US 12,447,459 B1
Polymer-monolith pre-oxidation to improve shape retention during subsequent heat treatment, and monolith produced
Joseph E. Cosgrove, Columbia, CT (US); Michael A. Serio, Sturbridge, MA (US); Marek A. Wójtowicz, Manchester, CT (US); and Andrew E. Carlson, Higganum, CT (US)
Assigned to ADVANCED FUEL RESEARCH, INC.
Filed by ADVANCED FUEL RESEARCH, INC., East Hartford, CT (US)
Filed on Jul. 6, 2022, as Appl. No. 17/858,638.
Claims priority of provisional application 63/220,263, filed on Jul. 9, 2021.
This patent is subject to a terminal disclaimer.
Int. Cl. B01J 20/20 (2006.01); B01J 20/28 (2006.01); B01J 20/30 (2006.01); B33Y 70/00 (2020.01); B33Y 80/00 (2015.01)
CPC B01J 20/20 (2013.01) [B01J 20/28045 (2013.01); B01J 20/3078 (2013.01); B01J 2220/4812 (2013.01); B33Y 70/00 (2014.12); B33Y 80/00 (2014.12)] 15 Claims
 
1. A method for the production of a carbon sorbent monolith for removing at least one gas from a gaseous environment in which the at least one gas is contained, comprising the steps:
(a) producing a shaped polymer monolith using 3-D printing of a polymer precursor consisting essentially of polyether ether ketone (PEEK);
(b) pre-oxidizing said shaped polymer monolith in a flow of an oxidizing gas at a temperature below the melting point of said polymer precursor for a time sufficient to preserve the shape of said polymer monolith during a subsequent carbonizing step;
(c) carbonizing said pre-oxidized shaped polymer monolith of step (b) so as to produce a carbon sorbent monolith by exposure to elevated temperatures in a non-oxidative atmosphere;
and
(d) optionally, activating said carbon sorbent monolith of step (c) by exposure to an oxidizing environment under conditions sufficient to cause a carbon weight loss in said carbon sorbent monolith of at least about 1 weight percent and thereby producing a microporous sorbent monolith with a surface area of at least about 100 m2/g, with the majority of pores being smaller than about 2 nm.