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US-20260124585-A1 - METHOD FOR NANOFILTRATION OF A SOLUTE-CONTAINING COMPOSITION

US20260124585A1US 20260124585 A1US20260124585 A1US 20260124585A1US-20260124585-A1

Abstract

The present disclosure provides a filtration membrane. The filtration membrane includes a thermoplastic substrate, a first layer comprising a polysulfone, a polyvinylpyrrolidone, and a pentaamine, and a second layer comprising the pentaamine and reacted units of a phthaloyl chloride cross-linked to form a polyamide. A method of preparing the filtration membrane by impregnating pentaamine in an ultrafiltration support matrix for rapidly fabricating a hyper-cross-linked polyamide membrane is also disclosed. The membrane prepared by the method of present disclosure can be used for organic solvent nanofiltration (OSN).

Inventors

  • Abdul Waheed
  • Umair Baig

Assignees

  • KING FAHD UNIVERSITY OF PETROLEUM AND MINERALS

Dates

Publication Date
20260507
Application Date
20251231

Claims (20)

  1. 1 . (canceled)
  2. 2 . The method of claim 16 , wherein the pentaamine in the first layer of the filtration membrane is physically adsorbed and/or dispersed in the polysulfone and the polyvinylpyrrolidone.
  3. 3 . The method of claim 16 , wherein the pentaamine in the second layer of the filtration membrane is covalently cross-linked with units of the phthaloyl chloride through at least one of a primary amine group and a secondary amine group of a first pentaamine and at least one of a primary amine group and a secondary amine group of a second pentaamine.
  4. 4 . The method of claim 16 , wherein the second layer of the filtration membrane comprises the polyamide in a hyper-branched cross-linked matrix.
  5. 5 . The method of claim 16 , wherein the pentaamine is a tetraethylenepentamine.
  6. 6 . The method of claim 16 , wherein the second layer of the filtration membrane is in the form of nanoparticles with a diameter of 10 to 500 nm.
  7. 7 . The method of claim 16 , wherein the first layer of the filtration membrane is in the form of vertical hollow tubes having a diameter of 0.5 to 10 μm and a length of 5 to 50 μm.
  8. 8 . The method of claim 7 , wherein the second layer of the filtration membrane covers the vertical hollow tubes of the first layer.
  9. 9 . The method of claim 16 , wherein the second layer of the filtration membrane has a thickness of 0.5 to 5 μm.
  10. 10 . The method of claim 16 , wherein a water contact angle of the filtration membrane is from 75 to 85°.
  11. 11 . The method of claim 16 , wherein the filtration membrane comprises carbon in an amount of 75 to 78% by weight, oxygen in an amount of 14 to 17% by weight, sulfur in an amount of 4 to 7% by weight, and nitrogen in an amount of 1 to 4% by weight based on a total weight of the filtration membrane.
  12. 12 . The method of claim 16 , wherein a surface roughness of the filtration membrane is from 24 to 27 nm.
  13. 13 . (canceled)
  14. 14 . The method of claim 16 , wherein the filtration membrane has a rate of flux of methanol of 5 to 7 L m −2 h −1 at a pressure of 4 bar.
  15. 15 . The method of claim 16 , wherein the filtration membrane has a rate of flux of methanol of 25 to 30 L m −2 h −1 at a pressure of 20 bar.
  16. 16 . A method of nanofiltration, comprising: passing a composition through a filtration membrane, wherein the composition comprises at least one solvent and at least one solute, collecting a permeate passing through the filtration membrane to obtain a purified composition having a reduced amount of the solute; wherein the filtration membrane comprises, in the following order: a thermoplastic substrate, a first layer comprising a polysulfone, a polyvinylpyrrolidone, and a pentaamine, a second layer comprising the pentaamine and reacted units of a phthaloyl chloride cross-linked to form a polyamide.
  17. 17 . The method of claim 16 , wherein the filtration membrane has a rejection profile of the solute of from 85 to 100% by weight in methanol.
  18. 18 . The method of claim 17 , wherein the solute comprises Congo Red, Eriochrome Black T, and Methylene Blue.
  19. 19 . The method of claim 16 , wherein the solvent is selected from the group consisting of water, methanol, ethanol, and isopropanol.
  20. 20 . The method of claim 16 , wherein the solvent is methanol, the solute is Congo Red, and the membrane has a rejection profile from 95 to 100% by weight.

Description

STATEMENT REGARDING PRIOR DISCLOSURE BY THE INVENTORS Aspects of the present disclosure were disclosed in an article titled “Exploiting phase inversion for penta-amine impregnation of ultrafiltration support matrix for rapid fabrication of a hyper-cross-linked polyamide membrane for organic solvent nanofiltration” published in Volume 169, Process Safety and Environmental Protection, which is incorporated herein by reference in its entirety. STATEMENT OF ACKNOWLEDGEMENT The support provided by the Interdisciplinary Research Center for Membranes and Water Security, King Fahd University of Petroleum and Minerals, Saudi Arabia, through project INMW2213 is gratefully acknowledged. BACKGROUND Technical Field The present disclosure relates to membranes, and more particularly, relates to a penta-amine-impregnated ultrafiltration support matrix for the rapid fabrication of a hyper-cross-linked polyamide membrane. Discussion of Related Art The “background” description provided herein is for the purpose of generally presenting the context of the disclosure. Work of the presently named inventors, to the extent it is described in this background section, as well as aspects of the description which may not otherwise qualify as prior art at the time of filing, are neither expressly nor impliedly admitted as prior art against the present invention. One of the major challenges faced by the pharmaceutical industry is organic solvent waste. 80% of the waste generated in pharmaceutical companies consists of organic solvents. Such organic solvents are needed in large quantities for the separation and purification of active pharmaceutical ingredients (API); hence, recovering organic solvents can cover up to 80% of the capital cost in such industries. The need to develop efficient, cost-effective technologies with a lesser footprint for the recovery and purification of organic solvents exists. Among a multitude of technologies available for recovering organic solvents, membrane-based separation is advantageous due to its low operation and capital cost, ease of handling, smaller carbon footprint, and ease of tunability. The development of efficient membranes for organic solvent nanofiltration (OSN) is an area to explore for a better future of industrial development. Polyamide thin film composite (PA-TFC) membranes are evolving and have a potential for different applications such as desalination, water treatment, and organic solvent nanofiltration (OSN). Generally, PA-TFC membranes are fabricated by interfacial polymerization (IP), in which a reaction takes place at an interface between an aqueous solution of an amine (for example, meta-phenylenediamine (MPD)) and non-aqueous solution of a crosslinker, such as trimesoyl chloride (TMC). Conventionally, PA-TFC membranes are fabricated by following two steps. The first step is the fabrication of an ultrafiltration support, such as polyacrylonitrile (PAN), polysulfone (PSU), and/or polyether sulfone (PESf), through dry or wet phase inversion. During phase inversion, the polymer dope solution is cast on a non-woven fabric, such as polyester terephthalate (PET), which is subsequently dipped in a non-solvent coagulation bath. The dipping in the non-solvent coagulation bath leads to the inversion of polymer from liquid to solid phase, which leads to the ultrafiltration support. After phase inversion is the second step of PA-TFC membrane fabrication, in which the ultrafiltration support is dipped simultaneously in deionized (DI) water and sodium dodecyl sulfate (SDS) solution for 24 hours each, and then the ultrafiltration support is impregnated by dipping the support in aqueous amine solution. Afterward, an amine-impregnated ultrafiltration support is dipped in another solution of an appropriate crosslinker, such as TMC. Advances have been made for fabricating a variety of membranes by adopting a traditional two-step IP process. Efforts have been focused on improving the membrane performance by altering the chemistry of the active layer of the membrane. Various additives such as nanoparticles, covalent organic frameworks (COFs), and metal-organic frameworks (MOFs) have been incorporated in either active layer or ultrafiltration support of the membranes. In addition, a variety of interlayers has also been explored in order to develop membranes with desired surface geometries and performance [J. E. Gu, J. S. Lee, S. H. Park, I. T. Kim, E. P. Chan, Y. N. Kwon, J. H. Lee, Tailoring interlayer structure of molecular layer-by-layer assembled polyamide membranes for high separation performance, Appl Surf Sci. 356 (2015) 659-667, incorporated herein by reference in its entirety]. Less attention has been directed to improving the procedure of membrane fabrication, which may lead to better membranes with less effort and resources. A relatively less explored and robust methodology has been explored for fabricating crosslinked PA-TFC membranes, which is simple and rapid compared to conventional IP pro