Method and arrangement for determining at least one pore-related parameter of a porous structure

Patent metadata

Field	Value
Publication number	US-10996158-B2
Application number	US-201716311037-A
Country	US
Kind code	B2
Filing date	Jun 21, 2017
Priority date	Jun 22, 2016
Publication date	May 4, 2021
Grant date	May 4, 2021

Abstract

In the present invention, a method for determining at least one pore-related parameter of a porous structure is provided. In a preferred embodiment, an enhanced evapoporometry (EP) technique is provided to determine pore size distribution of continuous pores of a porous structure. In this enhanced EP technique, a volatile liquid, such as isopropoyl alcohol or water, is supplied to one side of a porous structure in order to enable the volatile liquid to penetrate and saturate the porous structure through capillary force. Thereafter, an immiscible non-volatile liquid, such as glycerol, mineral oils, silicon oils or hydrophilic ionic liquid, is supplied to the one side of the porous structure. As the volatile liquid evaporates progressively from the filled pores, the emptied pores may be immediately filled by the non-volatile liquid drawn upwards by capillary action. This prevents formation of a t-layer formed from the adsorption of vapour emanating from the volatile liquid that is used to saturate the pores.

First claim

The invention claimed is:

1. A method for determining at least one pore-related parameter of a porous structure, the method comprising:
arranging the porous structure in a test cell so that a first space is at least partially defined by a first surface of the porous structure and a second space is at least partially defined by a second surface of the porous structure opposite the first surface;
supplying a volatile liquid to the first space so that one or more continuous pores of the porous structure are filled with the volatile liquid;
supplying a non-volatile liquid to the first space so that the non-volatile liquid fills the one or more continuous pores of the porous structure after the volatile liquid evaporates from the one or more continuous pores of the porous structure;
determining an effective mass of the test cell over a period of time due to evaporation of the volatile liquid from the one or more continuous pores; and
determining the at least one pore-related parameter of the porous structure based on the effective mass determined.

2. The method according to claim 1 ,
wherein the porous structure is a flat sheet membrane.

3. The method according to claim 2 ,
wherein the test cell comprises a base including a cavity, and a chamber;
wherein arranging the flat sheet membrane in the test cell comprises:
arranging the flat sheet membrane over the cavity so that the first space comprises the cavity; and
securing the flat sheet membrane to the base.

4. The method according to claim 3 ,
wherein the base comprises an inlet channel configured to direct the volatile liquid and the non-volatile liquid to the cavity.

5. The method according to claim 1 ,
wherein the porous structure is a hollow fiber;
wherein the first surface is an inner surface of the hollow fiber; and
wherein the second surface is an outer surface of the hollow fiber.

6. The method according to claim 5 ,
wherein arranging the hollow fiber in the test cell comprises:
sealing a first end of the hollow fiber using a seal comprising a suitable sealant material or a suitable potting material;
attaching a second end of the hollow fiber to a fluid delivery device.

7. The method according to claim 6 ,
wherein the fluid delivery device is configured to direct the volatile liquid and the non-volatile liquid to the first space is at least partially defined by the inner surface of the hollow fiber and the seal.

8. The method according to claim 1 ,
wherein supplying the volatile liquid into the first space comprises supplying the volatile liquid so that the volatile liquid comes into contact with the first surface of the porous structure.

9. The method according to claim 1 , further comprising:
forming a hole on the porous structure before supplying the volatile liquid and the non-volatile liquid;
wherein a diameter of the hole is greater than a diameter of each of the one or more continuous pores.

10. The method according to claim 1 ,
wherein the volatile liquid supplied is equal to an amount required to saturate the one or more continuous pores, and one or more dead-end pores on the first surface of the porous structure.

11. The method according to claim 1 , further comprising
controlling evaporation of the volatile liquid in the test cell.

12. The method according to claim 11 ,
wherein controlling evaporation of the volatile liquid in the test cell comprises arranging a diffusional resistance element spaced over the porous structure; and
wherein the diffusional resistance element is configured to resist diffusion of vapour of the volatile liquid.

13. The method according to claim 1 , further comprising:
determining an evaporation rate from the effective mass determined; and
relating the evaporation rate to a vapour pressure of the volatile liquid at an interface between the volatile liquid in the porous structure and an ambient gas phase within the test cell;
wherein determining the at least one pore-related parameter of the porous structure comprises determining the at least one pore-related parameter based on the vapour pressure determined.

14. The method according to claim 1 , further comprising:
determining an evaporation rate from the effective mass determined; and
relating the evaporation rate to a mole fraction of the volatile liquid at an interface between the volatile liquid in the porous structure and an ambient gas phase within the test cell;
wherein determining the at least one pore-related parameter of the porous structure comprises determining the at least one pore-related parameter based on the mole fraction determined.

15. The method according to claim 1 ,
wherein determining an effective mass of the test cell comprises determining the effective mass of the test cell at a series of time intervals to generate a plurality of instantaneous masses.

16. The method according to claim 15 ,
wherein the at least one pore-related parameter comprises a pore-size distribution; and
wherein determining the pore-size distribution of the porous structure comprises:
associating a respective instantaneous mass of the generated plurality of instantaneous masses to a respective pore diameter of the porous structure; and
determining the pore-size distribution based on the plurality of instantaneous masses generated and the associated pore diameters.

17. The method according to claim 1 ,
wherein the at least one pore-related parameter comprises a mass-average pore diameter or a bulk porosity.

18. The method according to claim 1 ,
wherein the at least one pore-related parameter of the porous structure is a parameter of the one or more continuous pores of the porous structure.

19. The method according to claim 1 ,
wherein the non-volatile liquid is supplied to the first space after the volatile liquid is supplied.

20. An arrangement for determining at least one pore-related parameter of a porous structure, the arrangement comprising:
a test cell comprising the porous structure so that the test cell comprises a first space at least partially defined by a first surface of the porous structure and a second space at least partially defined by a second surface of the porous structure opposite the first surface;
a fluid delivery device configured to supply a volatile liquid into the first space so that one or more continuous pores of the porous structure are filled with the volatile liquid, and further configured to supply a non-volatile liquid into the first space so that the non-volatile liquid fills the one or more continuous pores of the porous structure after the volatile liquid evaporates from the one or more continuous pores of the porous structure; and
a mass-determination device configured to determine an effective mass of the test cell over a period of time due to evaporation of the volatile liquid from the one or more continuous pores;
wherein the at least one pore-related parameter of the porous structure is determined based on the effective mass determined.

Assignees

• Univ Nanyang Tech

Inventors

• Krantz William Bernard
• Chew Jia Wei
• Zamani Farhad

Classifications

• B01D69/06

  Flat membranes · CPC title

• B01D65/109

  Testing of membrane fouling or clogging, e.g. amount or affinity · CPC title

• B01D69/08

  Hollow fibre membranes (manufacture of hollow fibres D01D5/24, D01F1/08) · CPC title

• G01N15/0893 Primary

  by measuring weight or volume of sorbed fluid, e.g. B.E.T. method · CPC title

• G01N15/0806

  Details, e.g. sample holders, mounting samples for testing · CPC title