# US 12,767,560 B2 · Hydrothermal system for treatment of adsorbent regeneration byproducts

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- Number: US 12,767,560 B2
- Document ID: US12767560B2
- Status: Granted
- Kind: B2
- Application number: 18/261,618
- Filed: 2022-01-13
- Published: 2024-11-28
- Granted: 2026-10-20
- Earliest claimed: 2021-01-15
- Assignees: University of Washington
- Applicants: University of Washington
- Inventors: Brian Pinkard; Igor Novosselov
- Web page: https://patentgrep.com/patent/US12767560B2

## CPC

- C02F 1/025: {Thermal hydrolysis}
- C02F 1/5245: {using basic salts, e.g. of aluminium and iron}
- C02F 1/66: by neutralisation; pH adjustment (for degassing C02F1/20; using ion-exchange C02F1/42; for flocculation or precipitation of suspended impurities C02F1/52; for removing dissolved compounds C02F1/58)
- C02F 2101/101: {Sulfur compounds}
- C02F 2101/14: Fluorine or fluorine-containing compounds
- C02F 2101/36: containing halogen
- C02F 2209/02: Temperature
- C02F 2209/03: Pressure
- 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)

## Abstract

A continuous reactor and method for destroying contaminants, such as perfluoroalkyl and/or polyfluoroalkyl substances in various feedstocks. Liquid byproducts are continuously hydrolyzed in an aqueous alkaline solution to achieve greater than 99.99% destruction of the contaminants. Continuous hydrolysis achieves a greater conversion efficiency as compared to batch reactions and has a wide application of contaminated feedstocks.

## Claims

### Claim 1

A method for destroying perfluoroalkyl and/or polyfluoroalkyl substances, comprising:
introducing a liquid byproduct including a perfluoroalkyl and/or polyfluoroalkyl substance to a reactor;
hydrolyzing in the reactor under alkaline conditions the perfluoroalkyl and/or polyfluoroalkyl substance in the liquid byproduct, wherein a temperature of the reactor is maintained between 300° C. and 400° C., wherein a pressure in the reactor is maintained between 0.1 MPa and 50 MPa, and wherein a pH in the reactor is maintained between 13 and 15.3 (OH− ion loading of between 0.1 M and 20 M); and
producing a continuous stream of product from the reactor, wherein the liquid byproduct is selected from:
a brine containing water, 20% wt. or less of a salt or base, and 1% wt. or less of the perfluoroalkyl and/or polyfluoroalkyl substance, or
a solution containing 50 to 90 vol % of an alcohol, 10 to 50 vol % of water, 1 to 5 wt % of a salt or a base, and the perfluoroalkyl and/or polyfluoroalkyl substance, or
a byproduct from ozone foam fractionate processing having 100 ug/L (ppb) to 10 mg/L (ppm) of the perfluoroalkyl and/or polyfluoroalkyl substance, or
a byproduct from thermal treatment of soil or spent sorbents containing the perfluoroalkyl and/or polyfluoroalkyl substance, or
a byproduct from wet scrubbers used to capture contaminants in an emission stream of incinerators, rotary kilns or other thermal destructive processes; or
an aqueous film-forming foam having 0.3 to 6% by weight of the perfluoroalkyl and/or polyfluoroalkyl substance; or
reverse osmosis reject brine having from 1 ug/L (ppb) to 10 mg/L (ppm) of the perfluoroalkyl and/or polyfluoroalkyl substance; or
nanofiltration reject brine having from 1 ug/L (ppb) to 10 mg/L (ppm) of the perfluoroalkyl and/or polyfluoroalkyl substance.

### Claim 2 (depends on 1)

The method of claim 1, comprising mixing the liquid byproduct with an alkaline amendment before the reactor, wherein the alkaline amendment is NaOH, KOH, LiOH, NH4OH, Ca(OH)2 or a combination thereof.

### Claim 3 (depends on 1)

The method of claim 1, comprising introducing the liquid byproduct and an aqueous alkaline solution separately through a first inlet and a second inlet to the reactor.

### Claim 4 (depends on 1)

The method of claim 1, further comprising cooling an effluent leaving the reactor to produce a liquid effluent.

### Claim 5 (depends on 4)

The method of claim 4, further comprising cooling the effluent with the liquid byproduct before introducing to the reactor.

### Claim 6 (depends on 4)

The method of claim 4, further comprising introducing a neutralizing agent to the liquid effluent to adjust pH of the liquid effluent.

### Claim 7 (depends on 6)

The method of claim 6, wherein the neutralizing agent includes HCl or H2SO4.

### Claim 8 (depends on 4)

The method of claim 4, comprising adding a calcium salt to the liquid effluent to produce precipitates, wherein the precipitates include CaF2 or CaSO4 or both.

### Claim 9 (depends on 4)

The method of claim 4, comprising measuring one or more parameters of the liquid effluent including a concentration of the contaminant in the liquid effluent, a concentration of destruction byproducts, or a pH of the liquid effluent, or a combination thereof.

### Claim 10 (depends on 9)

The method of claim 9, wherein the concentration of destruction byproducts is an F− ion concentration.

### Claim 11 (depends on 1)

The method of claim 1, wherein the pressure in the reactor is between a pressure sufficient to maintain a liquid reaction environment and 50 MPa.

### Claim 12

A method for destroying a contaminant in a byproduct from an adsorbent media regeneration or reactivation process, comprising:
introducing a byproduct from an adsorbent media regeneration or reactivation process to a reactor; and
hydrolyzing in the reactor under alkaline conditions a contaminant in the byproduct, wherein a temperature of the reactor is maintained between 300° C. and 400° C., wherein a pressure in the reactor is maintained between 0.1 MPa and 50 MPa, and wherein a pH in the reactor is maintained between 13 and 15.3 (OH− ion loading of between 0.1 M and 20 M) wherein the byproduct is a liquid selected from:
a brine containing water, 20% wt. or less of a salt or base, and 1% wt. or less of the contaminant, or
a solution containing 50 to 90 vol % of an alcohol, 10 to 50 vol % of water, 1 to 5 wt % of a salt or a base, and the contaminant.

### Claim 13 (depends on 12)

The method of claim 12, wherein the contaminant is selected from a perfluoroalkyl compound, a polyfluoroalkyl compound, perfluorooctanesulfonate, perfluorooctanoic acid, 1′4-dioxane, a polycholorinated biphenyl, a hydrocarbon, and a volatile organic carbon, or a combination thereof.

### Claim 14 (depends on 12)

The method of claim 12, wherein an absorbent media in the absorbent media regeneration or reactivation process is granular activated carbon or an ion exchange resin.
