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A kind of industrial grade thulium raw material prepares 5n thulium method

An industrial-grade, raw material technology, applied in the direction of improving process efficiency, etc., to achieve the effects of high product purity, optimized separation section, and large production scale

Inactive Publication Date: 2017-12-12
NANCHANG HANGKONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] It is not difficult to see that there has been no report on the direct preparation of 5N grade high-purity thulium products by solvent extraction.

Method used

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  • A kind of industrial grade thulium raw material prepares 5n thulium method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1) YErTm / TmYbLu separation section

[0042] The first step is the YErTm / TmYbLu full-load fractionation extraction separation section to realize the separation of YErTm / TmYbLu. The C272 rare earth saponified organic phase with a saponification rate of 0.30 from the fourth step enters from the first stage of the YErTm / TmYbLu full-load fractionation extraction system, the rare earth concentration is 0.80mol / L, the ratio of the molar concentration of thulium to the molar concentration of rare earth is 0.995, and the pH The thulium chloride feed solution with a value of 4 enters from the 10th stage of the YErTm / TmYbLu full-load fractionation extraction system, and the raffinate aqueous thulium chloride ytterbium lutetium solution from the third step acid extraction section enters the YErTm / TmYbLu from the 30th stage as a detergent. TmYbLu fully loaded fractional distillation extraction system. The YErTm feed liquid is obtained from the first-stage raffinate aqueous phase of...

Embodiment 2

[0063] 1) YErTm / TmYbLu separation section

[0064] The first step is the YErTm / TmYbLu full-load fractionation extraction separation section to realize the separation of YErTm / TmYbLu. The C272 rare earth saponified organic phase with a saponification rate of 0.30 from the fourth step enters from the first stage of the YErTm / TmYbLu full-load fractionation extraction system, the rare earth concentration is 0.6mol / L, the ratio of the molar concentration of thulium to the molar concentration of rare earth is 0.999, pH The thulium chloride feed solution with a value of 5 enters from the 9th stage of the YErTm / TmYbLu full-load fractionation extraction system, and the raffinate aqueous thulium chloride ytterbium lutetium solution from the third step acid extraction section enters the YErTm / TmYbLu from the 26th stage as a detergent. TmYbLu fully loaded fractional distillation extraction system. The YErTm feed liquid is obtained from the first-stage raffinate aqueous phase of the YErTm...

Embodiment 3

[0085] 1) YErTm / TmYbLu separation section

[0086]The first step is the YErTm / TmYbLu full-load fractionation extraction separation section to realize the separation of YErTm / TmYbLu. The C272 rare earth saponified organic phase with a saponification rate of 0.30 from the fourth step enters from the first stage of the YErTm / TmYbLu full-load fractionation extraction system. The thulium chloride feed liquid with a value of 3 enters from the 12th stage of the YErTm / TmYbLu full-load fractionation extraction system, and the raffinate aqueous thulium chloride ytterbium lutetium solution from the third step acid extraction section enters the YErTm / TmYbLu from the 35th stage as a detergent. TmYbLu fully loaded fractional distillation extraction system. The YErTm feed liquid is obtained from the first-stage raffinate aqueous phase of the YErTm / TmYbLu full-load fractionation extraction system, in terms of moles of rare earths, of which 79.2785% is used in the fourth step of rare earth sa...

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Abstract

A method for preparing 5N thulium from industrial-grade thulium raw materials in the present invention uses 2N-3N grade thulium chloride as feed liquid, acidic phosphine reagent C272 as extraction agent, and TBP as additive for extracting organic phase, including 12 steps, including 3 separation steps and 5 auxiliary steps; the 3 separation steps are respectively YErTm / TmYbLu separation, YEr / Tm separation and Tm / YbLu separation section, and the 5 auxiliary steps are respectively concentration section, acid extraction section, saponification section, stripping section and soap Chemical section. YEr / Tm separation is in tandem with Tm / YbLu separation. The invention can obtain 5N grade high-purity thulium products with a relative purity of 99.9990% to 99.9996%, and the yield reaches 94.39% to 98.29%. The invention has the advantages of high thulium product purity, high thulium product yield, large production scale, less consumption of chemical reagents, simple and convenient operation, low production cost and the like.

Description

technical field [0001] The invention relates to a method for preparing 5N thulium from industrial-grade thulium raw materials, in particular to using 2N-3N grade thulium chloride solution as the feed liquid, di(2,4,4-trimethylpentyl)phosphonic acid (abbreviated as C272 or Cyanex272) is the extractant, tributyl phosphate (abbreviated as TBP) is the additive for extracting the organic phase, and an extraction and separation process for preparing thulium products with a purity of ≥99.999%. The invention belongs to the technical field of rare earth separation in solvent extraction. Background technique [0002] Thulium is widely used in high-tech fields such as fluorescent materials, magnetic bubble materials, laser materials, and optical glass materials. The purity of thulium products is one of the key factors affecting the performance and function of related thulium materials, so improving the purity of thulium products has important practical significance. Thulium products ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B59/00C22B3/38
CPCC22B59/00C22B3/3846Y02P10/20
Inventor 钟学明
Owner NANCHANG HANGKONG UNIVERSITY