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Inactive experiments for advanced separation processes prior to high activity trials in ATALANTEJ. Duhamet, J.-Y. Lanoë, P. Rivalier, G. Borda

Introduction

The search for new hydrometallurgical processes for minor actinide separation has led the CEA to develop suitable apparatus for carrying out feasibility tests on representative aqueous solutions produced by the dissolution of irradiated nuclear fuels.Two major constraints had to be taken into account: on the one hand, the need to reduce the amount of effluents produced by the trials as much as possible, and on the other, the need to use laboratory apparatus whose results could reliably be extrapolated to industrial-scale equipment.

Several types of apparatus were developed or adapted to meet these criteria.

Conclusions

P1-03

Extraction apparatus developed to meet Atalante's needs

The approach adopted

Stockage solvant

COLONNE COUETTE 2type CBP

Lavage Ln 3BSCOLONNE COUETTE 3

type CBPDésextraction An 3BX

A/O=0,51

TPHQ: mL/h

Désextraction Zr,Fe3CXX

Acidif icationQ : mL/h]

Traitement soude

Désextraction8 ECLHA

3HAAECRANS

COLONNE COUETTE 1type CBP

Extraction-lavage 3AX+3AS

COLONNE COUETTE 4type CBP

Désextraction Ln 3CX

Lavage 3ASQ : mL/h[HNO3]

Charge aqueuse : 3AFQ : mL/h

[HNO3] : N

Charge aqueuse dedémarrage et de chasse

[HNO3] :

RaffinatQ : mL/h

Solvant recyclé 3AX

Solvant recyclé 3BSQ: mL/h

Sortie AnQ :mL/h

Désextraction AnQ : mL/h

Sortie LnQ :mL/h

Désextraction LnQ : mL/h[HNO3]

Sortie Ln

Légende

Analyse en ligne

Echantillonnage

Flux aqueux

Flux organiques

E 14P

ANL NdHellma

Densimètre Anton-Paar

ANL Nd tuyau

E 12

E 11

E 24

E 23

E 22

E 21

E 34

E 33

E 32

E 31

E 45

E 44

E 43

E 42

E 25P

E 35P

E 41P

3AP

3BSW 3BW 3CXW

3CW

SO3HAA

3HAAW3AW 3BP

3BXP3CLn

pH 1

pH 2(secours)

3CXXW

1 1

1

Pompe àengrenages

ou piston

Pompe àpiston C11/C12 Pompe à

piston C11/C12

pompe20 L

pompe

Pompe àengrenages

ou piston

Seringueplastique

1Pot type C11/C12

pompe

TPH

PompeSTEPDOS

PD 11

COM 6

HE BLNC 04

COM 8

HE BLNC 30

COM 9

HE BLNC 03

COM 10

HE BLNC 32

HNO3

Pompe àpiston C11/C12

COM 5

HE BLNC 31

Clapetanti-retour

ANLNd , FeT. Davin

E 13P

3AX

ANLNd, Fe

T. Davin

PD 17

PD 08

Péristaltique

PD 07

PD 01

ANLrefracto

COM 4

EA3BS

Several steps can be identified prior to high activity trials:- Apparatus design in consultation with the teams in charge of the high activity trials, so as to be fully aware of the special issues regarding its implementation in a shielded cell: bulk, ease of dismantling, limited accessibility, etc.- Follow-up of the apparatuses’ construction,- Individual checking of hydraulic operation with water, then with phases representative of those used in the separation processes- Implementation of separation processes coupling the different apparatus chosen under inactive conditions.

Results

From theoretical scheme to implementation of liquid/liquid extraction process

DIAMEX TRIALS IN COUETTE-TAYLOR COLUMNS

These trials in pulsed columns were also the opportunity to see that the breakdown of a vital element (in this case, the solvent pump) and its replacement in 3 hours, given the longer time imposed by the difficulties of working in a shielded cell, do not mean the trial has failed and that restarting following a suitable procedure enables a return to a state of equilibrium.The on-line spectrophotometry monitoring of the neodymium content of the back-extraction aqueous phase after restarting the solvent pump shows that equilibrium is recovered in less than 1.5 hour.

It was necessary to have columns with hydrophobized internal surfaces, in order to be able to function in continuous organic phase mode. A silanization treatment to the glass external cylinder was applied, and the stainless steel rotor was coated with a Teflon film.

Trials run for the whole process showed that precipitates appeared in the extraction column. Their analysis showed them to be lanthanide oxalates linked to the use of oxalic acid as a complexing agent. Overly weak acidity in the washing step caused these precipitates to appear. Analysis of the trial results enabled the modelling team to suggest a modified process flowchart.

DIAMEX TRIALS IN PULSED COLUMNS

Some column hydraulic malfunctions were identified, coming from wetting effects of the aqueous phase on the internal surfaces which very significantly reduced the interfacial exchange area. A hydrophobization treatment in situ for the columns has been used. The result obtained (showed that it was possible to establish a satisfying emulsion in the column.

Phase inversion on hydrophilic surfaces

Good hydrodynamic conditions with hydrophobic surfaces

Phase inversion on hydrophilic surfaces

Emulsion sticking to the walls of a non hydrophobized column

Emulsion in a hydrophobized column

These inactive trials, carried out in G1 facility, have demonstrated that it has been of primary importance to create a mock-up as representative as possible of the most significant apparatuses’ location as planned for the shielded line in order to identify implementation problems and find solutions more easily. It was also the opportunity to train the personnel in the implementation of the new separation processes in a less complex, more easily-understood environment.

Solvent

Feed

Extractioncolumm

Back extr.columm

Scrubcolumm

Solvent pump