# US 12,109,538 B2 · Polysulfone-supported separation membrane

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- Number: US 12,109,538 B2
- Document ID: US12109538B2
- Status: Granted
- Kind: B2
- Application number: 18/603,314
- Filed: 2024-03-13
- Published: 2024-08-08
- Granted: 2024-10-08
- Earliest claimed: 2019-10-17
- Assignees: King Fahd University of Petroleum and Minerals
- Applicants: King Fahd University of Petroleum and Minerals
- Inventors: Isam Hassan Aljundi
- Web page: https://patentgrep.com/patent/US12109538B2

## CPC

- B01D 67/0006: {by chemical reactions (in-situ polymerisation, polycondensation, cross-linking or reaction for manufacturing composite membranes B01D69/125)}
- B01D 69/125: {In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction}
- B01D 69/12: Composite membranes; Ultra-thin membranes
- B01D 69/1251: {by interfacial polymerisation}
- B01D 71/441: {Polyvinylpyrrolidone}
- B01D 71/56: Polyamides, e.g. polyester-amides
- B01D 71/62: Polycondensates having nitrogen-containing heterocyclic rings in the main chain
- B01D 71/68: Polysulfones; Polyethersulfones
- C02F 1/265: {Desalination}
- C02F 1/44: by dialysis, osmosis or reverse osmosis {(general membrane separation processes B01D61/00, membrane modules B01D63/00, electrodialysis C02F1/4693, combination of membrane modules and bioreactors C02F3/1268)}
- B01D 2323/12: Specific ratios of components used
- B01D 2323/40: in-situ membrane formation
- B01D 2325/0283: Pore size
- C02F 1/442: {by nanofiltration}
- C02F 2103/08: Seawater, e.g. for desalination
- Y02A 20/131: Reverse-osmosis
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- C02F: TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE (separation in general B01D; special arrangements on waterborne vessels of installations for treating water, waste water or sewage, e.g. for producing fresh water, B63J; adding materials to water to prevent corrosion C23F; treating radioactively-contaminated liquids G21F9/04; regeneration of reactants for recirculation into processes, see the relevant places for the processes)
- Y02A: TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE

## Abstract

A multi-layer membrane which has a mixed polyamide selective layer supported on a porous polysulfone layer. The mixed polyamide selective layer includes reacted units of a polyfunctional acyl halide (e.g. trimesoyl chloride) and a diamine mixture containing 4,7,10-trioxa-1,13-tridecanediamine and a cyclic diamine (e.g. piperazine). Methods of fabricating the multi-layer membrane via techniques such as phase inversion and interfacial polymerization are described. The inventive membrane is evaluated on its water flux and salt rejection (e.g. sulfate and chloride salts) capabilities. A water desalination system containing the multi-layer membrane(s) is also provided.

## Claims

### Claim 1

A polysulfone-supported separation membrane, comprising:
a porous support layer comprising a polysulfone and polyvinylpyrrolidone, wherein the support layer has a thickness of 50-800 μm;
a selective layer consisting of a polyamide and having a thickness of 0.1 μm to 0.5 μm,
wherein the polyamide comprises as reacted units a polyfunctional acyl halide having at least two acyl halide groups, 4,7,10-trioxa-1,13-tridecanediamine and a cyclic diamine of formula (I)
wherein:
R1, R2, R3, and R4 are each independently selected from the group consisting of a hydrogen, an optionally substituted alkyl, an optionally substituted cycloalkyl, an optionally substituted arylalkyl, and an optionally substituted aryl;
m and n are each independently 2 or 3;
a weight ratio of the 4,7,10-trioxa-1,13-tridecanediamine to the cyclic diamine (I) in the polyamide is in a range of 1:5 to 2:1; and
the selective layer is disposed on at least a portion of a surface of the porous support layer.

### Claim 2 (depends on 1)

The polysulfone-supported separation membrane of claim 1, wherein a weight ratio of the polysulfone to polyvinylpyrrolidone is in a range of 10:1 to 50:1.

### Claim 3 (depends on 1)

The polysulfone-supported separation membrane of claim 1, wherein the polyfunctional acyl halide is a polyfunctional acyl chloride.

### Claim 4 (depends on 1)

The polysulfone-supported separation membrane of claim 1, wherein the polyfunctional acyl halide is at least one selected from the group consisting of trimesoyl chloride, 1,2,4-benzenetricarbonyl trichloride, 1,2,4,5-benzenetetracarbonyl tetrachloride, isophthaloyl chloride, terephthaloyl chloride, and [1,1′-biphenyl]-4,4′-dicarbonyl dichloride.

### Claim 5 (depends on 1)

The polysulfone-supported separation membrane of claim 1, wherein the polyfunctional acyl halide is trimesoyl chloride.

### Claim 6 (depends on 1)

The polysulfone-supported separation membrane of claim 1, wherein m and n are 2.

### Claim 7 (depends on 1)

The polysulfone-supported separation membrane of claim 1, wherein the cyclic diamine is piperazine.

### Claim 8 (depends on 1)

The polysulfone-supported separation membrane of claim 1, wherein the selective layer has pores with an average diameter in a range of 1-500 nm.

### Claim 9 (depends on 1)

The polysulfone-supported separation membrane of claim 1, which has a water flux of 53-300 Lm−2h−1, determined by exposing the polysulfone-supported separation membrane to water at a temperature of 4-60° C., and a transmembrane pressure of 5-60 bar.

### Claim 10 (depends on 1)

The polysulfone-supported separation membrane of claim 1, which has a chloride salt rejection of 30-75%, determined by exposing the polysulfone-supported separation membrane to water containing 500-5,000 ppm chloride salt at a temperature of 4-60° C., and a transmembrane pressure of 5-60 bar.

### Claim 11 (depends on 1)

The polysulfone-supported separation membrane of claim 1, which has a sulfate salt rejection of 70-99.5%, determined by exposing the polysulfone-supported separation membrane to water containing 500-5.000 ppm sulfate salt at a temperature of 4-60° C. and a transmembrane pressure of 5-60 bar.