IP Library Granted Patent US 12,492,296
Granted Patent B2
US 12,492,296 · App. 17/786,101 · Granted Dec 9, 2025

Method for obtaining a purified diester effluent by depolymerising a polyester comprising opaque polyethylene terephthalate

Inventors: David Chiche (Rueil-Malmaison, FR); Damien Leinekugel Le Cocq (Rueil-Malmaison, FR); Christine Bounie (Rueil-Malmaison, FR)
Assignee: IFP ENERGIES NOUVELLES
C08J11/24C07C67/03C07C67/56C02F1/285C08J2367/02
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Quick Facts
Patent No.
US 12,492,296
App. No.
17/786,101
Granted
Dec 9, 2025
Kind
B2
Abstract

The present invention relates to a process for depolymerizing a polyester feedstock comprising opaque PET, which comprises: a) a conditioning step; b) a step of glycolysis, operated at between 180 and 400° C., a residence time of from 0.1 to 10 h in the presence of diol; c) a diol separation step, at a temperature of between 100 and 250° C., a pressure lower than that of step b) and producing a diol effluent and an effluent rich in monomers; d) a step of separating into a heavy impurities effluent and a prepurified monomers effluent, at a temperature of less than 250° C. and a pressure of less than 0.001 MPa and a residence time of less than 10 min; e) a step of decolourizing the prepurified monomers effluent, by adsorption of a mixture comprising between 20% and 90% by weight of the prepurified monomers effluent and a solvent, at a temperature of between 100 and 200° C., a pressure of between 0.1 and 1.0 MPa and in the presence of at least one adsorbent.

Claims (28)

1 . A process for depolymerizing a polyester feedstock comprising opaque polyethylene terephthalate (PET), said process comprising:

a) a conditioning step comprising a conditioning section supplied at least with said polyester feedstock, to produce a conditioned stream;

b) a step of depolymerization by glycolysis, which is supplied at least with the conditioned stream and with a supplement of diol so that the molar amount of diol is adjusted to between 1 to 20 moles of diol per mole of diester in said polyester feedstock, conducted at a temperature of between 18° and 400° C. and for a residence time of between 0.1 and 10 h;

c) a diol separation step, which is supplied at least with the effluent from step b), and is conducted at a temperature of between 10° and 250° C., at a pressure less than that of step b), and which produces a diol effluent and a liquid effluent rich in monomers, wherein said diol separation step is implemented in two to five successive gas-liquid separation sections, each producing a gaseous effluent and a liquid effluent, wherein the liquid effluent from the preceding section supplies the subsequent section, a liquid effluent obtained from a last gas-liquid separation section forms the liquid effluent rich in monomers, and all the gaseous effluents are recovered to form the diol effluent;

d) a step of separation of the liquid effluent rich in monomers obtained from step c) into a heavy impurities effluent and a prepurified monomers effluent, which is conducted at a temperature of less than 250° C. and a pressure of less than 0.001 MPa with a liquid residence time of less than 10 min, and

e) a step for decolorizing the prepurified monomers effluent, comprising at least a mixing section for mixing the prepurified monomers effluent obtained in step d) with a solvent to form a mixture wherein the prepurified monomers effluent represents between 20% and 90% by weight of the total weight of the mixture, and an adsorption section conducted at a temperature of between 10° and 200° C. and at a pressure of between 0.1 and 1.0 MPa in the presence of at least one adsorbent selected from activated carbons, alumina and clays, to obtain a purified monomers effluent.

2 . The process according to claim 1 , wherein said polyester feedstock comprises at least 50% by weight of polyethylene terephthalate.

3 . The process according to claim 1 , wherein said polyester feedstock comprises at least 10% by weight of opaque PET.

4 . The process according to claim 1 , wherein said polyester feedstock comprises colored PET.

5 . The process according to claim 1 , wherein said polyester feedstock comprises between 0.1% and 10% by weight of pigments.

6 . The process according to claim 1 , wherein said polyester feedstock comprises between 0.05% and 1% by weight of dyes.

7 . The process according to claim 1 , wherein the solvent in decolorizing step e) comprises a fraction of the diol effluent obtained from step c), a supplement of diol external to the process, or mixtures thereof.

8 . The process according to claim 1 , wherein the prepurified monomers effluent represents between 30% and 80% by weight of the total weight of the mixture in step e).

9 . The process according to claim 1 , wherein at least one adsorbent in step e) is an activated carbon.

10 . The process according to claim 1 , wherein the adsorption section in step e) is operated in the presence of an adsorbent or two different adsorbents.

11 . The process according to claim 1 , wherein the adsorption section comprises two or more different adsorbents, said different adsorbents being in a mixture or placed in series in said adsorption section.

12 . The process according to claim 11 , wherein each of said different adsorbents are in different reactors placed in series.

13 . The process according to claim 1 , wherein the adsorption section of step e) is implemented in fixed bed adsorption mode.

14 . The process according to claim 1 , wherein the adsorption section of step e) is operated at a temperature of between 10° and 170° C.

15 . The process according to claim 1 , wherein said polyester feedstock comprises at least 70% by weight of polyethylene terephthalate.

16 . The process according to claim 1 , wherein said polyester feedstock comprises at least 90% by weight of polyethylene terephthalate.

17 . The process according to claim 1 , wherein said polyester feedstock comprises at least 15% by weight of opaque PET.

18 . The process according to claim 1 , wherein said polyester feedstock comprises between 0.1% and 5% by weight of pigments.

19 . The process according to claim 1 , wherein the prepurified monomers effluent represents between 50% and 75% by weight, of the total weight of the mixture in step e).

20 . The process according to claim 1 , wherein the adsorption section of step e) is operated at a temperature of between 120° C. and 150° C.

21 . The process according to claim 1 , wherein said polyester feedstock comprises 0.05% and 0.2% by weight of dyes.

22 . Process according to claim 1 , wherein the mixing section employs a static or dynamic mixer, and the residence time of the mixture in the mixing section is between 0.5 second and 20 minutes.

23 . Process according to claim 22 , wherein the mixture from the mixing section supplies the adsorption section which contains at least one adsorber, wherein the adsorption section is operated at a temperature of between 10° and 200° C. and a pressure of between 0.1 and 1.0 MPa, and the residence time of the mixture in each adsorber of the adsorption section is between 20 minutes and 40 hours.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 15, 2022
From: CHICHE, DAVID; LEINEKUGEL LE COCQ, DAMIEN; BOUNIE, CHRISTINE
To: IFP ENERGIES NOUVELLES
Reel/Frame 060674/0213 →
Priority Claims (1)
FR 1914992 · Dec 19, 2019 · national
Continuity (1)
Related Publication 20230028123A1 · Jan 26, 2023
References Cited (9)
US 4502957A · Jehle · 1985 [cited by examiner]
US 6642350B1 · Asakawa et al. · 2003 [cited by applicant]
US 10544276B2 · Charra et al. · 2020 [cited by applicant]
US 20060074136A1 · Smith et al. · 2006 [cited by applicant]
US 20150105532A1 · Allen et al. · 2015 [cited by applicant]
US 20190161595A1 · Charra · 2019 [cited by examiner]
EP 0080434B1 · 1986 [cited by applicant]
WO 2018007356A1 · 2018 [cited by applicant]
International Search Report PCT/EP2020/084851 dated Apr. 1, 2021 (pp. 1-2). [cited by applicant]