Method for preparing cerous fluoride

Abstract

The invention relates to a method for preparing cerous fluoride, and belongs to the technical field of hydrometallurgy. The technical problem that in the prior art, the purity of CeF3 prepared with Baotou rare earth mine sulfuric acid leaching liquid as a raw material is not high, the content of sulfate radical in the product is high and difficult to removal is solved. The method includes the steps that roasting mine obtained agter oxidizing roasting of baotite is leached by a salpeter solution, and baotite nitric acid leaching liquid is obtained; a neutral organophosphorus reagent Cyanex923 is used for conducting Ce4+ and F joint extraction from the baotite nitric acid leaching liquid, the recovery rate of Ce is larger than 95%, and the recovery rate of F is larger than 70%; reduction and reextraction are carried out to obtain nanometer cerous fluoride, the obtained cerous fluoride is roasted in a muffle furnace for 30 minutes at 200 DEG C to 400 DEG C, and the high-purity cerous fluoride is obtained. Phosphoric acid rare earth sediment can be obtained from raffinate by adjusting the nitric acid concentration, and the recovery rate of P is larger than 95%. By means of the method, the high-purity cerous fluoride can be prepared, recycling of the Ce, the F and the P in the Baotou rare earth mine sulfuric acid leaching liquid can be achieved, and F and P separation is achieved.

Description

technical field

[0001] The invention relates to the technical field of hydrometallurgy, in particular to a method for preparing cerium trifluoride by using the nitric acid leaching solution of Baotou rare earth roasted ore as a raw material. Background technique

[0002] In recent years, due to the application in the fields of polishing powder, solid lubricant, optoelectronic devices, and electrolytic preparation of metal cerium, cerium trifluoride (CeF 3 ) are getting more and more attention. Currently CeF 3 Common synthetic methods include HF(NH 4 HF 2 ) precipitation-vacuum dehydration method, HF (NH 4 HF 2 ) fluorination method, NH 4 HCO 3 Transformation preparation method, microwave solid-phase redox synthesis method, polyol method, microemulsion preparation method, etc.

[0003] Due to the complex composition of Baotou rare earth concentrate, after oxidative roasting, the acid leaching solution obtained by leaching with nitric acid or sulfuric acid contains not...

Examples

preparation example Construction

[0024] The method for preparing cerium trifluoride provided by the invention specifically comprises the following steps:

[0025] (1) Oxidize and roast Baotou ore at a temperature of 400-600°C for 60-90 minutes. The obtained roasted ore is leached with nitric acid solution, HNO 3 The concentration is 3-8M, the liquid-solid ratio is 3-6, the leaching time is 20-90 minutes, the leaching temperature is 20-50°C, suction filtration, washing to obtain Baotou Mine nitric acid leachate and monazite-rich slag. Monazite slag can be treated by acid method or alkali method, which is not considered in the present invention.

[0026] (2) Co-extract Ce from Baotou mine nitric acid leaching solution by neutral phosphorus extractant Cyanex923+isooctanol+n-heptane 4+ and F, then use a mass percentage of 0.1% H 2 o 2 Nano-CeF obtained by reduction stripping 3 , calcining the obtained cerium trifluoride in a muffle furnace at 200-400° C. for 30 minutes, preferably at a temperature of 350° C.,...

Embodiment 1

[0028] Take 100g of Baotou rare earth concentrate (50 ore), and oxidize and roast it in a muffle furnace at 400°C for 60 minutes. The obtained roasted ore was leached with 4M nitric acid solution, the solid-to-liquid ratio was 3, the leaching time was 90 minutes, and the leaching temperature was 20° C., and the nitric acid leaching solution of Baotou ore was obtained after filtration. [REO] = 60g / L in the leaching solution, where [Ce 4+ ]=25g / L, with 300mL 15% of Cyanex923+10% isooctyl alcohol+75% n-heptane as extractant, extract the Ce in the leachate 4+ and F - , the recovery rate of Ce is greater than 95%, and the recovery rate of F is 70%. Then with 0.1% H 2 o 2 Reductive stripping was carried out to obtain cerium trifluoride with an average particle diameter of 70 nm. Calcining the obtained cerium trifluoride in a muffle furnace at 350°C for 30 minutes to obtain high-purity cerium trifluoride with a purity greater than 99.99%. Adjust the acidity of the extracted wat...

Embodiment 2

[0031] Take 100g of Baotou rare earth concentrate (65 ore), and oxidize and roast it in a muffle furnace at 500°C for 60 minutes. The obtained roasted ore was leached with 3M nitric acid solution, the solid-to-liquid ratio was 4, the leaching time was 20 minutes, and the leaching temperature was 40°C. After filtration, the nitric acid leaching solution of Baotou ore was obtained. [REO] = 120g / L in the leaching solution, where [Ce 4+ ]=55g / L, with 300mL 30% of Cyanex923+10% isooctyl alcohol+60% n-heptane as extractant, extract the Ce in the leachate 4+ and F - , the recovery rate of Ce is greater than 95%, and the recovery rate of F is 70%. Then with 0.1% H 2 o 2 Reductive stripping was carried out to obtain cerium trifluoride with an average particle diameter of 70 nm. Calcining the obtained cerium trifluoride in a muffle furnace at 200°C for 30 minutes to obtain high-purity cerium trifluoride with a purity greater than 98.92%. Adjust the acidity of the extracted water p...

technical field

[0001] The invention relates to the technical field of hydrometallurgy, in particular to a method for preparing cerium trifluoride by using the nitric acid leaching solution of Baotou rare earth roasted ore as a raw material. Background technique

[0002] In recent years, due to the application in the fields of polishing powder, solid lubricant, optoelectronic devices, and electrolytic preparation of metal cerium, cerium trifluoride (CeF 3 ) are getting more and more attention. Currently CeF 3 Common synthetic methods include HF(NH 4 HF 2 ) precipitation-vacuum dehydration method, HF (NH 4 HF 2 ) fluorination method, NH 4 HCO 3 Transformation preparation method, microwave solid-phase redox synthesis method, polyol method, microemulsion preparation method, etc.

[0003] Due to the complex composition of Baotou rare earth concentrate, after oxidative roasting, the acid leaching solution obtained by leaching with nitric acid or sulfuric acid contains not...

Examples

preparation example Construction

[0024] The method for preparing cerium trifluoride provided by the invention specifically comprises the following steps:

[0025] (1) Oxidize and roast Baotou ore at a temperature of 400-600°C for 60-90 minutes. The obtained roasted ore is leached with nitric acid solution, HNO 3 The concentration is 3-8M, the liquid-solid ratio is 3-6, the leaching time is 20-90 minutes, the leaching temperature is 20-50°C, suction filtration, washing to obtain Baotou Mine nitric acid leachate and monazite-rich slag. Monazite slag can be treated by acid method or alkali method, which is not considered in the present invention.

[0026] (2) Co-extract Ce from Baotou mine nitric acid leaching solution by neutral phosphorus extractant Cyanex923+isooctanol+n-heptane 4+ and F, then use a mass percentage of 0.1% H 2 o 2 Nano-CeF obtained by reduction stripping 3 , calcining the obtained cerium trifluoride in a muffle furnace at 200-400° C. for 30 minutes, preferably at a temperature of 350° C.,...

Embodiment 1

[0028] Take 100g of Baotou rare earth concentrate (50 ore), and oxidize and roast it in a muffle furnace at 400°C for 60 minutes. The obtained roasted ore was leached with 4M nitric acid solution, the solid-to-liquid ratio was 3, the leaching time was 90 minutes, and the leaching temperature was 20° C., and the nitric acid leaching solution of Baotou ore was obtained after filtration. [REO] = 60g / L in the leaching solution, where [Ce 4+ ]=25g / L, with 300mL 15% of Cyanex923+10% isooctyl alcohol+75% n-heptane as extractant, extract the Ce in the leachate 4+ and F - , the recovery rate of Ce is greater than 95%, and the recovery rate of F is 70%. Then with 0.1% H 2 o 2 Reductive stripping was carried out to obtain cerium trifluoride with an average particle diameter of 70 nm. Calcining the obtained cerium trifluoride in a muffle furnace at 350°C for 30 minutes to obtain high-purity cerium trifluoride with a purity greater than 99.99%. Adjust the acidity of the extracted wat...

Embodiment 2

[0031] Take 100g of Baotou rare earth concentrate (65 ore), and oxidize and roast it in a muffle furnace at 500°C for 60 minutes. The obtained roasted ore was leached with 3M nitric acid solution, the solid-to-liquid ratio was 4, the leaching time was 20 minutes, and the leaching temperature was 40°C. After filtration, the nitric acid leaching solution of Baotou ore was obtained. [REO] = 120g / L in the leaching solution, where [Ce 4+ ]=55g / L, with 300mL 30% of Cyanex923+10% isooctyl alcohol+60% n-heptane as extractant, extract the Ce in the leachate 4+ and F - , the recovery rate of Ce is greater than 95%, and the recovery rate of F is 70%. Then with 0.1% H 2 o 2 Reductive stripping was carried out to obtain cerium trifluoride with an average particle diameter of 70 nm. Calcining the obtained cerium trifluoride in a muffle furnace at 200°C for 30 minutes to obtain high-purity cerium trifluoride with a purity greater than 98.92%. Adjust the acidity of the extracted water p...

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