scholarly journals Continuous and scalable synthesis of a porous organic cage by twin screw extrusion (TSE)

2020 ◽  
Vol 11 (25) ◽  
pp. 6582-6589 ◽  
Author(s):  
Benjamin D. Egleston ◽  
Michael C. Brand ◽  
Francesca Greenwell ◽  
Michael E. Briggs ◽  
Stuart L. James ◽  
...  

Twin screw extrusion (TSE) is demonstrated as an alternative synthetic method for preparing a prolific porous organic cage.

2020 ◽  
Author(s):  
Benjamin Egleston ◽  
Michael C. Brand ◽  
Francesca Greenwell ◽  
Michael E. Briggs ◽  
Stuart L. James ◽  
...  

The continuous and scalable synthesis of a porous organic cage (<b>CC3</b>), obtained through a 10-component imine polycondensation between triformylbenzene and a vicinal diamine, was achieved using twin screw extrusion (TSE). Compared to both batch and flow syntheses, the use of TSE enabled the large scale synthesis of <b>CC3</b> using minimal solvent and in short reaction times, with liquid-assisted grinding (LAG) also promoting window-to-window crystal packing to form a 3-D diamondoid pore network in the solid state. A new kinetically trapped [3+5] product was also observed alongside the formation of the targeted [4+6] cage species. Post-synthetic purification by Soxhlet extraction of the as-extruded ‘technical grade’ mixture of <b>CC3</b> and [3+5] species rendered the material porous.


2020 ◽  
Author(s):  
Benjamin Egleston ◽  
Michael C. Brand ◽  
Francesca Greenwell ◽  
Michael E. Briggs ◽  
Stuart L. James ◽  
...  

The continuous and scalable synthesis of a porous organic cage (<b>CC3</b>), obtained through a 10-component imine polycondensation between triformylbenzene and a vicinal diamine, was achieved using twin screw extrusion (TSE). Compared to both batch and flow syntheses, the use of TSE enabled the large scale synthesis of <b>CC3</b> using minimal solvent and in short reaction times, with liquid-assisted grinding (LAG) also promoting window-to-window crystal packing to form a 3-D diamondoid pore network in the solid state. A new kinetically trapped [3+5] product was also observed alongside the formation of the targeted [4+6] cage species. Post-synthetic purification by Soxhlet extraction of the as-extruded ‘technical grade’ mixture of <b>CC3</b> and [3+5] species rendered the material porous.


Polymers ◽  
2021 ◽  
Vol 13 (13) ◽  
pp. 2128
Author(s):  
Paulo F. Teixeira ◽  
José A. Covas ◽  
Loïc Hilliou

The dispersion mechanisms in a clay-based polymer nanocomposite (CPNC) during twin-screw extrusion are studied by in-situ rheo-optical techniques, which relate the CPNC morphology with its viscosity. This methodology avoids the problems associated with post extrusion structural rearrangement. The polydimethylsiloxane (PDMS) matrix, which can be processed at ambient and low temperatures, is used to bypass any issues associated with thermal degradation. Local heating in the first part of the extruder allows testing of the usefulness of low matrix viscosity to enhance polymer intercalation before applying larger stresses for clay dispersion. The comparison of clay particle sizes measured in line with models for the kinetics of particle dispersion indicates that larger screw speeds promote the break-up of clay particles, whereas smaller screw speeds favor the erosion of the clay tactoids. Thus, different levels of clay dispersion are generated, which do not simply relate to a progressively better PDMS intercalation and higher clay exfoliation as screw speed is increased. Reducing the PDMS viscosity in the first mixing zone of the screw facilitates dispersion at lower screw speeds, but a complex interplay between stresses and residence times at larger screw speeds is observed. More importantly, the results underline that the use of larger stresses is inefficient per se in dispersing clay if sufficient time is not given for PDMS to intercalate the clay galleries and thus facilitate tactoid disruption or erosion.


2013 ◽  
Vol 80 (3) ◽  
Author(s):  
Thelma G. Manning ◽  
Joseph Leone ◽  
Martijn Zebregs ◽  
Dinesh R. Ramlal ◽  
Chris A. van Driel

In order to eliminate residual solvents in ammunition and to reduce the emissions of volatile organic compounds to the atmosphere, the U.S. Army ARDEC has teamed with TNO in developing a new process for the production of solventless propellant for tank ammunition. To reduce the costs of solventless propellants production, shear roll mill and continuous extrusion processing was investigated. As described in this paper JA-2 a double base propellant cannot be processed without solvent by the extrusion process. An alternative JA-2 equivalent propellant was defined. The aim of this work is to demonstrate the manufacturing of this propellant by solventless continuous twin screw extrusion processing while maintaining gun performance characteristics of conventional JA-2 propellant. This is elucidated by explicitly researching the relationship between interior ballistic properties of the gun propellant and utilizing a continuous manufacturing process. Processing conditions were established, and the propellant was manufactured accordingly. The extruded propellant has the desired properties, which resulted in a comparable gun performance as the conventional JA-2 propellant.


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