US 12,280,340 B2Granted

Carbon molecular sieve membrane and its use in separation processes

AssigneesFundacion Tecnalia Research & Innovation, Eindhoven University of Technology

InventorsDavid Alfredo Pacheco Tanaka, Margot Anabell Llosa Tanco, Maria Luisa Vittoria Nordio, Jose Antonio Medrano Jimenez, Fausto Gallucci

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Abstract

It is provided a water-saturated carbon molecular sieve membrane obtainable by a) providing a hydrophilic carbon molecular sieve membrane (CMSM) comprising pores of a pore size from 0.25 nm to 0.55 nm for molecular sieving, pores of a pore size from 0.55 nm to 0.90 nm for adsorption diffusion and a negligible amount of pores larger than 0.90 nm such that a plot of N2 permeance versus pressure of permeation at room temperature and at a pressure from 1 to 4 bar has zero or negative slope; and b) humidifying the membrane until obtaining a water-saturated carbon molecular sieve membrane. It is also provided a process for the separation of a gas from a gas mixture with such a water-saturated membrane, and its use for solvent dehydration, and as a membrane reactor.

Claims20

Dependent claims

A water-saturated carbon molecular sieve membrane obtainable by a process comprising:

i) providing a hydrophilic carbon molecular sieve membrane (CMSM) comprising pores of a pore size as defined herein from 0.25 nm to 0.55 nm for molecular sieving, and of a pore size from higher than 0.55 nm to 0.90 nm for adsorption diffusion and a negligible amount of pores larger than 0.90 nm, such that a plot of N2 permeance as defined herein versus pressure of permeation at room temperature and at a pressure from 1 to 4 bar has zero or negative slope;
and
ii) humidifying the CMSM obtained in step i) to obtain a water-saturated CMSM by:
treating it with water vapor at a temperature from 5° C. to 180° C. and at atmospheric pressure and a relative humidity higher than 95% during a period of time such that after further treatment with water vapor, the permeation flux of a non-adsorbable gas at 4 bar at the temperature at which the CMSM has been treated with water vapor is constant during a particular period of time;
or
alternatively, by exposing the CMSM to a N2 or He gas stream saturated with water by bubbling the gas at a temperature from 5° C. to 180° C. into a tank filled with water such that after further exposure to the N2 or He gas stream saturated with water, the permeation flux of a non-adsorbable gas at 4 bar and at the mentioned temperature is constant during a particular period of time.

3 more elements

A process for the preparation of water-saturated composite alumina-carbon molecular sieve membrane (water-saturated Al-CMSM) comprising:

i) preparing a hydrophilic Al-CMSM by:
providing a porous α-Al2O3 support;
preparing a solution containing from 5 to 20 wt % of phenol formaldehyde resin, from 0.5 to 5 wt % of formaldehyde, from 0.1 to 2 wt % of ethylenediamine, from 0.1 to 5 wt % of boehmite in N-methyl-2-pyrrolidone, and heating the solution to carry out a pre-polymerization process in order to obtain a coating solution;
dip-coating the porous α-Al2O3 support in the coating solution in order to obtain a coated support;
drying the coated support at a temperature from 70 to 120° C. in order to complete the polymerization process;
and
carbonizing the dried coated support at a carbonization temperature from 450° C. to 750° C. in order to obtain the hydrophilic Al-CMSM;
and
ii) humidifying the hydrophilic Al-CMSM prepared in step i) to obtain a water-saturated Al-CMSM by:
treating the hydrophilic Al-CMSM with water vapor at a temperature from 5° C. to 180° C. and at atmospheric pressure and a relative humidity higher than 95% during a period of time such that, after further treatment with water vapor, the permeation flux of a non-adsorbable gas at 4 bar at the temperature at which the hydrophilic Al-CMSM has been treated with water vapor is constant during a particular period of time;
or
alternatively, by exposing the hydrophilic Al-CMSM to a N2 or He gas stream saturated with water by bubbling the gas at a temperature from 5° C. to 180° C. into a tank filled with water such that after further exposure to the N2 or He gas stream saturated with water, the permeation flux of a non-adsorbable gas at 4 bar and at the mentioned temperature is constant during a particular period of time.

9 more elements

Dependencies are inferred from the claim text.

Facts

Application: 17/784,580Filed 10 Dec 2020
Priority: EP 1938309511 Dec 2019
Published: US 2022/0347632 A13 Nov 2022
Granted: 22 Apr 2025
Term ends: Not estimatedThe source records don’t support an estimate.

Classification22 codes

B01D 71/0212
Carbon: carbon nanotubes
B01D 17/02
Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion: separation of non-miscible liquids
B01D 53/228
By diffusion: characterised by specific membranes
B01D 67/0067
Inorganic membrane manufacture: by carbonisation or pyrolysis