WO2024144450A1 - Procédé pour membrane polymère renforcée par un substrat hydrophile induite par du titane in situ et dispositifs associés - Google Patents

Procédé pour membrane polymère renforcée par un substrat hydrophile induite par du titane in situ et dispositifs associés Download PDF

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Publication number
WO2024144450A1
WO2024144450A1 PCT/SG2022/050945 SG2022050945W WO2024144450A1 WO 2024144450 A1 WO2024144450 A1 WO 2024144450A1 SG 2022050945 W SG2022050945 W SG 2022050945W WO 2024144450 A1 WO2024144450 A1 WO 2024144450A1
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WO
WIPO (PCT)
Prior art keywords
substrate
membrane
nozzle module
membrane solution
titanium
Prior art date
Application number
PCT/SG2022/050945
Other languages
English (en)
Inventor
Lilin Zhang
Darren SUN
Zhengtao LI
Wee TIO
Original Assignee
Nanosun Pte. Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanosun Pte. Ltd. filed Critical Nanosun Pte. Ltd.
Priority to PCT/SG2022/050945 priority Critical patent/WO2024144450A1/fr
Publication of WO2024144450A1 publication Critical patent/WO2024144450A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/10—Supported membranes; Membrane supports
    • B01D69/105—Support pretreatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002—Organic membrane manufacture
    • B01D67/0006—Organic membrane manufacture by chemical reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/10—Supported membranes; Membrane supports
    • B01D69/107—Organic support material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12—Composite membranes; Ultra-thin membranes
    • B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B01D71/022—Metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/08—Specific temperatures applied
    • B01D2323/081—Heating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/34—Use of radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/42—Details of membrane preparation apparatus

Definitions

  • the present disclosure relates to a method for fabricating a hydrophilic composite membrane.
  • the present disclosure also relates to a system operable to carry out aforesaid method for fabricating a hydrophilic composite membrane.
  • Filtration techniques are traditionally adopted for use in water and/or wastewater treatments so as to exclude pollutants to obtain cleaned water. Filtration techniques are also traditionally adopted for use in concentration of a filtrate, such as to obtain fruit juice, wine, pharmaceutics, etc.
  • a flat sheet membrane tends to employ a stiff resin backbone as a support plate, wherein both sides of the stiff resin backbone support plate tend to be traditionally mounted with guiding layer.
  • the guiding layer serves as one or more thin flow path channels.
  • the stiff resin backbone may be topped with a filtrate membrane having all sides sealed.
  • a flat sheet membrane in a flat membrane module was developed with a rigid spacer to separate and hold each individual membrane such that during scouring every piece of flat sheet membrane may be thoroughly scoured and cleaned by the air that may be evenly distributed. This helps to eliminate and/or reduce fouling tendency of the flat sheet membranes.
  • a flat sheet may tend to be suitable for use in applications that require high strength.
  • Non-limiting examples of such applications may include wastewater filtration, wherein the wastewater may have a high suspended solid concentration, applications involving use of a membrane bioreactor, filtration of landfill leachate, etc.
  • the resin support plate of a flat sheet membrane e.g. may range from about 5 mm to about 10 mm in thickness
  • the packing density of membrane may be relatively poor
  • the cost of the resin based support plate also tends to be higher than the actual filtration membrane. Therefore, these shortcomings of having a large space required by the resin support plate (and hence the poor packing density) and its cost tend to significantly limit flat sheet membrane’s market economic viability.
  • traditional tubular membranes and traditional hollow fibre membranes may help address the packing density issue mentioned above encountered for flat sheet membranes. It may be distinguished that a traditional hollow fibre membrane may have a smaller diameter (for example, from about 1 mm to 2 mm) as compared to a tubular membrane that may have a larger diameter of about 10 mm or above. As such, the outer surface area renders a much larger specific surface area per footprint.
  • the hollow fibre membranes may be assembled into a bundle, after which multiple bundles may be arranged to form hollow fibre membrane curtains. Such curtains may then be further arranged into a cartridge form, which may be immersed directly in waterbodies that are to be filtered.
  • the solution should at least provide for a method and/or system which resolves one or more of aforesaid limitations for producing a hollow fibre membrane.
  • the solution should provide for membranes with good hydrophilicity, good packing density, good mechanical strength, and/or low peeling tendency (between membrane and its substrate).
  • the solution should, for example, provide for a composite hydrophilic hollow fibre membrane reinforced with a substrate that helps in overcoming fouling, poor packing density and mechanical strength limitations.
  • a system operable to carry out the method described in various embodiments of the first aspect, the system comprises: a spool which a substrate is wrapped; an ionization reactor operable to treat a substrate; a nozzle module configures to dope the substrate with a dope liquid; a moisture control ring module operable to dry the substrate; a membrane solution coating nozzle module configured to coat or dispense a membrane solution on the substrate; and a water bath for forming a membrane on the substrate from the membrane solution.
  • the substrate e.g. in the form of a hollow fibre
  • the substrate can be inserted into a pole configured to fit into the lumen of a substrate.
  • the ionization reactor can contain one or more of such poles to accommodate multiple substrates.
  • At one end of the ionization reactor distal end away from where the substrate is fed, there can be an end plate having supporting structures thereon which the substrate may be supported on.
  • the supporting structures may be connected to the one or more poles, such that when the end plate is removed, the one or more substrates may be retrieved (i.e.
  • the ionization reactor can be configured to treat a flat sheet substrate (e.g. by rolling the flat sheet substrate into a tubular configuration or by removing the one or more poles so as to fit the flat sheet substrate into the ionization reactor).
  • FIG. 3 shows a cross-sectional view of the nozzle module shown in FIG. 2. From the cross-sectional view, it can be seen that the nozzle module has sharp structures protruding away and inwards within the nozzle module.
  • the sharp structures may be interchangeably referred to herein as “rifling structures” and “guide structures”.
  • the rifling structures may define the walls of the dope liquid chamber (denoted as “dope feeding chamber” in FIG. 3) contained in the nozzle module.
  • the rifling structures help confine the dope liquid to the dope liquid chamber by capillary action and also by surface tension of the dope liquid against the rifling structures.
  • the one or more hollow fibre substrates are lined conformably (i.e.
  • the rifling structure may have a height of about 0.4 mm as shown in FIG. 3.
  • FIG. 4 shows a moisture control ring module.
  • the one or more substrates are conveyed through the moisture control ring module.
  • the moisture control ring module channels hot air to the one or more substrates passing through for moisture control. This helps to remove any excess liquid on the one or more substrates from the nozzle module. Also, the hot air’s moisture content can be adjusted to evaporate or air-brushed off any excessive liquid on the one or more substrates. This helps to control and/or maintain the desired moisture level for phase inversion of the membrane that is to be formed on the one or more substrates. The control and/or maintain of the moisture level in the one or more substrates may in turn help control the rate of the phase inversion of the membrane that is subsequently formed thereon.
  • the moisture control ring module may contain a heating coil (not shown) or coupled to a heating coil (not shown) to heat up air that is delivered via a gap that is positioned peripheral to the one or more substrates passing through.
  • the temperature of the heating coil may be controlled by a heating coil current supply (not shown).
  • moisture may be introduced at a controlled amount to control the evaporation rate and final wetted moisture content, for example, by adjusting the temperature of the hot air from the moisture control ring module.
  • FIG. 5 shows a cross-sectional view of the membrane solution coating nozzle module.
  • the membrane solution coating nozzle has the same configuration as the nozzle module shown in FIG. 3.
  • the membrane solution coating nozzle module has sharp structures protruding away and inwards within the membrane solution coating nozzle module.
  • the sharp structures may be interchangeably referred to herein as “rifling structures” and “guide structures”.
  • the rifling structures may define the walls of the membrane solution feeding chamber contained in the membrane solution coating nozzle module. The rifling structures help confine the membrane solution to the membrane solution feeding chamber by capillary action and by surface tension of the membrane solution against the rifling structures.
  • the one or more hollow fibre substrates are lined conformably (i.e. fit tightly) around the membrane solution feed chamber to be exposed to the membrane solution for the membrane solution to be coated thereon as the one or more substrates are guided (i.e. conveyed) through the membrane solution coating nozzle module.
  • the rifling structure may have a height of about 0.4 mm as shown in FIG. 5.
  • FIG. 6 shows the heterogeneous pore structures across the substrate due to different phase separation speed with the influence of the dope liquid content.
  • the membrane is formed under rapid phase separation in a water bath.
  • smaller pores are due to the present of water in the dope liquid.
  • Large finger-like tunneling structure are formed across the substrate.
  • FIG. 7 is a schematic of the system 100 of the present disclosure for fabricating a hollow fibre composite membrane.
  • the system 100 includes a spool 102 wrapped with one or more hollow fibre substrates.
  • This spool 102 may be referred to herein as a “substrate feed spool” as it feeds the substrate into downstream modules of the system 100.
  • the substrate may be connected to a roller 104 (this roller may be interchangeably referred to herein as a “speed counter roller” and “counter wheel”, as the speed of the roller 104 is used to regulate the feeding of the substrate into various modules of the system 100 and to maintain a tension in the substrate as the substrate conveys through various modules of the system 100).
  • Treating the surface of each of the one or more substrates can involve oxidizing (clean) any debris on the surface of each of the one or more substrates. Treating the surface of each of the one or more substrates can involve polarizing the surface of each of the one or more substrate(s) so as to improve adhesiveness of a substrate with a membrane. Treating the surface of each of the one or more substrates can involve introduction of a functional material or chemical or one or more functional groups to the surface of each of the one or more substrates so as to improve adhesiveness of a substrate with a membrane.
  • This spool 202 may be referred to herein as a “substrate feed spool” as it feeds the substrate into downstream modules of the system 200.
  • the substrate may be connected to a roller 208 (this roller may be interchangeably referred to herein as a “speed counter roller” and “counter wheel”, as the speed of the roller 208 is used to regulate the feeding of the substrate into various modules of the system 200 and to maintain a tension in the substrate as the substrate conveys through various modules of the system 200). From the number of revolutions of the roller 208, the linear feeding speed of the substrate can be regulated.
  • Treating the surface of each of the one or more substrates can involve oxidizing (clean) any debris on the surface of each of the one or more substrates. Treating the surface of each of the one or more substrates can involve polarizing the surface of each of the one or more substrate(s) so as to improve adhesiveness of a substrate with a membrane. Treating the surface of each of the one or more substrates can involve introduction of a functional material or chemical or one or more functional groups to the surface of each of the one or more substrates so as to improve adhesiveness of a substrate with a membrane.
  • the present method and system may involve non-solvent induced phase separation (NPIS) for forming the membrane of the composite membrane.
  • NPIS non-solvent induced phase separation
  • the solvent may comprise dimethyl sulfoxide, dimethylacetamide, dimethylformamide, N-methyl-2-pyrrolidone, or a mixture thereof.
  • the acetic acid glacier may have a purity of 99.99% or more.
  • drying the substrate may comprise conveying the substrate through a moisture control ring module which channels air to remove excess liquid from the substrate.
  • drying the substrate may comprise conveying the substrate to a moisture control ring module which channels air to remove excess liquid from the substrate.
  • forming the membrane on the substrate may comprise conveying the substrate to a casting platform from the ionization reactor and have the substrate conveyed under a membrane solution coating nozzle module which dispenses a membrane solution on the substrate.
  • the membrane solution may comprise a polymer.
  • the polymer may comprise polyvinylidene fluoride, polyether sulfone, polyacrylonitrile, polyamide, or cellulose acetate.
  • the ionization reactor may be configured upstream of the spool but downstream of the roller. In certain non-limiting embodiments, the ionization reactor may be configured downstream of the spool.
  • the nozzle module may be configured to have the one or more substrates arranged conformably and peripheral to the dope feeding chamber for the dope liquid to be coated on the substrate. [0060] In certain non-limiting embodiments, the nozzle module may be configured to dispense the dope liquid on a substrate which may be conveyed under the nozzle module.
  • the moisture control ring module may be configured to have the substrate conveyed through the moisture control ring module which channels air to remove excess liquid from the substrate.
  • the membrane solution coating nozzle module may comprise more than one rifling structures that protrude away and inward within the nozzle module to define one or more membrane solution feed chamber.
  • the present disclosure relates to a method for fabricating a titanium induced substrate reinforced polymer membrane.
  • the present disclosure also relates to a system operable to carry out aforesaid method.
  • the method and system of the present disclosure are advantageous for the fabrication of a mesoporous composite polymer membrane having a substrate which reinforces a polymer membrane of the mesoporous composite polymer membrane.
  • the method can utilize the hydrophilicity from crystalline titanium and can involve in situ titanium crystal seeding, its growth and curing.
  • Example 1 A non-limiting general discussion of the present method, system and the components in the system
  • FIG. 7 illustrates for the system operable to fabricate a hollow fibre composite membrane
  • FIG. 8 illustrates for the system operable to fabricate a flat sheet membrane.
  • the substrate may be fabricated or purchased. Such a substrate may be referred to as a “raw substrate”.
  • the raw substrate may be in the form of a hollow fibre or a flat sheet.
  • the hollow fibre raw substrates may be braided and bundled.
  • the braided and bundled hollow fibre raw substrates may be loaded onto a non-solvent induced phase separation coating module.
  • the surface of each substrate may be braided.
  • the substrate can be made from, for example, polyethylene terephthalate (PET), polyethylene (PE), polyamide (PA, also called “nylon”), polypropylene (PP), a fluorinated derivative thereof, and/or a combination thereof.
  • PET polyethylene terephthalate
  • PE polyethylene
  • PA polyamide
  • PP polypropylene
  • fluorinated derivative thereof and/or a combination thereof.
  • Other suitable polymers can be used.
  • the nozzle tip material can be any flexible material, such as but not limited to, silicon, latex rubber, etc. Other suitable soft flexible material can be used.
  • the one or more substrates from the nozzle module are conveyed through the moisture control ring module.
  • the moisture control ring module channels hot air to the one or more substrates passing through for moisture control. This helps to remove any excess liquid on the one or more substrates from the nozzle module.
  • the hot air’s moisture content can be adjusted to evaporate or air-brushed off any excessive liquid on the one or more substrates. This helps to control and/or maintain the desired moisture level for phase inversion of the membrane that is to be formed on the one or more substrates.
  • the control and/or maintain of the moisture level in the one or more substrates may in turn help control the rate of the phase inversion of the membrane that is subsequently formed thereon.
  • moisture may be introduced at a controlled amount to control the evaporation rate and final wetted moisture content of the one or more substrates, for example, by adjusting the temperature of the hot air from the moisture control ring module.
  • the controlled moisture may help in delaying the crystallisation rate of titanium nanocrystals incorporated via the dope liquid, wherein the titanium nanocrystals may be rooted across the thickness of the membrane and the one or more substrates.
  • a warmer substrate may also favour diffusion process as well as mass transfer.
  • the membrane solution can comprise dimethyl sulfoxide (DMSO), dimethylacetamide (DMAc), dimethylformamide (DMF), N-methyl-2-pyrrolidone (NMP), or a combination thereof.
  • DMSO dimethyl sulfoxide
  • DMAc dimethylacetamide
  • DMF dimethylformamide
  • NMP N-methyl-2-pyrrolidone
  • Each of these may be a solvent for the polymer (i.e. membrane polymer) used to form the membrane.
  • FIG. 7 shows a schematic illustrating a single braided substrate feeding, it is applicable to multiple substrate feeders of up to, for example, 8 units.
  • PVDF substrate supported titanium-polyvinylidene fluoride
  • the dope liquid is prepared with the following composition: dimethylacetamide (DMAc) 70%, water 20%, acetic acid glacier 3%, titanium isopropoxide (TTIP) 2%, polyethylene glycol (PEG) 5% (w/w %).
  • DMAc dimethylacetamide
  • TTIP titanium isopropoxide
  • PEG polyethylene glycol
  • Plasma is then initialised to ionise the mixed gas on the substrate surface.
  • the surfaced treated substrate then conveys onwards to the nozzle module where the dope liquid is coated onto the substrate and diffuse across the substrate wall.
  • the wetted substrate then conveys through the moisture control ring module at 60°C with moisture limited at about 21%.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

Est divulgué dans la présente invention un procédé de fabrication d'une membrane composite hydrophile, le procédé comprenant les étapes suivantes : fourniture d'un substrat ; traitement du substrat dans un réacteur d'ionisation ; dopage du substrat avec un liquide de dopage pour incorporer des nanocristaux de titane ; séchage du substrat ; et formation d'une membrane sur le substrat. La présente invention concerne également un système utilisable pour mettre en œuvre le procédé, le système comprenant : une bobine sur laquelle un substrat est enveloppé ; un réacteur d'ionisation utilisable pour traiter un substrat ; un module de buse conçu pour doper le substrat avec un liquide de dopage ; un module en anneau de contrôle de l'humidité utilisable pour sécher le substrat ; un module de buse de revêtement de solution de membrane conçu pour revêtir ou distribuer une solution de membrane sur le substrat ; et un bain d'eau pour former une membrane sur le substrat à partir de la solution de membrane.
PCT/SG2022/050945 2022-12-29 2022-12-29 Procédé pour membrane polymère renforcée par un substrat hydrophile induite par du titane in situ et dispositifs associés WO2024144450A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/SG2022/050945 WO2024144450A1 (fr) 2022-12-29 2022-12-29 Procédé pour membrane polymère renforcée par un substrat hydrophile induite par du titane in situ et dispositifs associés

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/SG2022/050945 WO2024144450A1 (fr) 2022-12-29 2022-12-29 Procédé pour membrane polymère renforcée par un substrat hydrophile induite par du titane in situ et dispositifs associés

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160263530A1 (en) * 2013-11-28 2016-09-15 B.G. Negev Technologies And Applications Ltd Fabrication and modification of polymer membranes using ink-jet printing
US20220032240A1 (en) * 2020-07-29 2022-02-03 Aspen Products Group, Inc. Separation Membrane and Methods of Preparation Thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160263530A1 (en) * 2013-11-28 2016-09-15 B.G. Negev Technologies And Applications Ltd Fabrication and modification of polymer membranes using ink-jet printing
US20220032240A1 (en) * 2020-07-29 2022-02-03 Aspen Products Group, Inc. Separation Membrane and Methods of Preparation Thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
LI XIN, FANG XIAOFENG, PANG RUIZHI, LI JIANSHENG, SUN XIUYUN, SHEN JINYOU, HAN WEIQING, WANG LIANJUN: "Self-assembly of TiO2 nanoparticles around the pores of PES ultrafiltration membrane for mitigating organic fouling", JOURNAL OF MEMBRANE SCIENCE, ELSEVIER BV, NL, vol. 467, 1 October 2014 (2014-10-01), NL , pages 226 - 235, XP093194894, ISSN: 0376-7388, DOI: 10.1016/j.memsci.2014.05.036 *
ROSSOUW ARNOUX, OLEJNICZAK ANDRZEJ, OLEJNICZAK KATARZYNA, GORBERG BORIS, VINOGRADOV ILIYA, KRISTAVCHUK OLGA, NECHAEV ALEXANDER, PE: "Ti and TiO2 magnetron sputtering in roll-to-roll fabrication of hybrid membranes", SURFACES AND INTERFACES, vol. 31, 1 July 2022 (2022-07-01), pages 101975, XP093195316, ISSN: 2468-0230, DOI: 10.1016/j.surfin.2022.101975 *

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