IP Library › Granted Patent US 12,655,268
Granted Patent B2
US 12,655,268 · App. 18/738,615 · Granted Jun 16, 2026

Methods for recycling cotton and polyester fibers from waste textiles

Inventors: Florin G. Barla (Danville, VA); Todd Showalter (Danville, VA); Hsun-Cheng Su (Chapel Hill, NC); Jeremy Jones (Danville, VA); Iulian Bobe (Danville, VA)
Assignee: Circ, LLC
C08J11/26C07C51/09C07C63/26C08B16/00C08J11/14C08L1/02D06M13/184C08J2367/02C08J2401/02
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 12,655,268
App. No.
18/738,615
Granted
Jun 16, 2026
Kind
B2
Abstract

Systems and methods are provided that involve a subcritical water reaction to recycle the cellulose and polyester components of waste cotton and cotton/polyester blend textiles that would otherwise be discarded or disposed of. Specifically, the disclosed methods provide for treatment of the waste textiles to produce advanced materials including cellulose and terephthalic acid (TPA) with a low environmental impact. The cellulose and TPA that are produced are of a high quality allowing for production of regenerated cellulose and regenerated polyethylene terephthalate (PET) suitable for fiber spinning and textile applications.

Claims (19)

1 . A method of producing one or both of cellulose and terephthalic acid (TPA) from a waste textile material comprising cotton or cotton/polyester blend material, the method comprising:

treating the waste textile material in a subcritical water reactor at a temperature of about 105° C. to 190° C., a pressure of about 40 to 300 psi, or both for about 0 to 90 minutes,

wherein one or both of a cellulose that comprises a degree of polymerization ranging from about 150-2500 and a dissolved TPA and ethylene glycol (EG) is produced.

2 . The method of claim 1 , wherein the waste textile material comprises cotton/polyester blend material and the treating in the subcritical water reactor comprises a pH ranging from about 10-14.

3 . The method of claim 2 , further comprising recovering the TPA.

4 . The method of claim 2 , further comprising recovering the cellulose.

5 . The method of claim 4 , further comprising subjecting the recovered cellulose to a disintegration process.

6 . The method of claim 1 , wherein the waste textile material comprises cotton/polyester blend material and the treating in the subcritical water reactor comprises a first treating at a pH ranging from about 10-14, wherein the dissolved TPA and EG are produced, and a second treating of the cellulose that is produced in the first treating at a pH ranging from about 2-4, wherein the cellulose that is produced in the second treating in the subcritical water reactor comprises a degree of polymerization ranging from about 150-2000.

7 . The method of claim 6 , further comprising subjecting the cellulose produced after the second treating to one or more steps of wash, disintegration, sour wash, activation process, dissolution dope, or wet spinning.

8 . The method of claim 1 , wherein the waste textile material comprises cotton material, the treating in the subcritical water reactor comprises a pH ranging from about 2-4, and further comprising recovering the cellulose that is produced.

9 . The method of claim 8 , further comprising subjecting the recovered cellulose to a mechanical disintegration process.

10 . The method of claim 1 , further comprising removing color from the waste textile material before, during, or after treating with the subcritical water reactor.

11 . The method of claim 10 , wherein the color removal comprises treatment with one or more of hydrogen peroxide, sodium peroxide, sodium hypochlorite, calcium hypochlorite, dimethyl sulfoxide, lithium hypochlorite, sodium perborate, ozone, oxygen, activated carbon, biochar, sodium carbonate, peracetic acid, potassium permanganate, persulfate, sodium chloride, calcium oxychloride, chloramine, chlorine dioxide, sulfur dioxide, sodium hydrosulfite, or TAED (tetra-acetyl-ethylene-di-amine).

12 . The method of claim 1 , wherein the subcritical water reactor treatment comprises one or more of methanol, ethanol, isopropanol, tetra-n-butylphosphonium bromide (TBPB), or benzyltributylammonium chloride (BTBAC), or co-polymers thereof.

13 . The method of claim 1 , wherein the ratio of waste textile material to water within the subcritical water reactor is about 1:5-1:95.

14 . The method of claim 1 , further comprising adjusting the pH of water within the subcritical water reactor before subcritical water treatment.

15 . The method of claim 14 , wherein the pH is adjusted to about 2-4.

16 . The method of claim 14 , wherein the pH is adjusted to about 10-14.

17 . The method of claim 14 , wherein the pH is adjusted using 0.01-5% (v/v) organic acid, 0.5-20% (w/v) sodium hydroxide, or 0.5-20% (w/v) potassium hydroxide.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 10, 2024
From: BARLA, FLORIN G.; SHOWALTER, TODD; SU, HSUN-CHENG; JONES, JEREMY; BOBE, IULIAN
To: TYTON BIOSCIENCES, LLC
Reel/Frame 067674/0029 →
CHANGE OF NAME Recorded Jun 10, 2024
From: TYTON BIOSCIENCES LLC
To: CIRC, LLC
Reel/Frame 067681/0740 →
Continuity (6)
Continuation 17850030 · Jun 27, 2022
Continuation 17019877 · Sep 14, 2020
Continuation 16695969 · Nov 26, 2019
Continuation 16246044 · Jan 11, 2019
Provisional Application 62616543 · Jan 12, 2018
Related Publication 20240327603A1 · Oct 3, 2024
References Cited (102)
US 4436586A · Elmore · 1984 [cited by applicant]
US 5151368A · Brimhall et al. · 1992 [cited by applicant]
US 5236959A · Oakley et al. · 1993 [cited by applicant]
US 6468390B1 · Snekkenes et al. · 2002 [cited by applicant]
US 6545061B1 · Murdoch et al. · 2003 [cited by applicant]
US 6772767B2 · Mua et al. · 2004 [cited by applicant]
US 7544635B2 · Liang et al. · 2009 [cited by applicant]
US 8268126B2 · Fang · 2012 [cited by applicant]
US 8460898B2 · Diner · 2013 [cited by applicant]
US 8546560B2 · Kilambi · 2013 [cited by applicant]
US 8637718B2 · Gupta · 2014 [cited by applicant]
US 8679352B2 · Olivier et al. · 2014 [cited by applicant]
US 9388529B2 · Lindstrom et al. · 2016 [cited by applicant]
US 9469693B2 · Henriksson et al. · 2016 [cited by applicant]
US 9611371B2 · Walker · 2017 [cited by applicant]
US 9751955B2 · Lindstrom et al. · 2017 [cited by applicant]
US 9902815B2 · Tamminen et al. · 2018 [cited by applicant]
US 10266610B2 · Varhimo et al. · 2019 [cited by applicant]
US 10300464B2 · Lin et al. · 2019 [cited by applicant]
US 10322395B2 · Kumar et al. · 2019 [cited by applicant]
US 10392565B2 · Xiao et al. · 2019 [cited by applicant]
US 10501599B2 · Barla · 2019 [cited by examiner]
US 10603651B2 · Kumar et al. · 2020 [cited by applicant]
US 11108629B1 · Cahyadi · 2021 [cited by examiner]
US 11370895B2 · Barla · 2022 [cited by examiner]
US 12006403B2 · Barla · 2024 [cited by examiner]
US 20040154760A1 · Dean · 2004 [cited by applicant]
US 20070193706A1 · Kirov et al. · 2007 [cited by applicant]
US 20080097120A1 · Jermolovicius et al. · 2008 [cited by applicant]
US 20090053777A1 · Hennessey et al. · 2009 [cited by applicant]
US 20100178677A1 · Dunson et al. · 2010 [cited by applicant]
US 20130192123A1 · Maschmeyer et al. · 2013 [cited by applicant]
US 20130276801A1 · Byrd, Jr. et al. · 2013 [cited by applicant]
US 20140234936A1 · Kusuda et al. · 2014 [cited by applicant]
US 20140242684A1 · Harlick et al. · 2014 [cited by applicant]
US 20140275299A1 · Bedwell et al. · 2014 [cited by applicant]
US 20140331993A1 · Kumar et al. · 2014 [cited by applicant]
US 20140345341A1 · Fiato et al. · 2014 [cited by applicant]
US 20150225901A1 · Asikainen et al. · 2015 [cited by applicant]
US 20160053058A1 · Tabor · 2016 [cited by applicant]
US 20160311997A1 · Rangaswamy et al. · 2016 [cited by applicant]
US 20170008826A1 · Essaddam · 2017 [cited by applicant]
US 20170218162A1 · Walker et al. · 2017 [cited by applicant]
US 20170362775A1 · Juvonen et al. · 2017 [cited by applicant]
US 20180002837A1 · Yu et al. · 2018 [cited by applicant]
US 20180127515A1 · Ropponen et al. · 2018 [cited by applicant]
US 20180347111A1 · Lee · 2018 [cited by applicant]
US 20190255506A1 · Kumar et al. · 2019 [cited by applicant]
CN 1139719 · 1997 [cited by applicant]
CN 101448581 · 2009 [cited by applicant]
CN 102392378 · 2012 [cited by applicant]
CN 106674588 · 2017 [cited by applicant]
EP 1383955 · 2010 [cited by applicant]
EP 2171154 · 2010 [cited by applicant]
EP 1454009 · 2010 [cited by applicant]
EP 2425024 · 2013 [cited by applicant]
EP 2247623 · 2014 [cited by applicant]
EP 2452014 · 2016 [cited by applicant]
EP 2817448 · 2016 [cited by applicant]
EP 3172267 · 2017 [cited by applicant]
EP 2678474 · 2017 [cited by applicant]
EP 3307950 · 2018 [cited by applicant]
EP 2632957 · 2018 [cited by applicant]
EP 2895653 · 2019 [cited by applicant]
GB 1562493 · 1980 [cited by applicant]
GB 2528495 · 2016 [cited by applicant]
GB 2560726 · 2018 [cited by applicant]
JP H11269788 · 1999 [cited by applicant]
JP 2006241380 · 2006 [cited by applicant]
JP 2009261215 · 2009 [cited by applicant]
JP 2011032388 · 2011 [cited by applicant]
JP 2013528715 · 2013 [cited by applicant]
JP 646399 · 2018 [cited by applicant]
WO WO0202871 · 2002 [cited by applicant]
WO WO2009008822 · 2009 [cited by applicant]
WO WO2010009343 · 2010 [cited by applicant]
WO WO2011138633 · 2011 [cited by applicant]
WO WO2013124265 · 2013 [cited by applicant]
WO WO2014089412 · 2014 [cited by applicant]
WO WO2016004482 · 2016 [cited by applicant]
WO WO2016012755 · 2016 [cited by applicant]
WO WO2016034727 · 2016 [cited by applicant]
WO WO2016193542 · 2016 [cited by applicant]
WO WO2017135816 · 2017 [cited by applicant]
WO WO2018073177 · 2018 [cited by applicant]
WO WO2018104330 · 2018 [cited by applicant]
WO WO2018146386 · 2018 [cited by applicant]
WO WO2018197756 · 2018 [cited by applicant]
WO WO2018197756A1 · 2018 [cited by examiner]
WO WO2020084412 · 2020 [cited by applicant]
Palme, A., Peterson, A. et al. Development of an efficient route for combined recycling of PET and cotton from mixed fabrics. Text Cloth Sustain 3, 4 (2017) (Year: 2017). [cited by examiner]
Agrupis, Shirley, et al., Industrial utilization of tobacco stalks II: preparation and characterization of tobacco pulp DY steam explosion pulping, The Japan Wood Research Society, 2000, 46, pp. 222-229. [cited by applicant]
EPO, Extended European Search Report in European Application No. 16808506.6-1101 dated Mar. 20, 2019. [cited by applicant]
International Search Report and Written Opinion for PCT Application No. PCT/US2019/013270 dated Apr. 29, 2019. [cited by applicant]
International Search Report and Written Opinion for PCT Application No. PCT/US2017/065334 dated Mar. 30, 2018. [cited by applicant]
Liguori, Rossana et al. “Bioreactors for lignocellulose conversion into fermentable sugars for product of high added value products”, Applied Microbiology and Biotechnology, Nov. 16, 2015 (online), pp. 597-611, vol. 100. [cited by applicant]
Palme, Anna, et al., Development of an efficient route for combined recycling of PET and cotton from mixed fabrics, Wextiles and Clothing Sustainability, 2017, vol. 3, No. 4, pp. 1-9. [cited by applicant]
PCT, International Preliminary Report on Patentability, International application No. PCT/SE2008/050837, Aug. 26 □009. [cited by applicant]
PCT, International Search Report and Written Opinion, International application No. PCT/US2016/037188 dated Sep. 12, 2016. [cited by applicant]
PCT, International Preliminary Report on Patentability, International application No. PCT/US2016/037188 dated Dec. 12, 2017. [cited by applicant]
Sohail, et al, Hydrothermal liquefaction of biomass: A review of subcritical water technologies, Energy, 36, 2011, pp. 2328-2342. [cited by applicant]
WIPO; International Preliminary Report on Patentability for International Patent Application No. PCT/US2019/013270 dated Jul. 23, 2020, 7 pages. [cited by applicant]