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Process for extracting and separating thorium and extracting rare earth chloride from sulfuric and phosphoric mixed acid system

A technology of sulfur-phosphorus mixed acid and rare earth chloride, which is applied in the field of extracting and separating thorium and extracting rare earth chloride, can solve the problems of prolonging the radioactive pollution process, negative impact on the operating environment, and adding a large amount of mixed alcohol, and achieves simple process flow and high product quality. The effect of high recovery rate and low consumption

Inactive Publication Date: 2003-02-05
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] This technology first separates cerium (IV), and then extracts and separates thorium from the solution of rare earth and iron, which prolongs the process of radioactive contamination of thorium, and the addition of a large amount of mixed alcohol increases the cost and has negative effects on the operating environment. influences

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] The concentrated sulfuric acid low-temperature roasting water immersion liquid of bastnaesite and monazite mixed concentrate is used as raw material. The composition of the liquid is: the concentration of sulfuric acid is 0.5 mol / liter, the total amount of rare earth oxides is 20.6 grams / liter, and the concentration of thorium dioxide is 100 mg / L, cerium oxide content 10.3 g / L, iron content 2.73 g / L, phosphorus content 1.55 g / L, fluorine content 0.57 g / L, calcium content 0.42 g / L, silicon content 1.26 g / L Lift.

[0013] Separation of thorium using fractional distillation extraction, the extracted organic phase is 1% primary amine N 1923 -1% kerosene solution of methylheptanol, acid reversion is 0.1 mol / liter nitric acid, 7-stage extraction, 6-stage washing. The flow ratio is organic phase: solid liquid: acid reversed = 1.3: 4: 0.25. The mixing time is 5 minutes, and the clarification time is 5 minutes to obtain a thorium-containing organic phase and a raffinate rare e...

Embodiment 2

[0017] The composition of the feed liquid is: the concentration of sulfuric acid is 0.38 mol / liter, the total amount of rare earth oxides is 26.5 grams / liter, the concentration of thorium dioxide is 125 mg / liter, the content of cerium oxide is 13.2 grams / liter, and the content of iron is 3.51 grams / liter , the fluorine content is 0.74 g / L, the phosphorus content is 2.17 g / L, the calcium content is 0.56 g / L, and the silicon content is 1.62 g / L.

[0018] Separate the thorium and extract the organic phase to 3% N 1923 -1% methylheptanol-kerosene solution, the acid backlash is 0.3 mol / liter nitric acid. Using 13 stages of fractional distillation extraction, 6 stages of extraction, 7 stages of washing. The flow ratio is organic phase: solid liquid: acid reversed = 1: 4: 0.2. The mixing time is 5 minutes, and the clarification time is 5 minutes to obtain a thorium-containing organic phase and a raffinate rare earth solution. The thorium in the organic phase was back-extracted wit...

Embodiment 3

[0022] The composition of the feed liquid is: the concentration of sulfuric acid is 0.41 mol / liter, the total amount of rare earth oxides is 33.4 grams / liter, the concentration of thorium dioxide is 160 mg / liter, the content of cerium oxide is 16.7 grams / liter, and the content of iron is 4.42 grams / liter , the phosphorus content is 2.79 g / L, the fluorine content is 0.93 g / L, the calcium content is 0.70 g / L, and the silicon content is 2.04 g / L.

[0023] Separate the thorium and extract the organic phase to 4% N 1923 -2% methylheptanol-kerosene solution, the acid backlash is 0.3 mol / liter nitric acid. Using 12 stages of fractional distillation extraction, 4 stages of extraction, 8 stages of washing. The flow ratio is organic phase: solid liquid: acid reversed = 0.8: 4: 0.2. The mixing time is 5 minutes, and the clarification time is 5 minutes to obtain a thorium-containing organic phase and a raffinate rare earth solution. The thorium in the organic phase was back-extracted w...

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Abstract

The present invention belongs to a process for extracting and separating thorium from sulfo-phosphoric mixed acid and extracting rare earth chloride. Said process adopts primary amine added mixed alcohol as extracting agent, and makes direct fractionation of rare earth slurry to extract thorium, and the thorium content in the separated rare earth slurry is ThO2 / REO is less than or equal to 5X10 to the minus sixth. Said invention utilizes the thorium being in organic phase and adopts countercurrent reextraction process by means of nitric acid to obtain thorium nitrate product, its purity is 99%, and thorium recovery is up to 99%. Said invention adopts magnesium oxide precipitation method to remove the iron and phosphorus in the rare earth reffinate, uses ammoniated P507-kerosene to extract organic phase.

Description

Technical field: [0001] The invention belongs to a process for extracting and separating thorium from sulfur-phosphorus mixed acid system and extracting rare earth chloride. Background technique: [0002] Chinese patent 98122348.6 discloses a process for extracting and separating cerium and thorium from bastnaesite leaching solution. This patent uses the organic phase composed of extractant TRPO-alkane to extract cerium (IV) by fractional distillation to obtain an organic phase containing cerium and a raffinate containing rare earth and thorium. CeO in organic phase 2 / REO is 99%~99.99%, ThO 2 / CeO 2 Less than 0.01%. The thorium in the raffinate is fractionated and extracted with 0.5%-10% primary amine RNH2-alkane and 1%-10% mixed alcohol as the organic phase to obtain the raffinate containing thorium-containing organic phase, rare earth and iron. Thorium is back-extracted with 0.5-3 mol / L nitric acid, and the recovery rate of thorium reaches 99%. The thorium-extractin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F15/00C01F17/00C22B3/28C22B3/40C22B59/00C22B60/02
CPCY02P10/20
Inventor 李德谦左勇白彦王忠怀
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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