# US 10,873,100 B2 · Nanocomposite membrane for direct methanol fuel cells

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- Number: US 10,873,100 B2
- Document ID: US10873100B2
- Status: Granted
- Kind: B2
- Application number: 16/109,347
- Filed: 2018-08-22
- Published: 2019-05-09
- Granted: 2020-12-22
- Earliest claimed: 2017-08-22
- Applicants: Ali Amoo Zadeh; Hourieh Mazdarani; Hossein Beydaghi; Elham Tabrizian; Mehran Javanbakht
- Inventors: Ali Amoo Zadeh; Hourieh Mazdarani; Hossein Beydaghi; Elham Tabrizian; Mehran Javanbakht
- Web page: https://patentgrep.com/patent/US10873100B2

## CPC

- H01M 8/1048: Ion-conducting additives, e.g. ion-conducting particles, heteropolyacids, metal phosphate or polybenzimidazole with phosphoric acid
- B01D 67/0013: {Casting processes}
- B01D 67/00793: {Dispersing a component, e.g. as particles or powder, in another component}
- B01D 69/14111: {with nanoscale dispersed material, e.g. nanoparticles}
- B01D 71/024: {Oxides}
- B01D 71/381: {Polyvinylalcohol}
- B01D 71/82: characterised by the presence of specified groups, e.g. introduced by chemical after-treatment
- H01M 8/1011: Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
- H01M 8/1081: starting from solutions, dispersions or slurries exclusively of polymers
- B01D 71/34: Polyvinylidene fluoride
- B01D 71/68: Polysulfones; Polyethersulfones
- B01D 2323/21815: Acids
- H01M 2008/1095: {Fuel cells with polymeric electrolytes}
- H01M 2300/0082: Organic polymers
- H01M 2300/0091: in the form of mixtures
- Y02E 60/50: Fuel cells
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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)
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

A method for synthesizing a nanocomposite membrane, and a synthesized nanocomposite membrane made thereby. The method may include steps of preparing Fe3O4-tolylene di-isocyanate (TDI) nanoparticles by reacting Fe3O4 nanoparticles and TDI powder, preparing Fe3O4-TDI-TiO2 nanoparticles, sulfonating the Fe3O4-TDI-TiO2 nanoparticles, preparing a first polymer solution, dispersing the Fe3O4-TDI-TiO2—SO3H nanoparticles into the first polymer solution to obtain a second homogenous solution, and casting and drying the second homogenous solution to obtain the nanocomposite membrane.

## Claims

### Claim 1

A method for synthesizing a nanocomposite membrane, the method comprising:
preparing Fe3O4-tolylene di-isocyanate (TDI) nanoparticles by reacting Fe3O4 nanoparticles and TDI powder, comprising:
obtaining a mixture by dissolving the Fe3O4 nanoparticles and the TDI powder in a first dried solvent; and
obtaining an Fe3O4-TDI powder by stirring the mixture under an inert atmosphere;
preparing Fe3O4-TDI-TiO2 nanoparticles by:
obtaining a first dispersion by dispersing the Fe3O4-TDI powder in a second dried solvent;
adding TiO2 nanoparticles to the first dispersion; and
heating the first dispersion under continuous stirring;
sulfonating the Fe3O4-TDI-TiO2 nanoparticles by:
obtaining a second dispersion by dispersing the Fe3O4-TDI-TiO2 nanoparticles in a third dried solvent;
adding chlorosulfonic acid to the second dispersion in a drop-wise manner; and
obtaining Fe3O4-TDI-TiO2-SO3H nanoparticles by removing the third dried solvent;
preparing a first polymer solution;
obtaining a second homogenous solution by dispersing the Fe3O4-TDI-TiO2-SO3H nanoparticles into the first polymer solution; and
obtaining the nanocomposite membrane by casting and drying the second homogenous solution.

### Claim 2 (depends on 1)

The method according to claim 1, wherein dissolving Fe3O4 nanoparticles and TDI powder in the first dried solvent includes dissolving Fe3O4 nanoparticles and TDI powder in the first dried solvent with an Fe3O4 to TDI mass ratio (Fe3O4:TDI) of between 6:10 and 8:10.

### Claim 3 (depends on 1)

The method according to claim 1, wherein stirring the mixture under the inert atmosphere includes stirring the mixture at a temperature of approximately 95° C. for 20 hours under a nitrogen atmosphere.

### Claim 4 (depends on 1)

The method according to claim 1, wherein dispersing the Fe3O4-TDI powder in the second dried solvent to obtain the first dispersion includes dispersing 0.0067 g to 0.01 g of the Fe3O4-TDI powder in each mL of the second dried solvent to obtain the first dispersion.

### Claim 5 (depends on 1)

The method according to claim 1, wherein adding the TiO2 nanoparticles to the first dispersion includes adding the TiO2 nanoparticles to the first dispersion with a TiO2 to Fe3O4-TDI mass ratio (TiO2:Fe3O4-TDI) of approximately 3:10.

### Claim 6 (depends on 1)

The method according to claim 1, wherein heating the first dispersion under continuous stirring comprises heating the first dispersion at a temperature of 110° C. for 48 hours under continuous stirring.

### Claim 7 (depends on 1)

The method according to claim 1, wherein dispersing the Fe3O4-TDI-TiO2 in the third dried solvent to obtain the second dispersion comprises dispersing between 0.05 g and 0.067 g of the Fe3O4-TDI-TiO2 in each mL of the third dried solvent.

### Claim 8 (depends on 1)

The method according to claim 1, wherein adding chlorosulfonic acid to the second dispersion in a drop-wise manner comprises drop-wise addition of chlorosulfonic acid to the second dispersion with an addition rate between 0.008 and 0.01 mL/min.

### Claim 9 (depends on 1)

The method according to claim 1, wherein preparing the first polymer solution includes dissolving a polymer in a fourth solvent, the polymer comprising one of polyphtalazinone (SPP), sulfonated polyphtalazinone ether ketone (SPPEK), sulfonated poly(ether sulfone) (SPES), and poly(vinyl alcohol) (PVA), sulfonated poly vinylidene fluoride (SPVDF), the fourth solvent comprising one of DMAc, N-methyl-2-pyrrolidone (NMP), and dimethyl sulfoxide (DMSO).

### Claim 10 (depends on 1)

The method according to claim 1, wherein dispersing the Fe3O4-TDI-TiO2-SO3H nanoparticles into the first polymer solution comprises dispersing the Fe3O4-TDI-TiO2-SO3H nanoparticles into the first polymer solution to obtain the second homogenous solution with a concentration of between 3 and 7 wt % based on the total weight of the second homogeneous solution.