# US 12,109,539 B2 · Membrane permeation gas separation method

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- Number: US 12,109,539 B2
- Document ID: US12109539B2
- Status: Granted
- Kind: B2
- Application number: 18/607,160
- Filed: 2024-03-15
- Published: 2024-08-22
- Granted: 2024-10-08
- Earliest claimed: 2019-01-02
- Assignees: King Fahd University of Petroleum and Minerals
- Applicants: King Fahd University of Petroleum and Minerals
- Inventors: Isam H. Aljundi; Abdelrahman M. Awad
- Web page: https://patentgrep.com/patent/US12109539B2

## CPC

- B01D 69/148: {Organic/inorganic mixed matrix membranes}
- B01D 53/228: {characterised by specific membranes}
- B01D 67/0006: {by chemical reactions (in-situ polymerisation, polycondensation, cross-linking or reaction for manufacturing composite membranes B01D69/125)}
- B01D 67/0079: {Manufacture of membranes comprising organic and inorganic components}
- B01D 67/00791: {Different components in separate layers}
- B01D 67/00793: {Dispersing a component, e.g. as particles or powder, in another component}
- B01D 69/12: Composite membranes; Ultra-thin membranes
- B01D 69/1251: {by interfacial polymerisation}
- B01D 69/14111: {with nanoscale dispersed material, e.g. nanoparticles}
- B01D 71/021: {Carbon}
- B01D 71/0211: {Graphene or derivates thereof}
- B01D 71/0212: {Carbon nanotubes}
- B01D 71/56: Polyamides, e.g. polyester-amides
- B01D 71/68: Polysulfones; Polyethersulfones
- B01D 2256/245: Methane
- B01D 2257/504: Carbon dioxide
- B01D 2323/40: in-situ membrane formation
- Y02C 20/40: of CO2
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- Y02C: CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]

## Abstract

New carbon nanomaterials, preferably titanium carbide-derived carbon (CDC) nanoparticles, were embedded into a polyamide film to give CDC/polyamide mixed matrix membranes by the interfacial polymerization reaction of an aliphatic diamine, e.g., piperazine, and an activated aromatic dicarboxylate, e.g., isophthaloyl chloride, supported on a sulfone-containing polymer, e.g., polysulfone (PSF), layer, which is preferably previously prepared by dry/wet phase inversion. The inventive membranes can separate CO2 (or other gases) from mixtures of CO2 and further gases, esp. CH4, based upon the generally selective nanocomposite layer(s) of CDC/polyamide.

## Claims

### Claim 1

A membrane permeation gas separation method, comprising:
passing a gas mixture, comprising CO2 and at least one additional gas, through a gas filter to form a permeate that is enriched in CO2 content and a gaseous composition having a concentration of CO2 that is less than a concentration of CO2 in the gas mixture,
wherein the gas filter comprises:
a plurality of multilayered membranes fixed inside a cell;
wherein each multilayered membrane of the plurality of multilayered membranes comprises:
a first layer, comprising at least 50 wt. % of polysulfone;
a second layer, comprising at least 50 wt. % of a polyamide comprising, in condensation polymerized form, piperazine and isophthaloyl chloride; and
TiC-derived nanoparticles,
wherein the TiC-derived nanoparticles are embedded in the second layer in an amount of from 0.1 to 0.5 wt. %, based on a total weight of the second layer,
wherein the first layer directly contacts the second layer.

### Claim 2 (depends on 1)

The method of claim 1, wherein the TiC-derived nanoparticles are prepared by a method comprising:
heating titanium carbide and chlorine gas at temperature in a range of from 600 to 1000° C. for a time period in a range of from 2 to 6 hours;
replacing the chlorine gas with hydrogen gas at within 100° C. of the heating in (i); and
replacing the hydrogen gas with inert gas and cooling.

### Claim 3 (depends on 1)

The method of claim 1, wherein a content of the piperazine is at least 75 wt. % relative to a total aliphatic diamine.

### Claim 4 (depends on 1)

The method of claim 1, wherein the polysulfone has a Mw of from 10,000 to 50,000.

### Claim 5 (depends on 1)

The method of claim 1, wherein the at least one additional gas is methane.