# US 11,439,976 B2 · Advanced porous carbon adsorbents for CO2 capture and separation

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- Number: US 11,439,976 B2
- Document ID: US11439976B2
- Status: Granted
- Kind: B2
- Application number: 16/349,693
- Filed: 2017-11-17
- Published: 2020-03-05
- Granted: 2022-09-13
- Earliest claimed: 2016-11-17
- Assignees: Solvay SA
- Applicants: Solvay SA
- Inventors: Vincent Finsy; Eric Pierre Dubois
- Web page: https://patentgrep.com/patent/US11439976B2

## CPC

- B01J 20/20: comprising free carbon; comprising carbon obtained by carbonising processes
- B01D 53/02: by adsorption, e.g. preparative gas chromatography {(solid sorbent compositions B01J20/00, preparation of inorganic compounds or elements C01)}
- B01D 53/04: with stationary adsorbents {(B01D53/025 takes precedence)}
- B01J 20/28042: {Shaped bodies; Monolithic structures}
- B01J 20/28045: {Honeycomb or cellular structures; Solid foams or sponges}
- B01J 20/28057: {Surface area, e.g. B.E.T specific surface area}
- B01J 20/28069: {Pore volume, e.g. total pore volume, mesopore volume, micropore volume}
- B01J 20/28071: {being less than 0.5 ml/g}
- B01J 20/3007: {Moulding, shaping or extruding}
- B01J 20/3078: {Thermal treatment, e.g. calcining or pyrolizing}
- C01B 32/05: Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
- C01B 32/50: Carbon dioxide
- C04B 38/0032: {one of the precursor materials being a monolithic element having approximately the same dimensions as the final article, e.g. a paper sheet which after carbonisation will react with silicon to form a porous silicon carbide porous body}
- B01D 2253/102: Carbon
- B01D 2253/311: Porosity, e.g. pore volume
- B01D 2253/3425: Honeycomb shape
- B01D 2257/504: Carbon dioxide
- B01J 2220/4812: the starting material being of organic character
- Y02C 20/40: of CO2
- Y02P 20/151: Reduction of greenhouse gas [GHG] emissions, e.g. CO2
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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)
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- Y02C: CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

The present invention concerns a process for manufacturing a porous carbonaceous monolith structure comprising the steps of (i) introducing a precursor material comprising particles comprising a halogenated polymer having a melting point in a mold; (ii) forming a shaped body comprising aggregates of the particles of the precursor material, by concurrently applying to the precursor material a pressure P ranging from 10 to 300 bars when the halogenated polymer is a vinylidene chloride homopolymer and from 10 to 150 bars when the halogenated polymer differs from a vinylidene chloride homopolymer, and maintaining the precursor material at a temperature T1 ranging from T1,min=20° C. to T1,max=Tm−50° C. wherein Tm is the melting point of the halogenated polymer, and; (iii) optionally cooling then demolding the shaped body; (iv) introducing the shaped body in a furnace; (v) causing the pyrolysis of the halogenated polymer in the furnace until the porous carbonaceous monolith structure is obtained.

## Claims

### Claim 1

A method of manufacturing a grooved carbonaceous monolith, said method comprising sculpting a carbonaceous monolith structure obtained by a process for manufacturing a porous carbonaceous monolith structure comprising the steps of:
i— introducing a precursor material comprising particles comprising a halogenated polymer having a melting point in a mold,
ii— forming a shaped body comprising aggregates of the particles of the precursor material, by concurrently applying to the precursor material a pressure P ranging from 10 to 300 bars when the halogenated polymer is a vinylidene chloride homopolymer and from 10 to 150 bars when the halogenated polymer differs from a vinylidene chloride homopolymer, and maintaining the precursor material at a temperature T1 ranging from T1,min=20° C. to T1,max=Tm−50° C. wherein Tm is the melting point of the halogenated polymer, and,
iii— optionally cooling then demolding the shaped body,
iv— introducing the shaped body in a furnace,
v— causing the pyrolysis of the halogenated polymer in the furnace until the porous carbonaceous monolith structure is obtained,
wherein the carbonaceous monolith structure has a length to width and/or a length to thickness ratio of at least 4, and in that it presents a microporosity and at least one of an intra-particle macroporosity and an inter-particles macroporosity.

### Claim 2 (depends on 1)

The method according to claim 1, wherein the pressure P ranges from 10 to 150 bars whatever the halogenated polymer.

### Claim 3 (depends on 1)

The method according to claim 1 wherein step v comprises:
va— bringing the temperature of the shaped body up to a temperature T2 strictly above T2,min=Tm−50° C. and strictly below T2,max=Tm,
vb— maintaining the shaped body, at the temperature T2 under inert gas flow, to cause the pyrolysis of the halogenated polymer and the formation of an infusible char,
vc— bringing the temperature of the infusible char up to a temperature T3 strictly above T3,min=Tm and strictly below T3,max=900° C.,
vd— maintaining the infusible char, at the temperature T3 under inert gas flow, to cause the pyrolysis of the halogenated polymer, thereby obtaining the porous carbonaceous monolith structure.

### Claim 4 (depends on 1)

The method according to claim 1 wherein the particles comprising the halogenated polymer have a mean diameter ranging from 145 μm to 400 μm.

### Claim 5

A method of manufacturing a grooved carbonaceous monolith, said method comprising:
manufacturing a porous carbonaceous monolith structure by a process for manufacturing a porous carbonaceous monolith structure comprising the steps of:
i— introducing a precursor material comprising particles comprising a halogenated polymer having a melting point in a mold,
ii— forming a shaped body comprising aggregates of the particles of the precursor material, by concurrently applying to the precursor material a pressure P ranging from 10 to 300 bars when the halogenated polymer is a vinylidene chloride homopolymer and from 10 to 150 bars when the halogenated polymer differs from a vinylidene chloride homopolymer, and maintaining the precursor material at a temperature T1 ranging from T1,min=20° C. to T1,max=Tm−50° C. wherein Tm is the melting point of the halogenated polymer, and,
iii— optionally cooling then demolding the shaped body,
iv— introducing the shaped body in a furnace,
v— causing the pyrolysis of the halogenated polymer in the furnace until the porous carbonaceous monolith structure is obtained, and
sculpting the so-manufactured porous carbonaceous monolith structure.

### Claim 6 (depends on 1)

A grooved carbonaceous monolith obtained by the method of claim 1, wherein the grooved carbonaceous monolith presents a microporosity and at least one of an intra-particle macroporosity and an inter-particles macroporosity and has canals wherein a gas can circulate.

### Claim 7 (depends on 1)

A method of manufacturing a honeycomb porous carbonaceous structure presenting a microporosity and at least one of an intra-particle macroporosity and an inter-particles macroporosity, said method comprising:
manufacturing grooved carbonaceous monoliths by the method of claim 1, and
assembling the so-manufactured grooved carbonaceous monoliths.

### Claim 8 (depends on 7)

The method according to claim 7 wherein assembling the so-manufactured grooved carbonaceous monoliths is achieved by sticking with glue or by wrapping up with a polymer film.

### Claim 9 (depends on 7)

A honeycomb porous carbonaceous structure obtained by the method of claim 7, wherein the honeycomb porous carbonaceous structure presents a microporosity and at least one of an intra-particle macroporosity and an inter-particles macroporosity and has canals wherein a gas can circulate.

### Claim 10 (depends on 6)

A method for extracting CO2 from a gas composition by selectively adsorbing CO2 gas using the grooved monolith according to claim 6.

### Claim 11 (depends on 9)

A method for extracting CO2 from a gas composition by selectively adsorbing CO2 gas using the honeycomb structure according to claim 9.

### Claim 12 (depends on 1)

The method according to claim 1, wherein the pressure P ranges from 10 to 50 bars.