slurry is characterized by sequentially comprising the following steps of: (1) Uniformly mixing vanadium-containing slurry and sodium carbonate according to a mass ratio of 100:5.8-6.2, placing the mixture in a microwave-mechanical coupling field for roasting, controlling the roasting temperature to 550-650 ℃ and the roasting time to 1.5-2.5h, cooling to room temperature after roasting, and crushing to a particle size less than or equal to 1mm to obtain a roasting modified product, wherein the microwave power is 200-300W, the frequency is 2.45GHz, and the mechanical stirring rotating speed is 30-60 r/min; (2) Mixing the roasting modified product obtained in the step (1) with water according to a solid-liquid ratio of 1:1.2-1.5, adding sodium sulfate and sodium metabisulfite, regulating the pH value of a system to 4.0-5.0, leaching for 45-60min under the conditions of 80-90 ℃ and stirring rotation speed of 60-80r/min, and carrying out solid-liquid separation to obtain vanadium-containing leaching solution and leaching slag; The concentration of the sodium sulfate adding system is 5-8g/L and the concentration of the sodium metabisulfite adding system is 0.5-1.0g/L; (3) And (3) carrying out staged oxidation and vanadium precipitation: ① Adding ammonium sulfate into the vanadium-containing leaching solution in the step (2), adding according to the molar ratio of V 2 O 5 to NH 4 + of 1:1.5-1.8, regulating the pH value to 1.8-2.0, stirring and reacting for 30-40min at 80-100r/min, separating out ammonium polyvanadate coarse precipitate, and filtering and separating to obtain coarse precipitate and primary vanadium-precipitating filtrate; ② Oxidation adjustment, namely adding sodium chlorate into the primary vanadium precipitation filtrate, wherein the adding amount is 1.2-1.5 times of the molar amount of V 3+ in the filtrate, and oxidation is completed within 20-30 min; ③ Adding ammonium oxalate into the oxidized filtrate, adding according to the molar ratio of V 2 O 5 to NH 4 + of 1:2.0-2.5, regulating the pH value to 2.2-2.5, stirring for reaction for 30-40min at 80-100r/min, separating out ammonium polyvanadate fine precipitate, filtering and separating to obtain fine precipitate, combining the coarse precipitate and the fine precipitate, washing, drying, and calcining at 550-600 ℃ for 2-3h to obtain a V 2 O 5 product; (4) And (3) carrying out recycling closed-loop treatment, namely washing leaching residues in the step (2) with deionized water for 2-3 times, wherein the liquid-solid ratio is 1:1.0-1.2 each time until no obvious chloride ion remains, and then, using nanofiltration membranes with the molecular weight cut-off of 100-200Da to concentrate filtrate obtained after the secondary vanadium precipitation in the step (3) for 3-5 times, intercepting soluble impurities, supplementing sodium carbonate until the concentration is consistent with that of the initial mixture in the step (1), and recycling to the roasting modification procedure in the step (1).
  2. 2. The method of claim 1, wherein the vanadium-containing slurry in step (1) is dehydrated to a water content of 65-80% by plate-and-frame press filtration before being mixed, so that the influence of excessive water content on the roasting efficiency is avoided.
  3. 3. The method of claim 1, wherein in the microwave-mechanical coupling roasting in step (1), the microwave power is controlled by gradient, the microwave power is controlled by 200W for 0-0.5h, and the microwave power is controlled by 250-300W for 0.5-2.5h, so that vanadium lattice agglomeration caused by local overheating is avoided.
  4. 4. The method of claim 1, wherein in the complex co-leaching of step (2), the pH adjustment is performed using 5% strength by mass dilute sulfuric acid.
  5. 5. The method of claim 1, wherein the reaction temperature of the primary vanadium precipitation in step (3) ① is 60-70 ℃, and the reaction temperature of the secondary vanadium precipitation in step (3) ③ is 70-80 ℃.
  6. 6. The method of claim 1, wherein the constant stirring speed is 60-80r/min during the oxidation adjustment in step (3) ②.
  7. 7. The method according to claim 1, wherein the vanadium concentrate washing in step (3) uses dilute ammonia water with a concentration of 1-2wt% to remove sulfate and chloride impurities adsorbed on the surface.
  8. 8. The method according to claim 1, wherein the operation pressure is controlled to be 0.3-0.5MPa and the temperature is controlled to be 25-35 ℃ in the nanofiltration membrane concentration process in the step (4).
  9. 9. The method according to claim 1, wherein 10-15% of kaolin by mass of the leaching residue is added when the leaching residue in step (4) is used for preparing silicate bricks.
  10. 10. The method according to claim 1, wherein after the sodium carbonate is supplemented in the recycled filtrate, the chloride ion content of the system is detected, so that the chloride ion residual quantity of the recycled system is ensured to be less than or equal to 0.5%.

Description

Method for deep extracting vanadium from vanadium-containing mud Technical Field The invention relates to the technical field of extraction, in particular to a method for deeply extracting vanadium from vanadium-containing mud. Background Vanadium is an important strategic metal, and is widely applied to various fields of steel, chemical industry, new energy sources and the like, and the market demand is continuously growing. The vanadium-containing mud is solid waste generated in the processes of vanadium smelting, chemical production and the like, the vanadium content is usually between 0.5% and 3.0%, if the mud is directly stacked or buried, the waste of vanadium resources can be caused, and serious environmental hazards can be caused because heavy metal ions in the mud permeate, soil and underground water are polluted. Therefore, the method realizes the efficient extraction and recycling of vanadium in the vanadium-containing slurry, accords with the industrial policy of recycling the resources, can solve the problem of solid waste pollution, and has important economic value and environmental protection significance. At present, the common process for extracting vanadium from vanadium-containing slurry mainly comprises three steps of roasting, leaching and precipitating vanadium, but the prior process has various technical defects generally, and is difficult to meet the high-efficiency and environment-friendly requirements of industrial production. In the roasting step, the traditional process adopts a muffle furnace for static roasting, the mode is not uniformly heated, the mixing of vanadium-containing slurry and fluxing agent is insufficient, vanadium lattice agglomeration is easy to cause, part of vanadium is wrapped in a slurry matrix and cannot be effectively released, further the subsequent leaching efficiency is reduced, meanwhile, the static roasting time is longer, the energy consumption is higher, and the production cost is increased. In the leaching step, most processes only adopt a single leaching agent, the leaching selectivity is poor, the leaching rate of vanadium is low, and a large amount of impurities are leached together, so that the subsequent vanadium precipitation and purification are difficult. The current vanadium extraction technology of vanadium-containing mud has the problems of low vanadium leaching rate, insufficient product purity, low resource utilization rate, high energy consumption, serious pollution and the like, and is difficult to consider economic benefit, environmental benefit and social benefit. Therefore, developing a method for deep extracting vanadium from vanadium-containing slurry, which can solve the technical defects and realize efficient extraction, high-purity recovery and closed-loop utilization of resources, becomes a technical problem to be solved by the current technicians in the field. Disclosure of Invention The invention aims to provide a method for deeply extracting vanadium from vanadium-containing mud. In order to achieve the above purpose, the present invention provides the following technical solutions: The method for deeply extracting vanadium from the vanadium-containing mud sequentially comprises the following steps of: (1) Uniformly mixing vanadium-containing slurry and sodium carbonate according to a mass ratio of 100:5.8-6.2, placing the mixture in a microwave-mechanical coupling field for roasting, controlling the roasting temperature to 550-650 ℃ and the roasting time to 1.5-2.5h, cooling to room temperature after roasting, and crushing to a particle size less than or equal to 1mm to obtain a roasting modified product, wherein the microwave power is 200-300W, the frequency is 2.45GHz, and the mechanical stirring rotating speed is 30-60 r/min; (2) Mixing the roasting modified product obtained in the step (1) with water according to a solid-liquid ratio of 1:1.2-1.5, adding sodium sulfate and sodium metabisulfite, regulating the pH value of a system to 4.0-5.0, leaching for 45-60min under the conditions of 80-90 ℃ and stirring rotation speed of 60-80r/min, and carrying out solid-liquid separation to obtain vanadium-containing leaching solution and leaching slag; The concentration of the sodium sulfate adding system is 5-8g/L and the concentration of the sodium metabisulfite adding system is 0.5-1.0g/L; (3) And (3) carrying out staged oxidation and vanadium precipitation: ① Adding ammonium sulfate into the vanadium-containing leaching solution in the step (2), adding according to the molar ratio of V 2O5 to NH 4+ of 1:1.5-1.8, regulating the pH value to 1.8-2.0, stirring and reacting for 30-40min at 80-100r/min, separating out ammonium polyvanadate coarse precipitate, and filtering and separating to obtain coarse precipitate and primary vanadium-precipitating filtrate; ② Oxidation adjustment, namely adding sodium chlorate into the primary vanadium precipitation filtrate, wherein the adding amount is 1.2-1.5 times of the molar amount of V