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Method for preparing praseodymium-neodymium fluoride from praseodymium-neodymium oxalate

A technology of praseodymium neodymium oxalate and praseodymium neodymium fluoride, applied in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc., can solve the problems of long process steps, high cost of wastewater treatment, unfavorable environmental protection, etc., and has great prospects for industrial promotion Effect

Inactive Publication Date: 2015-10-14
BAOTOU REWIN RARE EARTH METAL MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Disadvantages: Every ton of praseodymium and neodymium fluoride produces more than 4 tons of waste acid water, which needs to be neutralized and discharged up to standard
Disadvantages: NdPr oxide must be calcined from NdPr oxalate or NdPr oxalate at high temperature, and the cost is 2,000 yuan / ton higher
[0004] To sum up, the disadvantages of the existing PrNd fluoride production process are: 1) Method 1 has long process steps, resulting in a low yield of PrNd by about 95%, generating a large amount of waste water and high treatment costs, which is not conducive to environmental protection
Disadvantages: NdPrO should be calcined from NdPrO at high temperature, and the cost per ton is 2000 yuan higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Put 300kg of praseodymium neodymium oxalate (REO 45wt%) into the fluorination furnace, raise the temperature at 0-300°C for 6h, and at 300-350°C for 19h, the excess of HF gas is 20wt% (purity 99.99%), and the gas flow rate is 8kg / h. The by-products of the reaction are absorbed by condensation into hydrofluoric acid, CO 2 emptying.

[0016] The fluorination rate of the product is not less than 99%, O<0.05 wt % in the product, F is 28.10 wt %, and the yield of praseodymium and neodymium is 99.54%.

Embodiment 2

[0018] Put 300kg of praseodymium neodymium oxalate (REO 50wt%) into the fluorination furnace, raise the temperature at 0-300°C for 8h, and at 300-350°C for 38h, the excess of HF gas is 20wt% (purity 99.99%), and the gas flow rate is 4kg / h. The by-products of the reaction are absorbed by condensation into hydrofluoric acid, CO 2 emptying.

[0019] The fluorination rate of the product is not less than 99%, O<0.05 wt % in the product, F is 28.58 wt %, and the yield of praseodymium and neodymium is 99.89%.

Embodiment 3

[0021] Put 300kg of praseodymium neodymium oxalate (REO 50.32wt%) into the fluorination furnace, raise the temperature at 0-300°C for 9h, and 300-350°C for 25h, the excess of HF gas is 20wt% (purity 99.99%), and the gas flow rate is 6kg / h. The by-products of the reaction are absorbed by condensation into hydrofluoric acid, CO 2 emptying.

[0022] The fluorination rate of the product is not less than 99%, O<0.05 wt%, F in the product is 28.78 wt%, and the yield of praseodymium and neodymium is 99.78%.

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PUM

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Abstract

The invention relates to a method for preparing praseodymium-neodymium fluoride from praseodymium-neodymium oxalate. In the provided preparation method, praseodymium-neodymium oxalate directly reacts with HF gas at a temperature of 200 to 350 DEG C to generate praseodymium-neodymium fluoride, acidic water, and CO2, and anhydrous praseodymium-neodymium fluoride is produced. The provided preparation method has the advantages that the step that praseodymium-neodymium oxalate is burned into oxides at a high temperature is eliminated, the problem that a large amount of waste acid is discharged is solved, the cost is reduced, the cost for each ton can be reduced by 2000 yuan, and the industrial promotion prospect is wide.

Description

technical field [0001] The invention relates to a method for preparing praseodymium neodymium fluoride from praseodymium neodymium oxalate, which belongs to the technical field of metallurgical rare earth preparation. Background technique [0002] The existing praseodymium-neodymium fluoride is prepared by reacting hydrofluoric acid (concentration: 40 wt%) with praseodymium-neodymium carbonate, and HF gas with praseodymium-neodymium oxide. The former method is called "wet process" by the rare earth industry. Production steps: Mix an excess of 20wt% hydrofluoric acid (concentration 40wt%) with praseodymium neodymium carbonate (42-45wt% REO) and react at 60°C to generate praseodymium neodymium fluoride and water, CO 2 , washed with water to pH = 7, filtered and drained, dried at above 500°C to remove crystal water, and anhydrous praseodymium neodymium fluoride was obtained. Disadvantages: Every ton of praseodymium and neodymium fluoride produces more than 4 tons of waste aci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00
Inventor 尹祖平梁行方郭海涛孔向民邓沅徐志广贾恩泽张志军蔡曙光刘雨邢佳骏
Owner BAOTOU REWIN RARE EARTH METAL MATERIALS