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Preparation method for niobium oxide or tantalum oxide with low use amount of ammonia gas

A technology of niobium oxide and usage, which is applied in chemical instruments and methods, niobium compounds, inorganic chemistry, etc., can solve the problems of large ammonia consumption, high operating costs, and high costs, so as to reduce usage, benefit environmental protection, and save cost effect

Active Publication Date: 2018-06-12
NINGXIA ORIENT TANTALUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this process needs to consume a large amount of ammonia gas, and once the ammonia gas enters the water body, the treatment method is cumbersome and the operating cost is high, resulting in a large amount of ammonia-containing wastewater, which contains a large amount of fluorine, which is difficult to treat with ordinary processes
Because ammonia-containing wastewater is difficult to treat, and the cost is high, and the one-time treatment is incomplete, it needs to be mixed and diluted with other wastewater before it can be discharged up to the standard.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Take 1000L of fluoroniobic acid solution with a content of 100g / L, and use 20mol / L hydrofluoric acid solution to adjust the HF acid content of the fluoroniobic acid solution to more than 4mol / L. In the 8-stage flow extraction tank, the organic phase Use MIBK (methyl isobutyl ketone) solution, adopt countercurrent method, control the ratio of organic phase and water phase to 1:1, and the flow rate is 30L / min. 1000L of MIBK loaded organic containing fluoroniobic acid was obtained. Add the solution into the distillation pot, heat the solution to 120°C, 1000L in the solution, MIBK will be distilled out. At this time, there is a white acidic substance in the reaction kettle. Through steam, and continue to heat to 150 degrees Celsius, keep warm for 2 hours. Then add pure water and ammonia water, neutralize until the pH is equal to 8, and obtain the product 98Kg niobium oxide product by washing, drying and roasting.

Embodiment 2

[0013] Take 1000L of fluorotantalic acid solution with a content of 100g / L, use 20mol / L hydrofluoric acid solution, adjust the HF acid content of the fluorotantalic acid solution to more than 4mol / L, and in the 12-stage flow extraction tank, the organic phase Second-octanol solution was used, and the countercurrent method was adopted to control the ratio of organic phase to water phase to 2:1, and the flow rate was 30L / min. 2000L of 2-octanol-loaded organic containing fluorotantalic acid was obtained. Add the solution into the distillation pot, heat it to 120°C, and distill 2000L of 2-octanol in the solution. At this time, there is a white acidic substance in the reaction kettle. Then add 200kg of alcohol, stir, and pass the white substance into the combustion chamber, which is made of high-nickel stainless steel. The feeding rate is 1 L per minute, and the combustion temperature is controlled to be 1000 degrees Celsius. Finally, 98 kg of white powder was obtained, washed w...

Embodiment 3

[0015] Take 1000L of fluoroniobic acid solution with a content of 60g / L, and use 20mol / L hydrofluoric acid solution to adjust the HF acid content of the fluoroniobic acid solution to be more than 4mol / L. In a 10-stage flow extraction tank, the organic phase Use MIBK (methyl isobutyl ketone) solution, adopt countercurrent method, control the ratio of organic phase and aqueous phase to 1:2, and the flow rate is 30L / min. 500 L of MIBK loaded organic containing fluoroniobic acid was obtained. Add the solution into the distillation pot, heat it to 120°C, and distill 500L of MIBK in the solution. At this time, there is a white acidic substance in the reaction kettle. Then continue to heat the white substance to 180 degrees Celsius, feed water vapor, and keep warm for 2 hours. Then put it into a converter, raise the temperature to 600-800 degrees Celsius, feed water vapor, and keep it warm for 10 hours to obtain 57 Kg of tantalum oxide powder product.

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PUM

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Abstract

A preparation method for niobium oxide or tantalum oxide with low use amount of ammonia gas includes steps of adjusting a fluoniobate or fluorotantalate solution until the content of HF acid is 4 mol / L or above; organically using MIBK (methyl isobuty ketone 4-methyl-2-pentanon) or octanol solution; extracting fluorotantalate or fluoniobate into an organic solution by using a mode of counter-current extraction in an extracting tank with 6-12 levels, wherein the ratio of an organic phase to a water phase is 1: 3 to 3: 1; setting the extracted solution at 100-150 g / L; distilling and recycling theMIBK or octanol solution; continuing heating remaining white substances; feeding water vapor; adding gasoline or ethanol, feeding the solution into a combustion chamber in a spraying mode; controlling the temperature at 800-1200 DEG C to obtain white tantalum oxide or niobium oxide product; and washing and roasting at low temperature to obtain a final product. By the preparation method, the usingamount of the ammonia gas can be reduced, the cost is saved, and environmental protection is facilitated.

Description

technical field [0001] The invention belongs to the field of rare metal processing, and in particular relates to a method for preparing niobium oxide or tantalum oxide with low ammonia consumption. Background technique [0002] In the traditional tantalum-niobium hydrometallurgical process, it is necessary to use ammonia gas to react with fluoroniobic acid or fluorotantalic acid solution to form niobium hydroxide or tantalum hydroxide precipitates, which are washed, dried, and roasted to obtain niobium oxide. However, this process needs to consume a large amount of ammonia gas, and once the ammonia gas enters the water body, the treatment method is cumbersome and the operating cost is high, resulting in a large amount of ammonia-containing wastewater, which contains a large amount of fluorine, which is difficult to treat with ordinary processes . Because ammonia-containing wastewater is difficult to treat, and the cost is high, and the treatment is not complete at one time,...

Claims

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Application Information

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IPC IPC(8): C01G35/00C01G33/00
CPCC01G33/00C01G35/00
Inventor 郑培生鲁东钟景明聂全新张伟宁刘呈义马应利喻文斌
Owner NINGXIA ORIENT TANTALUM IND
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