IP Library › Granted Patent US 12,434,222
Granted Patent B2
US 12,434,222 · App. 18/165,091 · Granted Oct 7, 2025

Cross-linked polymeric ammonium salts and their use in absorbing organic contaminants

Inventors: Seetha M. Coleman-Kammula (Newark, DE); Garret D. Figuly (Wilmington, DE); Charles R. Powley (Wilmington, DE); Debora Flanagan Massouda (Wilmington, DE)
Assignee: STRIDE
B01J20/267B01J20/20B01J20/3416B01J20/3425B01J20/3475C02F1/288C02F1/283C02F1/285C02F2101/36C02F2103/007C02F2103/34C02F2103/42C02F2303/16
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Quick Facts
Patent No.
US 12,434,222
App. No.
18/165,091
Granted
Oct 7, 2025
Kind
B2
Abstract

Use of poly(alkylamine)-derived (PAD) self-supported cross-linked polymeric ammonium salts and ionomer hydrogels for adsorbing and desorbing organic contaminants, specifically per and polyfluoro alkyl substances (PFAS) from water.

Claims (25)

1. A method for absorbing at least one PFAS molecule from an aqueous medium wherein said at least one PFAS molecule comprises a water soluble fluorinated amphiphilic structure with a carbon chain length that ranges from 4 to at least 14 carbon atoms which comprises:

contacting said PFAS molecule with at least one self-supported crosslinked polymeric ammonium salt, wherein said salt is a water-insoluble, solid polyelectrolyte having at least one polymer chain,

wherein said polyelectrolyte comprises a copolymer network wherein ammonium nitrogen atoms are separated by group Y or group Z ordered along (i) polymer chains as N—Z—[N—Y—N—Z] n —N and along (ii) cross-linking polymer chains as Y, or Y—N—Z—N—[Y—N—Z—N] n —Y, wherein said cross linking polymer chains connect between one ammonium nitrogen atom in one polymer chain, and another ammonium nitrogen atom in another polymer chain and (iii) along pendant polymer chains as Y—N—Z—[N—Y—N—Z] n —N wherein said pendant chains originate at ammonium nitrogen atoms in other polymer chains, wherein n has a value from 0 to any higher integer,

wherein group Y is an n-alkylene group or an alkyl substituted n-alkylene group, wherein said n-alkylene group or said alkyl substituted n-alkylene group has from 2 to at least 20 carbon atoms; and

group Z is a hydrocarbylene group containing from 2 to 50 carbon atoms, said hydrocarbylene group optionally substituted with one or more hydroxyl, ether, amino, thioether, keto, ester, silyl group or heterocyclic rings; and at least 25% of the ammonium nitrogen atoms are secondary ammonium nitrogen atoms,

with the result that said PFAS molecules are absorbed into said at least one crosslinked polymeric ammonium salt.

2. The method of claim 1 wherein said hydrocarbylene groups contain from 1 to 30 carbon atoms, and said PFAS molecule is contacted in the optional presence of a flocculent or a coagulant.

3. The method of claim 1 wherein the at least one crosslinked polymeric ammonium salt has a swell factor of at least about 2 in water.

4. The method of claim 3 wherein the at least one crosslinked polymeric ammonium salt is combined with an amount of granulated activated carbon.

5. The method of claim 3 wherein the at least one crosslinked polymeric ammonium salt is a poly(alkylamine) ammonium salt.

6. The method of claim 5 wherein the poly(alkylamine) ammonium salt is combined with an amount of granulated activated carbon.

7. The method of claim 5 wherein the poly(alkylamine) ammonium salt is prepared from hexamethylene diamine and 1,10-dibromodecane using DMF/methanol as solvent.

8. The method of claim 5 wherein the poly(alkylamine) ammonium salt is prepared from polyethylene imine and 1,10-dibromodecane using DMF/methanol as solvent.

9. The method of claim 1 which includes the additional steps of (i) desorbing said at least one PFAS molecule from said at least one crosslinked polymeric ammonium salt, by contacting the at least one crosslinked polymeric ammonium salt, which contains PFAS molecules with an aqueous alkaline solution having a pH in the range of from about 8 to 14 with the result that the at least one PFAS molecule is released from the at least one crosslinked polymeric ammonium salt, and (ii) recovering the at least one PFAS molecule and the at least one crosslinked polymeric ammonium salt.

10. The method of claim 9 , wherein the crosslinked polymeric ammonium salt is a poly(alkylamine) ammonium salt and the PFAS molecule is perfluoro-octanoic acid (PFOA).

11. The method of claim 10 wherein the crosslinked polymeric ammonium salt is a poly(alkylamine) ammonium salt prepared from hexamethylene diamine and 1,10-dibromodecane using DMF/methanol as solvent.

12. The method of claim 10 wherein the crosslinked polymeric ammonium salt is a poly(alkylamine) ammonium salt prepared from polyethylene imine and 1,10-dibromodecane using DMF/methanol as solvent.

13. The method of claim 1 which includes the additional steps of (i) desorbing said at least one PFAS molecule from said at least one crosslinked polymeric ammonium salt by contacting the at least one crosslinked polymeric ammonium salt which contains said at least one PFAS molecule with an ammonium hydroxide/methanol solution with the result that the at least one PFAS molecule is released from the at least one crosslinked polymeric ammonium salt, and (ii) recovering the at least one PFAS molecule and the at least one crosslinked polymeric ammonium salt.

14. The method of claim 13 , wherein the crosslinked polymeric ammonium salt is a poly(alkylamine) ammonium salt and the PFAS molecule is perfluoro-octanoic acid (PFOA).

15. The method of claim 1 which includes the additional steps of (i) desorbing said at least one PFAS molecule from said at least one crosslinked polymeric ammonium salt by contacting a crosslinked polymeric ammonium salt which contains a PFAS molecule with a sodium hydroxide/water solution with the result that the PFAS molecule is released from the crosslinked polymeric ammonium salt, and (ii) recovering the PFAS molecule and the crosslinked polymeric ammonium salt.

16. The method of claim 15 , wherein the crosslinked polymeric ammonium salt is a poly(alkylamine) ammonium salt and the PFAS molecule is perfluoro-octanoic acid (PFOA).

17. The method of claim 1 wherein said at least one PFAS molecule comprises a telomer alcohol of the type used in aqueous fire-fighting foam compositions.

18. The method of claim 1 wherein the at least one crosslinked polymeric ammonium salt is deployed in a polar organic chemical integrative sampler (POCIS).

19. The method of claim 1 wherein the aqueous medium comprises at least one of stagnant pools, wells, rivers, springs, estuarine systems, and industrial and municipal wastewater streams.

20. The method of claim 1 wherein said at least one PFAS molecule is contacted with a mixture of said crosslinked polymeric ammonium salts in the optional presence of at least one flocculent or at least one coagulant.

Continuity (4)
Continuation In Part 17822317 · Aug 25, 2022
Continuation 17480579 · Sep 21, 2021
Provisional Application 63081129 · Sep 21, 2020
Related Publication 20230182113A1 · Jun 15, 2023
References Cited (43)
US 3882153A · Seki et al. · 1975 [cited by applicant]
US 5633344A · Figuly · 1997 [cited by applicant]
US 9815712B2 · Diallo et al. · 2017 [cited by applicant]
US 10744497B2 · Zipplies et al. · 2020 [cited by applicant]
US 20150053620A1 · Suri et al. · 2015 [cited by applicant]
US 20170297926A1 · Nickelsen et al. · 2017 [cited by applicant]
US 20190185352A1 · Chiang · 2019 [cited by applicant]
US 20190263679A1 · Phillips et al. · 2019 [cited by applicant]
US 20190300387A1 · Nelson · 2019 [cited by applicant]
US 20200206793A1 · Brady · 2020 [cited by applicant]
US 20200262936A1 · Barin et al. · 2020 [cited by applicant]
US 20200283309A1 · Reid et al. · 2020 [cited by applicant]
US 20200306726A1 · James et al. · 2020 [cited by applicant]
US 20210008522A1 · Reeve · 2021 [cited by examiner]
US 20220017645A1 · Barin · 2022 [cited by examiner]
US 20240109989A1 · Leibfarth · 2024 [cited by examiner]
WO WO2007017864 · 2007 [cited by applicant]
WO WO2019186166 · 2019 [cited by applicant]
WO WO2020113004 · 2020 [cited by applicant]
WO WO2020167375 · 2020 [cited by applicant]
Senevirathna et al. (Chemosphere, 2010, 80, 647-651). (Year: 2010). [cited by examiner]
McCleaf et al. (Water Research, 2017, 120, 77-87). (Year: 2017). [cited by examiner]
Yu et al. (Water Research, 2009, 43, 1150-1158). (Year: 2009). [cited by examiner]
Liu et al. (Environmental Science & Technology, 2015, 49, 8657-8665). (Year: 2015). [cited by examiner]
Ray et al. (Water Research, 2019, 157, 454-462). (Year: 2019). [cited by examiner]
Sun et al. (Journal of Water Process Engineering, 2020, 37, 101416). (Year: 2020). [cited by examiner]
Xie et al. (Journal of Hazardous Materials, 2022, 431, 128521). (Year: 2022). [cited by examiner]
Ateia, M., Attia, M. F., Maroli, A., Tharayil, N., Alexis, F., Whitehead, D. C., & Karanfil, T. (2018). Rapid Removal of Poly- and Perfluorinated Alkyl Substances by Poly(ethylenimine)—Functionalized Cellulose Microcrys… [cited by applicant]
Chularueangaksorn, P., Tanaka, S., Fujii, S., & Kunacheva, C. (2014). Adsorption of perfluorooctanoic acid (PFOA) onto anion exchange resin, non-ion exchange resin, and granular-activated carbon by batch and column. Des… [cited by applicant]
Stebel, E. K., Pike, K. A., Nguyen, H., Hartmann, H. A., Klonowski, M. J., Lawrence, M. G., . . . Edmiston, P. L. (2019). Adsorption of short-chain to long-chain perfluoroalkyl substances using swellable organically mod… [cited by applicant]
Xiao, L., Ling, Y., Alsbaiee, A., Li, C., Helbling, D. E., & Dichtel, W. R. (2017). β Cyclodextrin Polymer Network Sequesters Perfluorooctanoic Acid at Environmentally Relevant Concentrations. Journal of the American Ch… [cited by applicant]
Yan, B., Wang, J., & Liu, J. (2021). STXM-XANES and computational investigations of adsorption of per- and polyfluoroalkyl substances on modified clay. Water Research, 201, 1-10. [cited by applicant]
Zhang, D., Luo, Q., Gao, B., Chiang, D., Woodward, D., & Huang, Q. (2016). Sorption of Perfluorooctanoic Acid, Perfluorooctane Sulfonate and Perfluoroheptanoic Acid 2 on Granular Activated Carbon. Chemosphere, 144, 2336… [cited by applicant]
Author: Genuis et al.; Title: Human Detoxification of Perfluorinated Compounds ;Jun. 19, 2010, Publisher: Public Health, 124 (2010) 367-375 (11 pages). (Year: 2010). [cited by applicant]
Author: Johnson et al.; Title: Cholestyramine-Enhanced Fecal Elimination of Carbon-14 in Rats after Administration of Ammonium [14C)Perfluorooctanoate or Potassium [14C)Perfluorooctanesulfonate; 1984, Publisher: Fundame… [cited by applicant]
Author: Gobelius et al.; Title: Calibration and application of passive sampling for per- and polyfluoroalkyl substances in a drinking water treatment plant;2019, Publisher: Journal of Hazardous Materials 362 (2019) 230-… [cited by applicant]
Author: Mitsubishi Chemical Corporation; Title: Product Data Sheet DIAION WA20; 2021; (2 pages). (Year: 2021). [cited by applicant]
Author: Pyvot; Title: Polyamine Type DIAION WA20, WA21J; 2021; (2 pages). https://pyvot.tech/product/ polyamine-type-diaion-wa20-wa21j/. (Year: 2021). [cited by applicant]
United States Patent and Trademark Office; DIAION WA 20 trademark; 1 page. (Year: 1982). [cited by applicant]
Wayback machine for Author: Pyvot; Title: Polyamine Type DIAION WA20, WA21J; 2021; (1 page). https://pyvot.tech/product/ polyamine-type-di aion-wa20-wa21j/. (Year: 2021). [cited by applicant]
International Search Report and Written Opinion dated Jan. 18, 2022; 9 pgs. [cited by applicant]
Mohamed Ateia, MD Arifuzzaman, Steven Pellizzeri, Mohamed F. Attia, Nishanth Tharayil, Jeffrey N. Anker, Tanju Karanfil (2019) Water Research 163 (2019) 114874, 8 pages, www.elsevier.com/locate/watres. [cited by applicant]
Extended European Search Report dated Aug. 30, 2024; (6 pgs). [cited by applicant]