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Unit I: Membrane Manufacture Methods

This document discusses various methods for manufacturing membranes, including phase inversion, track-etching, sol-gel, interfacial polymerization, melt pressing, film stretching, and template leaching. It describes the underlying principles and processes for each technique. Phase inversion methods like solvent evaporation and thermal inversion are outlined in detail. The document also covers pore characteristics and how membrane properties depend on manufacturing methods.

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AMOL RASTOGI 19BCM0012
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111 views

Unit I: Membrane Manufacture Methods

This document discusses various methods for manufacturing membranes, including phase inversion, track-etching, sol-gel, interfacial polymerization, melt pressing, film stretching, and template leaching. It describes the underlying principles and processes for each technique. Phase inversion methods like solvent evaporation and thermal inversion are outlined in detail. The document also covers pore characteristics and how membrane properties depend on manufacturing methods.

Uploaded by

AMOL RASTOGI 19BCM0012
Copyright
© © All Rights Reserved
Available Formats
Download as PPT, PDF, TXT or read online on Scribd
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Unit I

Membrane Manufacture
Methods
Membrane Manufacture Methods
• Underlying principle – Control the pore size, Control the pore size
distribution at the surface layer and Decrease the thickness of the
surface layer.

• Commonly used membrane manufacture processes.


- Phase Inversion process
* Solvent evaporation
* Thermal Inversion
- Track –etch method
- Sol – gel peptisation method
- Interfacial polymerization
- Melt pressing
- Film stretching
- Template leaching
Phase Inversion Method
• Very flexible technique to obtain membranes with a large sort of
morphologies.

• Membrane properties greatly vary depending on the kind of polymer


system used.

• Uses the concept of ternary diagram


Phase Inversion Method
Solvent Evaporation

• Polymer is dissolved in a suitable volatile solvent (acetone, dioxane,


pyridine) and a swelling agent (magnesium perchlorate, formamide)
is added – Casting solution

• Solvent evaporates resulting in increased concentration of polymer at


the solution – air interface (since solvent is more rapidly evaporated
from the surface), resulting in the formation of skin layer of the
asymmetric membrane.

• Swelling agent in the polymer separates out as a different phase,


resulting in two phases – polymer phase as the concentrated phase
and swelling agent as the dispersed phase.

• Eg: Cellulose acetate, Cellulose triacetate and polyamide membranes


Phase Inversion Method
Thermal Inversion

• Slightly soluble polymer in the solvent.

• Casting solution is initially kept at high temperature so that a single


phase is formed (non volatile solvent).

• Next, Rapid cooling to spilt the casting solution into polymer rich
phase and solvent rich phase, resulting in gelation of the polymer.

• Further, slow cooling below the freezing point of the solvent, to get a
more homogenous ultra structure made up of micro aggregates of
polymers.

• Finally, a second solvent, known as non solvent, can be used to leach


out the primary solvent.
Phase Inversion Method
Thermal Inversion

• On completion of solvent exchange, membranes are transferred to a


desiccators where the traces of solvents are slowly evaporated.

• Eg: Polypropylene, Polyethylene and polyolefin membranes

• Usage of different solvent and Controlled cooling rate combinations


results in membranes of different average pore size and pore size
distributions.
Phase Inversion Method
Thermal Inversion
Track – etch method
• Used to prepare tortuous free, straight cylindrical pore membranes .

• Polycarbonate, Polyester membranes. Also known as nucleopore


membranes.

• First step – Track step – polyester or polycarbonate films are


bombarded with massive energetic nuclei in a collimated beam of
U235 fission fragment in a nuclear reactor.

As beams pass through the material, they leave sensitized tracks


(radiation damaged materials).

Pore density is controlled by the residence time in irradiator.


Track – etch method
• Second step – tracks left by the particles are preferentially etched
into uniform, cylindrical pores in etch bath (generally warm caustic
soda solution) .

• Pore size is controlled by residence time in etch bath.


Track – etch method
Sol – gel peptisation method
• Used for the synthesis of ceramic membranes; ease of control of
membrane characteristics by control of preparation parameters.

• Peptisation of metal oxide in a suitable medium under optimized


condition resulting in a sol.

• Control of sol viscosity by addition of optimum binder and filtration


of the sol.

• Gelation of the sol with support materials and sintering.

• Eg: Titania and Zirconia membranes with porous alumina as the


supporting material
Sol – gel peptisation method
Interfacial Polymerization
• Developed by Film Tec for preparing composite membranes.

• Support is wetted with polymer precursor and then brought in


contact with the co-reactant.

• Polymerization takes place at the interface and the formation of the


polymer prevents further reaction from taking place.

• Eg: m-phenylenediamine and trimesoyl chloride membranes.


Interfacial Polymerization
Melt Pressing
• Insoluble polymers including polyethylene, polypropylene and nylons
are made into membranes using this technique.

• Method involves sandwiching the polymer at high pressure between


two heated plates for 0.5 to 5 min at a pressure of 2000 to 5000 psi
and a temperature just above the melting point of the polymer.

• Optimum temperature is the lowest temperature that yields a


membrane of completely fused polymer of desired thickness.

• If the polymer contains air or is in pellet form, massing the material


on a rubber mill before pressing improves the results.

• To prevent the membrane sticking to plates, polymer is usually placed


between two sheets of Teflon coated foil or non waterproof cellophane.
Film Stretching
• Generally used for small openings in a dense film of crystalline or
semi crystalline polymer (PTFE or PP).

• Film is first formed by extrusion and stretching at a temperature


near the melting point of the polymer.

• The film is stretched again subsequently in a direction perpendicular


to the original stretching direction, when a very large number of slit
like voids or pores (20 to 250 nm) are formed.

• Process results in high porosity membrane, as high as 90 %.

• Microporous hollow fibre membranes are made by Film stretching


techniques.
Template Leaching
• Homogenous film is prepared from a mixture of membrane matrix
material and a leachable component is removed with a suitable
solvent and a microporous membrane is formed.

• Not widely used. Eg; Microporous glass.


Ion exchange membrane synthesis
• Prepared by grafting of polymerizable monomer to polymer film by
ray irradiation.

• Acrylic acid, trifluoroacrylate and styrene are used are common


monomers.

• Ion exchange groups are heterogeneously distributed across the cross


section of the membrane.

• Other methods of ion exchange membrane preparation includes


- Direct introduction of cation or anion group in the conventional
polymers
- forming a highly cross linked layer of anion exchange
membrane over the porous polyvinylidene fluoride membrane
- Sulfonation of polymer film
Pore Characteristics
• Membrane permeates solution based on the size and number of pores
available on its surface.

• Membranes can have open pores (communication with both external


surface) and closed pores (communication with only one or no surface).
Pore Characteristics
• Meso and Macropores – associated with pressure driven membrane
process on general lab environment.

• Dialysis and gas dehumidification membranes use ultramicropores


materials.

• Pore size distribution, surface porosity and pore shape are specific
for a given membrane because of the
- physics of forming the pores in a thin film
- formation process
- materials used for synthesis

• For eg: 10 kDa rated membranes have different water permeabilities.

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