# US 10,245,558 B2 · Green synthesis nanocomposite membranes

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- Number: US 10,245,558 B2
- Document ID: US10245558B2
- Status: Granted
- Kind: B2
- Application number: 15/183,115
- Filed: 2016-06-15
- Published: 2016-12-22
- Granted: 2019-04-02
- Earliest claimed: 2011-09-09
- Assignees: University of Kentucky Research Foundation; U.S. Environmental Protection Agency
- Applicants: The University of Kentucky Research Foundation; U.S. Environmental Protection Agency
- Inventors: Dibakar Bhattacharyya; Vasile Smuleac; Rajender S. Varma; Subhas K. Sikdar
- Web page: https://patentgrep.com/patent/US10245558B2

## CPC

- B01D 67/00793: {Dispersing a component, e.g. as particles or powder, in another component}
- B01D 67/0088: {Physical treatment with compounds, e.g. swelling, coating or impregnation}
- B01D 67/0093: {Chemical modification}
- B01D 69/106: {Membranes in the pores of a support, e.g. polymerized in the pores or voids}
- B01D 71/02231: {Palladium}
- B01D 71/02232: {Nickel}
- B01D 71/34: Polyvinylidene fluoride
- B01D 71/401: {Polymers based on the polymerisation of acrylic acid, e.g. polyacrylate}
- B01D 71/44: Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds, not provided for in a single one of groups B01D71/26-B01D71/42
- C02F 1/444: {by ultrafiltration or microfiltration}
- C02F 1/705: {Reduction by metals}
- B01D 2323/30: Cross-linking
- B01D 2323/40: in-situ membrane formation
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- C02F 1/001: {Processes for the treatment of water whereby the filtration technique is of importance (C02F1/44 takes precedence; construction of filters in general B01D24/00 - B01D41/00)}
- C02F 1/70: by reduction {(C02F1/4676 takes precedence)}
- C02F 2101/36: containing halogen
- C02F 2103/06: Contaminated groundwater or leachate
- C02F 2305/08: Nanoparticles or nanotubes
- 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)
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES

## Abstract

A nanocomposite membrane includes a macroporous polymer membrane having a plurality of pores. A plurality of metal nanoparticles are synthesized and immobilized within those plurality of pores. The nanoparticles are reduced and capped with a green reducing and capping agent such as green tea extract.

## Claims

### Claim 1

An apparatus, comprising:
a macroporous polymer membrane including a plurality of polyacrylic acid (PAA)-functionalized pores and
a plurality of green capped and reduced metal nanoparticles entrapped and immobilized in situ by functionalized polyacrylic acid of said plurality of PAA-functionalized pores, said plurality of green capped and reduced metal nanoparticles comprising catalytically active iron oxide nanoparticles.

### Claim 2 (depends on 1)

The apparatus of claim 1 wherein said plurality of green capped and reduced metal nanoparticles are reduced by contact with a green reducing and capping agent selected from a group consisting of green tea extract, polyphenol, epicatechin, epicatechin gallate, epigallocatechin, rutin, tannic acid, D-glucose, glutathione, ascorbate, kaempferol, quercetin, myricetin, maltose and mixtures thereof.

### Claim 3 (depends on 2)

The apparatus of claim 2, wherein said green reducing and capping agent is green tea extract.

### Claim 4 (depends on 1)

The apparatus of claim 1 wherein each nanoparticle of said plurality of green capped and reduced nanoparticles has a size of between about 30 nm and about 70 nm.

### Claim 5 (depends on 4)

The apparatus of claim 4, wherein between about 70 and about 80 percent of said nanoparticles immobilized on said membrane are inside said plurality of PAA-functionalized pores, as compared to the surface of the membrane.

### Claim 6 (depends on 1)

The apparatus of claim 1, wherein said plurality of PAA-functionalized pores have diameters of between about 100 nm and 700 nm.

### Claim 7 (depends on 3)

The apparatus of claim 3, wherein said green tea extract reducing and capping agent comprises polyphenols.

### Claim 8

An apparatus, comprising:
a macroporous polymer membrane including a plurality of polyacrylic acid (PAA)-functionalized pores; and
a plurality of reduced and green capped iron oxide nanoparticles entrapped and immobilized in situ by functionalized polyacrylic acid within said plurality of PAA-functionalized pores, said plurality of reduced and green capped iron oxide nanoparticles reduced and capped in situ with a green reducing and capping agent; said apparatus being made by directly synthesizing and immobilizing said plurality of reduced and green capped iron oxide nanoparticles in-situ in said plurality of PAA-functionalized pores using said green reducing and capping agent while operating in diffusion mode.

### Claim 9 (depends on 8)

The apparatus of claim 8, wherein each nanoparticle of said plurality of reduced and green capped iron oxide nanoparticles has a size of between about 30 nm and about 70 nm.

### Claim 10 (depends on 9)

The apparatus of claim 9, wherein between about 70 and about 80 percent of said plurality of reduced and green capped iron oxide nanoparticles immobilized on said membrane are inside said plurality of PAA-functionalized pores.

### Claim 11 (depends on 10)

The apparatus of claim 10, wherein said reduced and green capped iron oxide nanoparticles are made from a material selected from a group consisting of Fe/Pd, Fe/Ni, Fe/Cu, Fe/Pt, Fe/Ag and mixtures thereof.

### Claim 12 (depends on 10)

The apparatus of claim 10, wherein said membrane is made from a material selected from a group consisting of polyacrylic acid-modified polyvinylidene fluoride, polysulfone, cellulose-based materials and polycarbonate.

### Claim 13 (depends on 12)

The apparatus of claim 12, wherein said plurality of PAA-functionalized pores have diameters of between about 100 nm and 700 nm.

### Claim 14 (depends on 8)

The apparatus of claim 8, wherein said green tea derived reducing and capping agents comprise polyphenols.

### Claim 15

A method of preparing a nanocomposite membrane, comprising:
functionalizing pores of a macroporous polymer membrane with polyacrylic acid (PAA);
passing a first metal salt solution and a first reducing solution through the PAA functionalized pores by diffusion or convection, thereby synthesizing, entrapping and immobilizing a plurality of metal nanoparticles in-situ within functionalized polyacrylic acid of the PAA functionalized pores;
passing a second metal salt solution and a second reducing solution through the PAA functionalized pores by diffusion or convection to deposit a second metal on the plurality of metal nanoparticles, thereby forming a plurality of iron oxide nanoparticles; and
using a green reducing and capping agent to cap the iron oxide nanoparticles.

### Claim 16 (depends on 15)

The method of claim 15 including:
immobilizing cations of precursor salts on the membrane; and
diffusing the green reducing and capping agent through the membrane pores.

### Claim 17 (depends on 16)

The method of claim 16 including using a macroporous polymer membrane made from a material selected from a group consisting of polyvinylidene fluoride, polysulfone, cellulose-based materials and polycarbonate.

### Claim 18 (depends on 17)

The method of claim 17, wherein the iron oxide nanoparticles comprise Fe/Pd, Fe/N, Fe/Cu, Fe/Pt, Fe/Ag or mixtures thereof.

### Claim 19 (depends on 16)

The method of claim 16, including using a macroporous polymer membrane made of polyacrylic acid-modified polyvinylidene fluoride and making said plurality of iron oxide nanoparticles from Fe/Pd bimetallic material.

### Claim 20 (depends on 19)

The method of claim 19, including immobilizing at least 70% of said plurality of iron oxide nanoparticles immobilized on said membrane within said plurality of PAA-functionalized pores.