# US 8,785,691 B2 · Dialkyldiaza-tetraalkyloctane diamide derivatives useful for the separation of trivalent actinides from lanthanides and process for the preparation thereof

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- Number: US 8,785,691 B2
- Document ID: US8785691B2
- Status: Granted
- Kind: B2
- Application number: 13/388,000
- Filed: 2009-09-11
- Published: 2012-07-05
- Granted: 2014-07-22
- Earliest claimed: 2009-07-30
- Assignees: Secretary, Department of Atomic Energy
- Applicants: Joti Nath Sharma; Ritesh Ruhela; Smitha Manohar; Piaray Kishen Wattal; Ashok Kumar Suri
- Inventors: Joti Nath Sharma; Ritesh Ruhela; Smitha Manohar; Piaray Kishen Wattal; Ashok Kumar Suri
- Web page: https://patentgrep.com/patent/US8785691B2

## CPC

- C07C 237/02: having the carbon atoms of the carboxamide groups bound to acyclic carbon atoms of the carbon skeleton
- C07C 237/06: having the nitrogen atoms of the carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms
- C22B 3/32: Carboxylic acids
- C22B 59/00: Obtaining rare earth metals
- G21C 19/46: Aqueous processes {, e.g. by using organic extraction means, including the regeneration of these means}
- G21F 9/125: {by solvent extraction}
- C07C 231/12: by reactions not involving the formation of carboxamide groups
- Y02E 30/30: Nuclear fission reactors
- Y02P 10/20: Recycling
- Y02W 30/50: Reuse, recycling or recovery technologies
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C22B: PRODUCTION AND REFINING OF METALS (electrolytic C25); PRETREATMENT OF RAW MATERIALS
- G21C: NUCLEAR REACTORS (fusion reactors, hybrid fission-fusion reactors G21B; nuclear explosives G21J)
- G21F: PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR (radiation protection by pharmaceutical means A61K8/00, A61Q17/04; in cosmonautic vehicles B64G1/54; combined with a reactor G21C11/00; combined with X-ray tubes H01J35/16; combined with X-ray apparatus H05G1/02)
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02W: CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT

## Abstract

The novel lipophilic metal extractants of the class dialkyldiaza-tetraalkyloctanediamide (DADA) useful to selectively separate trivalent americium (sup. 241 Am) from trivalent lanthanides are represented by the formula 1: Wherein R is a C1 to C5 normal alkyl and R′ is a C4 to C8 normal and branched alkyl group. The compounds are synthesized at high yield and purity by the reaction of corresponding N,N′-dialkylethylenediamine and N,N-dialkyl-2-chloroacetamide. The separation is achieved by utilizing the soft-soft interaction between the trivalent actinides and ‘N’ atoms of the extractant. Both soft donor “n” and hard donor ‘O’ sites are incorporated in the molecule for better extraction of trivalent actinides over trivalent lanthanides. Thus, this molecule can be used as selective extractant to separate trivalent actinides from trivalent lanthanides.

## Claims

### Claim 1

A lipophilic extractant capable of selectively extracting trivalent actinides from lanthanide ions, represented by the following structural formula:
wherein R is a C4 to C5 normal alkyl and R′ is a C4 to C8 normal and branched alkyl group.

### Claim 2

A process for the preparation of lipophilic extractant represented by the following structural formula:
wherein R is a C4 to C5 normal alkyl and R′ is a C4 to C8 normal and branched alkyl group;
the process comprising:
condensing one mole of N,N′-dialkylethylenediamine of structural formula:
with 2.2 to 5.0 moles of N,N-dialkyl-2-chloroacetamide of structural formula:
in the presence of 2.2 to 10 moles of triethylamine as a reaction mixture;
diluting the reaction mixture with xylene and neutralizing with 1.0M hydrochloric acid to produce an organic phase;
separating the organic phase and washing it with water and 2.0% sodium carbonate solution and further washing it with water to neutral pH;
drying the organic phase with anhydrous sodium sulphate and concentrating by distillation under reduced pressure to produce a residue;
distilling the residue at 120° C. under vacuum of about 1.0 millitorr using centrifugal molecular distillation unit to remove unreacted N,N-dialkyl-2-chloroacetamide;
obtaining the lipophilic extractant at a purity of about 96%.

### Claim 3 (depends on 2)

The process as claimed in claim 2, being carried out at a temperature of 60-85° C. for 48 hrs in N2 atmosphere.