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Method for separating lanthanide series elements

A lanthanide, thermal method, applied in chemical instruments and methods, crystal growth, liquid solvent solutions at room temperature, etc. Efficient crystallization separation, avoiding multiple separations, and low cost

Active Publication Date: 2016-12-07
SUZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the traditional fractional crystallization method, the biggest deficiency in the example of complexing crystals with lanthanides and precipitated ions is that most of the precipitated ions form one component from La to Lu, and most precipitated ion systems have no more than two components.
In the phosphate fractional crystallization system, the separation ratio of adjacent elements is between 1.1 and 1.5. This value does not depend on the initial ratio of lanthanides. Lanthanides can be purified through multiple separations and dissolutions. The defect of this technology is that the separation ratio is low. The number of separations required is tedious, and the purification of lanthanides takes a long time, etc.

Method used

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  • Method for separating lanthanide series elements
  • Method for separating lanthanide series elements
  • Method for separating lanthanide series elements

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Embodiment one: the separation of neodymium samarium (NdSm)

[0041] 0.3mmol NdCl 3 ·6H 2 O, 0.3 mmol SmCl 3 ·6H 2 O and 4.5 mmol H 3 BO 3 Put it in a 10ml polytetrafluoroethylene reaction kettle, add 0.1ml deionized water, seal it, heat up to 190°C, heat for 3 days, then cool to room temperature at a rate of 3-4oC / h, wash the product with a large amount of boiling water, and wash the lotion Collect them into a 100ml volumetric flask and make up to volume, and the resulting crystalline product is washed with ethanol and dried at room temperature.

[0042] The resulting crystals were characterized by a powder diffractometer, such as Figure 4Shown, prove that this doping reaction only generates the crystal of a kind of structure type, and this crystal has identical structure with NdBOCl crystal; Crystal is first dissolved with concentrated nitric acid, then diluted to low acidity, with inductively coupled plasma mass spectrometer ( ICP-Ms) measure the concentratio...

Embodiment 2

[0043] Embodiment two: the separation of neodymium dysprosium (NdDy)

[0044] 0.3mmolNdCl 3 ·6H 2 O, 0.3mmol DyCl 3 ·6H 2 O and 4.5 mmol H 3 BO 3 Put it in a 10ml polytetrafluoroethylene reaction kettle at a ratio of 1:1:15, add 0.1ml of deionized water, seal it, heat it up to 200°C, heat it for 3 days, and then cool it to room temperature at a rate of 3-4oC / h. After washing with a large amount of boiling water, the obtained crystal product was washed with ethanol and dried at room temperature, and the washing liquid was collected into a 100ml volumetric flask to constant volume.

[0045] The resulting crystals were characterized by a powder diffractometer, such as Image 6 As shown, it proves that the doping reaction only generates crystals of one structure type, and the crystals have the same structure as NdBOCl crystals; the crystals are first dissolved with concentrated nitric acid, then diluted to low acidity, and analyzed by an inductively coupled plasma mass spect...

Embodiment 3

[0046] Embodiment three: the separation of neodymium dysprosium (NdDy)

[0047] 0.3mmolNdCl 3 ·6H 2 O, 0.3mmol DyCl 3 ·6H 2 O and 6.0 mmol H 3 BO 3 Put it in a 10ml polytetrafluoroethylene reaction kettle at a ratio of 1:1:20, add 0.1ml of deionized water, seal it, heat it up to 210°C, heat it for 7 days, and then cool it to room temperature at a rate of 3-4oC / h. Wash with a large amount of boiling water, wash the product crystals with ethanol and dry at room temperature, and collect the washing liquid into a 100mL volumetric flask to constant volume.

[0048] The resulting product was characterized by a powder diffractometer, such as Figure 8 As shown, it was proved that the product contained three crystal types (NdBOCl, DyBO-1 and DyBO-2) with different structures.

[0049] Put the product in bromoform, stir well, let it stand for a period of time, and selectively suspend or precipitate in the bromoform solution due to the different densities of crystals of different...

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Abstract

The invention provides an environment-friendly, efficient and low-cost method for separating lanthanide series elements. The method comprises the following steps that crystals are generated by the lanthanide series elements and boric acid through a fusing hot method, and the crystals of the same structure are separated from crystal lotion or separation is achieved according to drifting in solvent due to the different densities of the crystals of the different structures. The separating method makes selective polymerization for different kinds of lanthanide series metal on the basis of the flexible ligand boric acid, the lanthanide series components are synthesized under the uniform reaction condition for the first time, the lanthanide series elements are divided into six different components, the crystal density is closely related to the crystal structure, the high separation ratio in the binary lanthanide series elements can be achieved, compared with traditional sub-step crystallization, multiple times of separation caused by the low separation ratio is avoided, and generation of a large amount of effluent is avoided.

Description

technical field [0001] The invention relates to an element separation method, in particular to a lanthanoid separation method. Background technique [0002] Lanthanides refer to the elements that fill up the 15 f-orbitals from No. 57 lanthanum to No. 71 lutetium in the periodic table of elements. Due to the contraction effect of lanthanides, the 3+ to Lu 3+ The ionic radius is reduced by less than 22%, and the adjacent lanthanide radius is only gap; chemically, all lanthanides are usually in the stable trivalent form Ln 3+ exist. This makes lanthanides often exist in the form of companions, and the separation and purification of single lanthanides in multi-component or binary components has always been a hot spot in the development of lanthanide separation technology. The separation of lanthanides mainly includes selective oxidation, selective reduction, fractional crystallization, ion exchange, solvent extraction and other methods. [0003] For some lanthanides that c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B59/00C30B29/12C30B29/22C30B7/14
CPCC22B59/00C30B7/14C30B29/12C30B29/22
Inventor 王殳凹尹雪苗王亚星
Owner SUZHOU UNIV
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