IP Library Granted Patent US 12,447,441
Granted Patent B2
US 12,447,441 · App. 17/994,686 · Granted Oct 21, 2025

Process for obtaining polyamide membrane with nanostructured coating, membranes and use

Inventors: Rodrigo Suhett De Souza (Ilha do Fundão, BR); Ricardo De Araujo Cid Da Silva (Ilha do Fundão, BR); Yara Luiza Brasil Zanon (Pampulha, BR); Vinícius Gomide De Castro (Pampulha, BR); Miriam Cristina Santos Amaral Moravia (Pampulha, BR); Glaura Goulart Silva (Pampulha, BR); Bruna Caroline De Jesus Ribeiro (Pampulha, BR); Ana Luiza Silvestre Assis (Pampulha, BR)
Assignees: Petróleo Brasileiro S.A.—Petrobras; Universidade Federal De Minas Gerais—UFMG
B01D61/026B01D67/0002B01D67/00931B01D71/56B82Y30/00B82Y40/00C02F1/265B01D2323/21819C02F2103/08
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Quick Facts
Patent No.
US 12,447,441
App. No.
17/994,686
Granted
Oct 21, 2025
Kind
B2
Abstract

The present invention refers to a surface coating of commercial polyamide (PA) membranes with graphene oxide (GO) using a technology that involves spin-coating with specific sequence of low and high rotation, interface phenomena provided by a set of materials containing ethyl alcohol in high concentration, as well as morphological characteristics and customized surface chemistry of GO, among other conditions that allow a differentiated technology to obtain an effective coating of GO on PA membrane.

Claims (9)

1. A process for obtaining polyamide membrane with nanostructured coating, the process comprising the following steps:

(a) prepare dispersion of graphene oxide (GO) in absolute ethyl alcohol (99.5%) between 0.1 g/L and 2 g/L;

(b) apply the dispersion obtained in step (a) on reverse osmosis membranes made of a selective polyamide (PA) layer, using spin coating technique, with low rotation stage followed by high rotation;

(c) repeat step (b) between 1 and 5 times; and

(d) immerse the membranes in water immediately after step (c).

2. The process according to claim 1 , wherein in the step (a) the GO presents a degree of oxidation greater than 35% by mass, layer distribution of up to 10 nanosheets and an average lateral dimension greater than 1 micrometer.

3. The process, according to claim 1 , wherein in the step (b) the application includes a ratio of between 10 and 30 ml of GO dispersion in ethyl alcohol per cm2 of PA membrane.

4. The process, according to claim 1 , wherein in step (b), the low rotation step in spin-coat is between 500 and 1000 rpm and the high rotation step is between 1600 and 2400 rpm.

5. The process, according to claim 1 , wherein after step (d) the membranes have properties of a permeability greater than 3.5 L/h·m2·bar, saline rejection greater than 96%, and preservation of oxygenates groups and groups related to polyamide after exposure to 1000 ppm/h of chlorine.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 21, 2025
From: SUHETT DE SOUZA, RODRIGO; DE ARAUJO CID DA SILVA, RICARDO
To: PETRÓLEO BRASILEIRO S.A. - PETROBRAS
Reel/Frame 069937/0129 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 21, 2025
From: LUIZA BRASIL ZANON, YARA; GOMIDE DE CASTRO, VINÍCIUS; CRISTINA SANTOS AMARAL MORAVIA, MIRIAM; GOULART SILVA, GLAURA; CAROLINE DE JESUS RIBEIRO, BRUNA; LUIZA SILVESTRE ASSIS, ANA
To: UNIVERSIDADE FEDERAL DE MINAS GERAIS - UFMG; UNIVERSIDADE FEDERAL DE MINAS GERAIS - UFMG
Reel/Frame 069937/0135 →
Priority Claims (1)
BR 10 2021 023979 4 · Nov 27, 2021 · national
Continuity (1)
Related Publication 20230166215A1 · Jun 1, 2023
References Cited (9)
US 10456754B2 · Hogen-esch et al. · 2019 [cited by applicant]
US 20170361284A1 · Lee et al. · 2017 [cited by applicant]
Shao et al, “Graphene oxide modified polyamide reverse osmosis membranes with enhanced chlorine resistance,” Journal of Membrane Science 525 (2017) 9-17 (Year: 2017). [cited by examiner]
Ashfaq et al. (Sep. 2020) “Functionalization Of Reverse Osmosis Membrane With Graphene Oxide To Reduce Both Membrane Scaling And Biofouling”, Carbon, 166:374-387. [cited by applicant]
Choi et al. (Nov. 2013) “Layer-by-Layer Assembly of Graphene Oxide Nanosheets on Polyamide Membranes for Durable Reverse-Osmosis Applications”, ACS Applied Materials & Interfaces, 5(23):12510-12519. [cited by applicant]
Inurria et al. (Feb. 1, 2019) “Polyamide Thin-film Nanocomposite Membranes With Graphene Oxide Nanosheets: Balancing Membrane Performance And Fouling Propensity”, Desalination, 451:139-147. [cited by applicant]
Mahdavi et al. (May 2018) “Zwitterion Functionalized Graphene Oxide/polyamide Thin Film Nanocomposite Membrane: Towards Improved Anti-fouling Performance For Reverse Osmosis”, Desalination, 433:94-107. [cited by applicant]
Shao et al. (Dec. 2016) “Graphene Oxide Modified Polyamide Reverse Osmosis Membranes with Enhanced Chlorine Resistance”, Journal of Membrane Science, 525:9-17. [cited by applicant]
Shao et al. (Dec. 2017) “Layer-by-layer Self-assembly TiO2 And Graphene Oxide On Polyamide Reverse Osmosis Membranes With Improved Membrane Durability”, Desalination, 423:21-29. [cited by applicant]