IP Library Granted Patent US 8,727,136
Granted Patent B2
US 8,727,136 · App. 12/789,593 · Granted May 20, 2014

Microfiltration membrane with improved filtration properties

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Quick Facts
Patent No.
US 8,727,136
App. No.
12/789,593
Granted
May 20, 2014
Kind
B2
Abstract

Method for producing this membrane from a casting solution comprising the hydrophobic first sulfone polymer and the hydrophilic second polymer in a solvent system, the method comprising the steps of pouring the casting solution, conditioned to a molding temperature, onto a carrier to form a film, which carrier has a temperature that is higher in comparison to the molding temperature, conveying the film through a climate-controlled zone, initiating the coagulation in a coagulation bath for the formation of a membrane structure, withdrawing the membrane structure from the carrier with a speed that is increased in comparison to the carrier speed, stabilizing, extracting, and subsequently drying the membrane.

Claims (39)

1. A method for producing an integrally asymmetric membrane for microfiltration in the form of a flat sheet, based on a film forming hydrophobic first polymer from the group of aromatic sulfone polymers, the integrally asymmetric membrane

having a membrane wall with a first porous surface and a second porous surface and an interior situated between the surfaces,

possessing a porous structure with a pore size distribution over the membrane wall, and

having a separating layer in the wall's interior with a minimum pore size, and

also having, in the direction from this separating layer towards the first porous surface, a first asymmetrical region, and towards the second porous surface, a second asymmetrical region, with pore sizes increasing towards the surfaces,

the second porous surface having pores with a mean diameter of at least 1 μm and

having a diameter of maximum separating pores of 0.1-5 μm in the separating layer,

whereby the method comprises the following steps:

a. producing a homogeneous casting solution from a polymer component and a solvent system, the polymer component consisting of 10-25 wt.%, relative to the weight of the solution, of the hydrophobic first polymer from the group of aromatic sulfone polymers and 2-20 wt. %, relative to the weight of the solution, of a hydrophilic second polymer, and the solvent system consisting of 5-80 wt. %, relative to the weight of the solvent system, of a solvent for the polymer component, 0-80 wt. %, relative to the weight of the solvent system, of a latent solvent for the polymer component, as well as 0-70 wt. %, relative to the weight of the solvent system, of a non-solvent for the polymer component,

b. conditioning the homogeneous casting solution to a molding temperature,

c. pouring the homogeneous casting solution onto a carrier to form a film, which carrier is temperature controlled and has a temperature that is at least 15° C. higher than the molding temperature of the casting solution, and which carrier has a speed v 1 ,

d. conveying the film located on the carrier through a climate-controlled zone with a temperature in the range from 35 to 55° C. and a relative humidity in the range from 40 to 75%,

e. introducing the film located on the carrier into a coagulation medium and initiating the coagulation of the film for the formation of a membrane structure,

f. withdrawing the membrane structure from the carrier within the coagulation medium by means of withdrawal device moving with a speed of v 2 , the speed v 2 being greater than the speed v 1 of the carrier, by which means the membrane structure is drawn,

g. stabilizing the membrane structure in the coagulation medium,

h. extracting the resulting membrane and subsequently drying the membrane.

2. Method according to claim 1 , characterized in that the aromatic sulfone polymer is a polysulfone or a polyethersulfone.

3. Method according to claim 2 , characterized in that the hydrophilic second polymer has an average molecular weight MW of more than 10 000 daltons.

4. Method according to claim 3 , characterized in that polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol, polyglycol monoester, polysorbitate, carboxymethylcellulose, polyacrylic acid, polyacrylate, or a modification or a copolymer of these polymers is used as the hydrophilic second polymer.

5. Method according to claim 1 , characterized in that the viscosity of the homogeneous casting solution is set to a viscosity below 10 Pa s, determined at 40° C.

6. Method according to claim 1 , characterized in that the ratio of the speed v 2 of the withdrawal device to the speed v 1 of the carrier lies in the range between 1.05:1 and 1.2:1.

7. Method according to claim 1 , characterized in that a polar, aprotic solvent or a protic solvent is used as the solvent for the polymer component.

8. A method for producing an integrally asymmetric membrane for microfiltration in the form of a flat sheet, based on a film forming hydrophobic first polymer from the group of aromatic sulfone polymers, the integrally asymmetric membrane

having a membrane wall with a first porous surface and a second porous surface and an interior situated between the surfaces,

possessing a porous structure with a pore size distribution over the membrane wall, and

having a separating layer in the wall's interior with a minimum pore size, and

also having, in the direction from this separating layer towards the first porous surface, a first asymmetrical region, and towards the second porous surface, a second asymmetrical region, with pore sizes increasing towards the surfaces,

the second porous surface having pores with a mean diameter of at least 1 μm and

having a diameter of maximum separating pores of 0.1-5 μm in the separating layer,

whereby the method comprises the following steps:

a. producing a homogeneous casting solution from a polymer component and a solvent system, the polymer component consisting of 10-25 wt. %, relative to the weight of the solution, of the hydrophobic first polymer from the group of aromatic sulfone polymers and 2-20 wt. %, relative to the weight of the solution, of a hydrophilic second polymer, and 0.220 wt. %, relative to the weight of the casting solution, of a hydrophilic third polymer, which is different from the hydrophilic second polymer, the hydropholic third polymer being a hydrophilocally modidied aromatic suffone polymer, and the solvent system consisting of 5-80 wt. %, relative to the weight of the solvent system, of a solvent for the polymer component, 0-80 wt. %, relative to the weight of the solvent system, of a latent solvent for the polymer component, as well as 0-70 wt. %, relative to the weight of the solvent system, of a non-solvent for the polymer component,

b. conditioning the homogeneous casting solution to a molding temperature,

c. pouring the homogeneous casting solution onto a carrier to form a film, which carrier is temperature controlled and has a temperature that is at least 15° C. higher than the molding temperature of the casting solution, and which carrier has a speed v 1 ,

d. conveying the film located on the carrier through a climate-controlled zone with a temperature in the range from 35 to 55° C. and a relative humidity in the range from 40 to 75%,

e. introducing the film located on the carrier into a coagulation medium and initiating the coagulation of the film for the formation of a membrane structure,

f. withdrawing the membrane structure from the carrier within the coagulation medium by means of withdrawal device moving with a speed of v 2 , the speed v 2 being greater than the speed v 1 of the carrier, by which means the membrane structure is drawn,

g. stabilizing the membrane structure in the coagulation medium,

h. extracting the resulting membrane and subsequently drying the membrane.

9. Method according to claim 8 , characterized in that the hydorphilically modified aromatic sulfone polymer is a sufoned sulfone polymer.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 1, 2024
From: 3M INNOVATIVE PROPERTIES COMPANY
To: SOLVENTUM INTELLECTUAL PROPERTIES COMPANY
Reel/Frame 066433/0105 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 3, 2015
From: MEMBRANA GMBH
To: 3M INNOVATIVE PROPERTIES COMPANY
Reel/Frame 036947/0783 →