ChemRxiv
A first example of diglycolamide flow synthesis was developed, showcasing algorithm-accelerated reaction optimization and its potential to accelerate ligand discovery and enable autonomous, AI controlled manufacturing of critical materials.
The increasing demand for manufacturing rare-earth elements (REEs) as critical materials has intensified research on sustainable synthesis of advanced extractants such as diglycolamides (DGAs). The development of ligands involves substrate scope development, process optimization, at-scale production, and separation evaluation. These components are typically disconnected in a conventional workflow, which is therefore time-consuming and labor-intensive. To accelerate extractant development and impact manufacturing, we present a streamlined workflow for DGAs that includes continuous-flow ligand synthesis and automated evaluation for REEs solvent extraction. The synthesis of DGAs is achieved using a digitized flow reactor, which enables online spectroscopic monitoring and control of residence time, temperature, and reactant stoichiometry. The use of Rxn Rover automation software enables artificial intelligence (AI) algorithm supervision to minimize the steps and time for process optimization by over 40%. A substrate scope of 7 structurally diverse DGAs was synthesized in yields up to 90% upon optimization. The process optimization mode can be seamlessly scaled up to mass production, yielding 19 grams of the high-extraction-efficiency ligand N,N′-dimethyl-N,N′-dioctyldiglycolamide (DMDODGA) over 48 hours of continuous operation. The ligands synthesized at scale can be used for highthroughput evaluation of liquid-liquid (L-L) extraction against 14 lanthanides (Ln) on a robotic platform. This work highlights the power of combining automated synthesis with applicationdriven testing to accelerate the discovery of functional ligands, laying the foundation for fully closed-loop, AI-controlled platforms for the smart and autonomous manufacturing of critical materials.
For details:
Continuous Flow Synthesis of Diglycolamides for Rare-Earth Elements Recovery: Algorithm-Accelerated Reaction Optimization Coupled with Automated Extraction Evaluation
Lun An 1, Zachery Crandall 1, Dulitha Prasanna Kulathunga 2, John Brittain 1, Elijah Jibben 1, Hailey M. Bates 1, Tyler B. Hall 1, Theresa L. Windus 1,2, Long Qi 1
1) U.S. DOE Ames National Laboratory Iowa State University
2) Department of Chemistry Iowa State University
ChemRxiv
https://chemrxiv.org/doi/full/10.26434/chemrxiv.15001636/v1
