US 11,896,954 B2
Microporous carbon materials to separate nitrogen in associated and non-associated natural gas streams
Federico Jesus Jimenez Cruz, Mexico City (MX); Jose Luis Garcia Gutierrez, Mexico City (MX); Jose Francisco Gaspar Silva Sanchez, Mexico City (MX); Liliana Alejandra Astudillo Lopez Lena, Mexico City (MX); Fidencio Hernandez Perez, Mexico City (MX); Alberto Cabrales Torres, Mexico City (MX); Maria Del Carmen Martinez Guerrero, Mexico City (MX); Marco Antonio Dominguez Aguilar, Mexico City (MX); Arturo Trejo Rodriguez, Mexico City (MX); and Florentino Rafael Murrieta Guevara, Mexico City (MX)
Assigned to INSTITUTO MEXICANO DEL PETROLEO, Mexico City (MX)
Filed by INSTITUTO MEXICANO DEL PETROLEO, Mexico City (MX)
Filed on Jun. 17, 2021, as Appl. No. 17/350,468.
Application 17/350,468 is a division of application No. 16/146,502, filed on Sep. 28, 2018, granted, now 11,059,027.
Claims priority of application No. a/2017/012563 (MX), filed on Sep. 29, 2017.
Prior Publication US 2021/0308652 A1, Oct. 7, 2021
Int. Cl. B01J 20/285 (2006.01); B01D 53/02 (2006.01); B01J 20/20 (2006.01); B01J 20/28 (2006.01); B01J 20/30 (2006.01)
CPC B01J 20/285 (2013.01) [B01D 53/02 (2013.01); B01D 53/025 (2013.01); B01J 20/20 (2013.01); B01J 20/2808 (2013.01); B01J 20/28021 (2013.01); B01J 20/3078 (2013.01); B01J 20/3085 (2013.01); B01D 2253/102 (2013.01); B01D 2256/10 (2013.01); B01D 2257/304 (2013.01); B01D 2257/504 (2013.01); B01D 2257/7025 (2013.01)] 21 Claims
 
1. A process for the preparation of a microporous carbon material from pyrolysis of microspheres of a poly (vinylidene chloride) copolymer that have been chemically treated with alkali or alkaline earth metal hydroxides or alkoxides, comprising:
carrying out a first heating of the microspheres at a rate of 0.25° C./min to 1.75° C./min to a temperature of between 700° C. to 1200° C., and a second heating of the microspheres for 300 min to 1200 min to a temperature of between 700° C. to 1200° C.; and
carrying out a cooling of the microspheres at a rate of 0.25° C./min to 1.75° C./min;
wherein the resulting microporous carbon materials have a carbon content in the microsphere shell of 80% to 97% by mass, and wherein the microporous carbon material has oxygen in the microsphere shell.
 
11. A process of manufacturing microporous carbon material, comprising:
first and second consecutive stages;
the first stage including the step of passivation of a surface of at least one copolymer of poly(vinylidene chloride) by chemical attack in an alkaline alcohol solution that includes an alkali hydroxide dissolved in an alcohol, to cause formation of a surface-passivated copolymer having precarbonization on the surface;
the second stage including the step of pyrolysis of the surface-passivated copolymer to increase a surface area of the surface-passivated copolymer;
wherein the chemical attack is performed by reacting the at least one copolymer of poly(vinylidene chloride) with the alkali hydroxide dissolved in the alcohol.