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CN-117737417-B - Sulfuric acid decomposition device and method for uranium-containing niobium multi-metal ore

CN117737417BCN 117737417 BCN117737417 BCN 117737417BCN-117737417-B

Abstract

The invention provides a sulfuric acid decomposition device and a sulfuric acid decomposition method for uranium-containing niobium multi-metal ores, and relates to the technical field of hydrometallurgy. The device provided by the invention is used for carrying out sulfuric acid decomposition on uranium-containing niobium multi-metal ore, realizes the mixing, curing and leaching processes of mineral powder and concentrated sulfuric acid, reduces the configuration of system equipment by designing a process and a decomposition-leaching integrated tank device and carrying out high-temperature acidolysis and leaching processes in the same equipment, avoids the transfer of high-temperature high-acid materials between decomposition and extraction equipment, and strengthens the reaction mass transfer and reduces the energy consumption by adopting a dynamic curing self-heating strengthening decomposition process. The invention realizes the efficient extraction of valuable metals uranium and niobium in uranium-containing niobium complex multi-metal ores, does not use fluorine-containing substances, has low reagent cost and does not generate fluorine-containing wastewater, and solves the technical problem of extracting uranium-containing niobium multi-metal ores. Moreover, the device provided by the invention has the advantages of simple equipment configuration, low energy consumption, high extraction rate of valuable metals and the like.

Inventors

  • LIU HUIWU
  • LI GUANG
  • WANG GUISHUO
  • CHENG HAO
  • Liang Gengyu
  • MA JIA
  • LIU ZHONGCHEN
  • XIANG QIULIN
  • LIU KANG
  • TIAN YUHUI

Assignees

  • 核工业北京化工冶金研究院

Dates

Publication Date
20260505
Application Date
20231227

Claims (9)

  1. 1. A sulfuric acid decomposition method of uranium-containing niobium multi-metal ore, characterized by being performed by a sulfuric acid decomposition apparatus, the sulfuric acid decomposition apparatus of uranium-containing niobium multi-metal ore comprising: The mixing device is arranged in the mixer (3), and the mixer (3) is also provided with a mineral powder inlet, a sulfuric acid feeding pipe and a discharge hole; the decomposing-leaching integrated tank (4) is communicated with the discharge port of the mixer (3), the decomposing-leaching integrated tank (4) is also provided with a water inlet pipe, a compressed air inlet pipe, a steam inlet pipe, a discharge port and a compressed air-steam mixing device (4-1), and valves are arranged on the water inlet pipe, the compressed air inlet pipe and the steam inlet pipe; the sulfuric acid decomposition method comprises the following steps: Mixing uranium-containing niobium polymetallic ore powder with concentrated sulfuric acid in a mixer (3) to obtain a mixture, wherein the mass fraction of the concentrated sulfuric acid is 90-98%; The mixed material is conveyed into a decomposition-leaching integrated tank (4) under the condition of first compressed air stirring, water is added to dilute concentrated sulfuric acid, ore decomposition is carried out under the condition of dilution heat and reaction heat, then process water is added to leach under the condition of second compressed air stirring, and acidolysis leaching liquid of uranium-containing niobium multi-metal ore is obtained, the ore decomposition temperature is 100-200 ℃, the concentration of sulfuric acid in the process water is 0.3-1.5 mol/L, the uranium concentration is 10-40 mg/L, and the niobium concentration is 25-100 mg/L.
  2. 2. The sulfuric acid decomposition method according to claim 1, wherein the mass ratio of the uranium-containing niobium polymetallic ore powder to the concentrated sulfuric acid is 1:0.4-2.
  3. 3. The sulfuric acid decomposition method according to claim 1 or 2, wherein the compressed air pressure of the first compressed air agitation is 300 to 600kpa; The mass ratio of the uranium-containing niobium polymetallic ore powder to the dilution water is 1:0.2-1.5; The temperature of the ore decomposition is 100-200 ℃ and the time is 30-120 min.
  4. 4. A sulfuric acid decomposition method according to claim 3, wherein the solid-to-liquid ratio of uranium-containing niobium polymetallic ore powder to process water is 1kg:2 to 5l.
  5. 5. The sulfuric acid decomposition method according to claim 1 or 4, wherein the pressure of the compressed air for the second compressed air agitation is 400 to 800kpa; the leaching time is 0.5-2 h.
  6. 6. The sulfuric acid decomposition method according to claim 1, further comprising separating uranium and niobium from the uranium-containing and niobium-containing polymetallic ore acidolysis leachate to obtain a uranium product, a niobium product and a metal separated solution, respectively, and transferring the metal separated solution to a decomposition-leaching integrated tank (4) to dilute concentrated sulfuric acid instead of water and using the concentrated sulfuric acid as process water for the leaching step.
  7. 7. The sulfuric acid decomposition method according to claim 6, wherein the uranium niobium separation includes thermal precipitation niobium extraction and uranium extraction, wherein the thermal precipitation niobium extraction and uranium extraction are not in chronological order; the temperature of the thermal precipitation niobium extraction is 150-250 ℃ and the time is 1-2 hours; the extractant system used for uranium extraction comprises a main extractant, an auxiliary extractant and a diluent, wherein the main extractant comprises diisooctyl phosphate and/or tri-n-octylamine, the auxiliary extractant comprises one or more of tributyl phosphate, trialkylphosphine oxide and isodecyl alcohol, the diluent comprises sulfonated kerosene, the volume fraction of the main extractant in the extractant system is 3-5%, the volume fraction of the auxiliary extractant is 5-15%, and the uranium extraction time is 3-5 min; In the recycling process of the solution after metal separation, the mass ratio of uranium-containing niobium multi-metal ore powder to the solution after metal separation is 1:0.2-1.5, and the time for conveying the solution after metal separation into the decomposition-leaching integrated tank (4) is 10-30 min.
  8. 8. The sulfuric acid decomposition method according to claim 1, 2 or 4, characterized in that the sulfuric acid decomposition apparatus further comprises: the discharge port is communicated with the mineral powder inlet of the mixer (3), and the feeder (2) is also provided with the mineral powder inlet; And the discharge hole is communicated with the mineral powder inlet of the feeder (2).
  9. 9. A sulfuric acid decomposition method according to claim 1,2, 4, 6 or 7, characterized in that the sulfuric acid decomposition device further comprises a discharge pump (5) with an inlet communicating with the discharge port of the decomposition-leaching integrated tank (4).

Description

Sulfuric acid decomposition device and method for uranium-containing niobium multi-metal ore Technical Field The invention relates to the technical field of hydrometallurgy, in particular to a sulfuric acid decomposition device and method for uranium-containing niobium multi-metal ores. Background Along with the continuous development of uranium ore resources, ores which are easy to mine are less and less, and complex uranium polymetallic ores are large in resource quantity, associated with strategic metals, high in value, and more in focus of production enterprises, and the complex uranium polymetallic ores also become a hot spot field of research in scientific research institutions and universities. The complex uranium polymetallic ore is generally uranium, titanium, niobium and tantalum-containing ore, has complex components and high chemical stability, and is often produced in refractory minerals such as monazite, biotite and the like, and is difficult to process. In order to decompose the difficult-to-treat ore, patent CN111020186A discloses a method for comprehensively recovering uranium and titanium from niobium and titanium uranium ore, sulfuric acid-hydrofluoric acid is adopted to leach the niobium and titanium uranium ore, 10-60wt% sulfuric acid and 1-8wt% hydrofluoric acid are added, stirring leaching is carried out for 1-8 hours at 50-90 ℃, leaching rates of uranium and niobium and titanium are respectively 98.4%, 80.3% and 47.4%, and comprehensive uranium and titanium niobium extraction can be realized. However, the method utilizes the strong corrosiveness of hydrofluoric acid to improve the extraction rate of valuable metals, and has higher reagent cost and higher treatment difficulty of fluorine-containing wastewater. Zhou Chunyan et al (Zhou Chunyan, tan Zhongren, li Shunan, et al. Research on uranium pyrochlore-niobium titanium uranium ore type ore treatment [ J ]. Nonferrous metal (beneficiation part, 1981 (05): 54.) proposed that uranium pyrochlore-niobium titanium uranium ore type ore adopts sulfuric acid-potassium fluosilicate synergistic leaching process, the dosages of sulfuric acid, potassium fluosilicate and manganese dioxide are respectively 16%, 5% and 2% of mineral quality, grinding granularity is-0.2 mm, and leaching is carried out under stirring for 3 hours at 80 ℃, uranium leaching rate reaches 93%, and niobium leaching rate is above 63%. The process realizes synchronous leaching of uranium and niobium, but still has the defects of high reagent cost, complex treatment of fluorine-containing wastewater and the like. Disclosure of Invention In view of the above, the present invention aims to provide a sulfuric acid decomposition apparatus and a sulfuric acid decomposition method for uranium-containing niobium multi-metal ores. The sulfuric acid decomposing device provided by the invention is adopted to carry out concentrated sulfuric acid curing and leaching on uranium-containing niobium multi-metal ores, so that efficient extraction of valuable metals uranium and niobium in the uranium-containing niobium complex multi-metal ores can be realized. In order to achieve the above object, the present invention provides the following technical solutions: The invention provides a sulfuric acid decomposition device of uranium-containing niobium multi-metal ore, which comprises The mixer 3 is internally provided with a stirring device, and the mixer 3 is also provided with a mineral powder inlet, a sulfuric acid feeding pipe and a discharge hole; The decomposing-leaching integrated tank 4 with a feeding hole communicated with a discharging hole of the mixer 3 is further provided with a water inlet pipe, a compressed air inlet pipe, a steam inlet pipe, a discharging hole and a compressed air-steam mixing device 4-1, and valves are arranged on the water inlet pipe, the compressed air inlet pipe and the steam inlet pipe. Preferably, the sulfuric acid decomposition device further comprises: A feeder 2 with a discharge hole communicated with a mineral powder inlet of the mixer 3, wherein the feeder 2 is also provided with the mineral powder inlet; And the discharge hole is communicated with the mineral powder inlet of the feeder 2. Preferably, the sulfuric acid decomposing device further comprises a discharge pump 5, wherein an inlet of the discharge pump is communicated with the discharge port of the decomposing-leaching integrated tank 4. The invention provides a sulfuric acid decomposition method of uranium-containing niobium multi-metal ore, which is carried out by using the sulfuric acid decomposition device according to the technical scheme, and comprises the following steps: mixing uranium-containing niobium multi-metal ore powder with concentrated sulfuric acid in a mixer 3 to obtain a mixture; And (3) conveying the mixture to a decomposition-leaching integrated tank 4 under the condition of first compressed air stirring, adding water to dilute concentrated sulfuric acid, decomposing