Upcycling perfluoropolymers into fluorinated olefins

Patent metadata

Field	Value
Publication number	US-11795126-B2
Application number	US-202117904611-A
Country	US
Kind code	B2
Filing date	Feb 19, 2021
Priority date	Feb 21, 2020
Publication date	Oct 24, 2023
Grant date	Oct 24, 2023

Abstract

Mechanical stirred bed reactors that incorporate a screen are described. Methods of using such reactors to process perfluoropolymers to form perfluorinated olefin monomers are also described. The reactors and methods may be used to upcycle filled perfluorinated materials.

First claim

What is claimed is:

1. A method of converting a filled perfluoropolymer into perfluorinated olefins comprising:
a) feeding a perfluoropolymer containing an inorganic filler into a reaction chamber of a mechanical stirred bed reactor comprising
i) a bottom wall, a side wall connected to and extending from the bottom wall to a top of the side wall;
ii) a screen comprising a plurality of openings extending through the screen from an opening entrance at the top side of the screen to an opening exit on the bottom side of the screen, wherein the screen is supported above the bottom wall and the reaction chamber has a total reaction volume bounded by the side wall and extending from the screen to the top of the side wall;
iii) a bed of beads supported by the screen and filling at least 20% of the total reaction volume; and
iv) an agitator comprising a screw thread surrounding an agitator shaft;

b) agitating at least 80 wt. % of the beads with the agitator while heating the perfluoropolymer to a temperature of at least 450° C. and passing a carrier gas through the beads;
c) decomposing the perfluoropolymer to form perfluorinated olefin monomers and releasing the filler; and
d) collecting the perfluorinated olefin monomers and the fillers below the screen;

wherein at least 95 wt. % of the filler has a maximum dimension of no greater than DF95, wherein no greater than 5 wt. % of beads have a maximum dimension of less than DB5; and wherein the minimum dimension of the openings in the screen on the side of the screen supporting the beads is Dmin; further wherein the ratio of Dmin over DF95 is at least 5, and the ratio of DB5 over Dmin is at least 1.5.

2. The method of claim 1 , wherein the inorganic filler comprises inorganic fibers.

3. The method of claim 1 , wherein the carrier gas comprises superheated steam.

4. The method of claim 1 , wherein the ratio of Dmin over DF95 ranges from 10 to 100, inclusive.

5. The method of claim 4 , wherein the ratio of DB5 over Dmin ranges from 3 to 10, inclusive.

6. The method of claim 1 , wherein the beads comprise a ceramic.

7. The method of claim 1 , wherein the beads comprise carbon.

8. The method of claim 1 , wherein the beads are spheroidal and have a density of less than 6 grams per cubic centimeter and a thermal conductivity of at least 3 W/mK.

9. The method of claim 8 , wherein the beads have an average density of 1.5 to 4 grams per cubic centimeter.

10. The method of claim 8 , wherein the beads have an average thermal conductivity of 50 to 300 W/mK.

11. The method of claim 8 , wherein the beads have a heat capacity of 300 to 1500 J/kg·K.

12. The method of claim 1 , wherein the reactor further comprises microwave active material mixed with the beads and a source of microwave energy.

Assignees

• 3M Innovative Properties Company

Inventors

• Hirschberg Markus E
• Hintzer Klaus
• Kolbeck Thomas G
• Wieland Matthias
• Bauer Peter
• Schmidt-Rodenkirchen Achim
• Gerdes Thorsten

Classifications

• C07C17/367 Primary

  by depolymerisation · CPC title

• B01J8/085

  Feeding reactive fluids (for solid material, see B01J8/0015) · CPC title

• B01J8/10

  moved by stirrers or by rotary drums or rotary receptacles {or endless belts} · CPC title

• C08J11/14

  by treatment with steam or water · CPC title

• C10B53/07

  {of solid raw materials consisting} of synthetic polymeric materials, e.g. tyres (recovery or working-up of waste materials of organic macromolecular compounds or compositions based thereon by dry-heat treatment for obtaining partially depolymerised materials C08J11/10; production of liquid hydrocarbon mixtures from rubber or rubber waste C10G1/10) · CPC title