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Separation process for coproduction of pure dysprosium and pure thulium by fractional extraction

An extraction and process technology, which is applied in the field of separation process of fractional distillation extraction and co-production of pure dysprosium and pure thulium, can solve the problems of low qualified rate of 4N grade products, poor process stability, low consumption of acid and alkali, and saves neutralizing reagents, The effect of reducing extraction waste and acid-base consumption

Inactive Publication Date: 2018-12-28
NANCHANG HANGKONG UNIVERSITY
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Problems solved by technology

[0004] A separation process for fractional extraction and co-production of pure dysprosium and pure thulium according to the present invention aims at the existing fractional distillation extraction process for preparing 4N-grade dysprosium chloride and 4N-grade thulium chloride, which has large acid-base consumption, poor process stability, and 4N-grade product qualification rate Lower deficiency provides a method for co-producing 4N grade dysprosium chloride and 4N grade thulium chloride with low acid-base consumption and high pass rate of 4N grade products

Method used

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  • Separation process for coproduction of pure dysprosium and pure thulium by fractional extraction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The organic phase of saponified P229 is 30% by volume of P229 in the kerosene solution of extractant P229, and the saponification rate is 36%.

[0031] The pH of 2N~3N dysprosium chloride solution is 3, and the concentrations of rare earth elements are: Gd 0.030g / L, Tb 0.20g / L, Dy 160.0g / L, Ho 0.30g / L, Y 0.050g / L, Er 0.030g / L.

[0032] The pH of 2N~3N grade thulium chloride solution is 2~4, and the concentrations of rare earth elements are: Ho 0.020g / L, Y 0.050g / L, Er 0.20g / L, Tm 165.0g / L, Yb 0.50g / L , Lu 0.10g / L.

[0033] Step 1: Fractional distillation and extraction to separate GdTbDy / DyHoYEr

[0034] The saponified P229 organic phase is used as the extraction organic phase, the 2N-3N grade dysprosium chloride solution is used as the first feed solution, and 3.0mol / L HCl is used as the washing acid. The saponified P229 organic phase enters the GdTbDy / DyHoYEr fractional extraction system from the first stage, the first feed liquid enters the GdTbDy / DyHoYEr fraction...

Embodiment 2

[0049] The organic phase of saponified P229 is 30% by volume of P229 in the kerosene solution of extractant P229, and the saponification rate is 36%.

[0050] The pH of 2N~3N dysprosium chloride solution is 2, and the concentrations of rare earth elements are: Gd 0.050g / L, Tb0.30g / L, Dy165.0g / L, Ho 0.60g / L, Y 0.10g / L, Er 0.050g / L.

[0051] The pH of 2N~3N thulium chloride solution is 2, and the concentrations of rare earth elements are: Ho 0.0040g / L, Y0.10g / L, Er0.30g / L, Tm 170.0g / L, Yb 0.90g / L, Lu 0.20g / L.

[0052] Step 1: Fractional distillation and extraction to separate GdTbDy / DyHoYEr

[0053] The saponified P229 organic phase is used as the extraction organic phase, the 2N-3N grade dysprosium chloride solution is used as the first feed solution, and 3.0mol / L HCl is used as the washing acid. The saponified P229 organic phase enters the GdTbDy / DyHoYEr fractional extraction system from the first stage, the first feed liquid enters the GdTbDy / DyHoYEr fractional extraction ...

Embodiment 3

[0068] The organic phase of saponified P229 is 30% by volume of P229 in the kerosene solution of extractant P229, and the saponification rate is 36%.

[0069] The pH of 2N~3N dysprosium chloride solution is 4, and the concentrations of rare earth elements are: Gd 0.010g / L, Tb 0.030g / L, Dy 155.0g / L, Ho 0.10g / L, Y 0.010g / L, Er 0.010g / L.

[0070] The pH of 2N~3N thulium chloride solution is 4, and the concentrations of rare earth elements are: Ho 0.0010g / L, Y 0.020g / L, Er 0.10g / L, Tm 160.0g / L, Yb 0.10g / L, Lu 0.010g / L.

[0071] Step 1: Fractional distillation and extraction to separate GdTbDy / DyHoYEr

[0072] The saponified P229 organic phase is used as the extraction organic phase, the 2N-3N grade dysprosium chloride solution is used as the first feed solution, and 3.0mol / L HCl is used as the washing acid. The saponified P229 organic phase enters the GdTbDy / DyHoYEr fractional extraction system from the first stage, the first feed liquid enters the GdTbDy / DyHoYEr fractional ext...

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Abstract

The invention relates to a separation process for coproduction of pure dysprosium and pure thulium by fractional extraction. P229 is used as an extracting agent, a 2N-3N grade dysprosium chloride solution is used as first material liquid, a 2N-3N grade thulium chloride solution is used as second material liquid, and the separation process comprises six steps of fractional extraction and separationof GdTbDy / DyHoYEr, fractional extraction and separation of HoYErTm / TmYbLu, full-load fractional extraction and separation of GdTb / Dy, full-load fractional extraction of Dy / HoYEr, full-load fractionalextraction and separation of HoYEr / Tm and fractional extraction and separation of Tm / YbLu. According to the separation process for the coproduction of the pure dysprosium and the pure thulium by thefractional extraction, two 4N-grade net products of a 4N-grade dysprosium chloride aqueous solution and a 4N-grade thulium chloride aqueous solution are simultaneously obtained through one extractionand separation process flow, and the characteristics of low acid and alkali consumption, good process stability, high product qualification rate, high degree of greening, low production cost and the like are achieved.

Description

technical field [0001] The invention relates to a separation process for fractional extraction and co-production of pure dysprosium and pure thulium. Specifically, P229 is used as the extraction agent, 2N-3N grade dysprosium chloride solution is the first feed liquid, and 2N-3N grade thulium chloride solution is the second feed liquid. Two kinds of feed liquids are prepared simultaneously with a 4N grade dysprosium chloride aqueous solution and a 4N grade thulium chloride aqueous solution. The invention belongs to the technical field of preparing 4N grade dysprosium chloride and 4N grade thulium chloride by a fractional distillation extraction method. Background technique [0002] At present, in the extraction and separation process of rare earth ores, dysprosium obtains a 2N-3N grade dysprosium chloride solution, and thulium also obtains a 2N-3N grade thulium chloride solution. In order to obtain 4N-grade dysprosium products and 4N-grade dysprosium products, extraction and...

Claims

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Application Information

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IPC IPC(8): C22B59/00C22B3/38
CPCC22B59/00C22B3/3844Y02P10/20
Inventor 徐玉娜钟学明
Owner NANCHANG HANGKONG UNIVERSITY
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