SU1439080A1 - Method of group separation of rare-earth elements - Google Patents

Abstract

The invention relates to methods for the group separation of rare earth elements (REE) and makes it possible to increase the coefficient of group separation. To a saturated isopropanol – nrmu solution of anhydrous chlorides of a mixture of REEs, acetylacetone imine-Å is added in a super-specimen amount based on the formation of a complex with a molar ratio of acetylacetomine and REE 3: 1. The precipitate containing the REE of the yttrium group is separated from the solution containing the REE of the cerium group. With a single precipitation, a separation is achieved, characterized by a separation coefficient of 1600. With the use of the known method, the value of the separation coefficient is 100. W

Description

NU

00

with

one

The invention relates to methods for separating rare-earth elements (REE) and can be used in chemical technology for group division of the amount of REE, mineralized, into cerium and yttrium subgroups of I.PI in separating individual elements of deerium and yttrium

The precipitation of REE in this example occurs as a result of the formation of a relatively poorly soluble complex of REE with acetylacetoninum (denoted by 0). The MClj 3Q complexes are not described in the literature; examples of the synthesis of individual complexes are given below.

subgroups in artificial mixtures, Q REE chlorides with acetylacetonimine. The individuality of the obtained complexes is proved by the methods of elemental analysis, IR spectroscopy, X-ray phase and thermal analysis.

PRI me R 2, Sex YbClySQ. 1.71 g Yhtlj dissolved in 200 ml

included in the composition of ceramics or other materials during their regeneration or analysis.

The aim of the invention is to increase the ratio of group separation of jenium, which will provide the possibility of a single treatment of the solution of chlorides of the amount of REE (or a mixture of representatives of the cerium and yttrium subgroups) of the complex.

PRI and CHER 1. Separation of a mixture of NdClj and YbClj.

To a mixture of finely divided NdClj and YbCl, taken in an amount of 1.25 nizopropanol, the solution is heated to 35-40 ° C and 2.42 g of acetylacetoneimine is added. The mixture of reagents is stirred in a closed vessel for 3 hours, the precipitated precipitate is separated by filtration and dried in vacuum (mm Hg) at 70 ° C. Yield 90%. Similarly, can be obtained

1.40 g, respectively (molar, corresponding to 25% yield from 73 to 90% complexes, NdrYb 1: 1 reduction), 450 ml of isopropanol, 4 g of acetylacetonimine are added and mixed thoroughly for 5 hours. An isopr. Ethanol solution is obtained,

REID Y and elements from Gd to Lu inclusive.

PRI me R 3. Getting.

A mixture of 0.97 g NdCl, 1.53 g at aceneodymium, and a precipitate containing ytterdyl tilacetonimine and 400 ml of isopropanol

biy

Products are analyzed as follows. The precipitate formed is filtered off, washed with a small amount of isopropanol, dissolved in 100 ml of water, and oxalates of Yb and Nd are precipitated with a solution of oxalic acid saturated at room temperature. The filtrate is evaporated to dryness, the residue is dissolved in 100 ml of water and REE oxalates are precipitated by this method. Oxate oxides are dried at 140 ° C and converted to oxides by calcination at. Oxide charge

35

40

to 40 ° C and stirred in a closed vessel until the reagents are completely dissolved. Greater than in example 2, the volume of solvent is necessary due to the significantly lower solubility of NdCl. compared with bC1, in isopropanol. The solution is evaporated in vacuo (10-15 mmHg) to a viscous syrupy form, 20 m of petroleum ether is added, mixed thoroughly, the precipitate is filtered off and dried in vacuum (10 mmHg at 70 ° C. Yield 70 %. Similarly, it can be obtained 5tc1z sp.

dissolved in a minimum amount of hydrochloric acid, made up to 50 ml with water and analyzed for neodymium content by a spectrophotometric method (- 521, 6 nm).

The mixture of oxides obtained from the precipitate contains 0.4% NdjO and 99.6% (molar ratio Nd: Yb 1: 236), the mixture of oxides from isopropanol filtrate — 86.8% and 13.2% YbaOj ( molar ratio NdrYb 7.7: 1).

About 90% of ytterbi is precipitated. The coefficient for the Yb-Nd blend is greater than 1600.

isopropanol, the solution is heated to 35-40 ° C and 2.42 g of acetylacetonimine is added. The mixture of reagents is stirred in a closed vessel for 3 hours, the precipitated precipitate is separated by filtration and dried in vacuum (mm Hg) at 70 ° C. Yield 90%. Similarly, can be obtained

REID Y and elements from Gd to Lu inclusive.

PRI me R 3. Getting.

A mixture of 0.97 g NdCl, 1.53 g acetylacetonimine and 400 ml isopropanol

to 40 ° C and stirred in a closed vessel until the reagents are completely dissolved. Greater than in example 2, the volume of solvent is necessary due to the significantly lower solubility of NdCl. compared with bC1, in isopropanol. The solution is evaporated in vacuo (10-15 mmHg) to a viscous syrupy form, 20 ml of petroleum ether is added, mixed thoroughly, the precipitate is filtered off and dried in vacuum (10 mmHg) at 70 C. Yield 70%. Similarly, it can be obtained 5tc1z sp.

The need to use a saturated solution follows from the fact that with an excess of solvent, readily soluble and poorly soluble complex compounds are present in the solution. This leads to a significant decrease in the group separation coefficient.

Claims (1)

Invention Formula The method of group separation of rare-earth elements into cerium and yttrium subgroups by adding to - 1439080- a solution of rare earth chlorides of elec- tric is added to the specific grades of the complexing agent with a post-pan anhydrous solution and the separation of the filtrate from the precipitates of the mixture of rare earth elements ka, which is limited by the amount of excess stoichiometry with the aim of increasing the for the separation of the complex with a molar pickle, acetylacetonimine, a co-earth element of 3: 1, is used as the complex-forming ratio of acetylacetonimine and rarely.