Process for purifying (hydro)fluoropropenes contaminated with halogenated ethane

Patent metadata

Field	Value
Publication number	US-11007471-B2
Application number	US-201916588802-A
Country	US
Kind code	B2
Filing date	Sep 30, 2019
Priority date	Jun 9, 2014
Publication date	May 18, 2021
Grant date	May 18, 2021

Abstract

A process for treating a composition comprising one or more desired (hydro)fluoroolefins and one or more undesired halogenated ethanes, halogenated methanes or mixtures thereof so as to reduce the concentration of at least one undesired halogenated ethane or halogenated methane, the process comprising contacting the composition with an adsorbent comprising pores having openings which have a size across their largest dimension of about 6 Å or less.

First claim

The invention claimed is:

1. A process of purifying a tetrafluoropropene composition comprising:
contacting a composition with an adsorbent, the composition comprising at least one tetrafluoropropene and an impurity comprising a halogenated ethane, the adsorbent comprising pores having openings which have a size across their largest dimension of about 6 Å or less, so as to remove at least a portion of the halogenated ethane from the composition.

2. The process according to claim 1 wherein the at least one tetrafluoropropene comprises at least 10 wt % of the composition to be treated.

3. The process according to claim 1 wherein the adsorbent comprises pores having openings which have a size across their largest dimension of from about 4 Å to about 6 Å.

4. The process according to claim 1 wherein the adsorbent is a molecular sieve.

5. The process according to claim 1 wherein the adsorbent comprises a zeolite.

6. The process according to claim 1 wherein the tetrafluoropropene is 2,3,3,3-tetrafluoropropene (1234yf).

7. The process according to claim 1 wherein the halogenated ethane is a fluorinated ethane.

8. The process according to claim 7 wherein the fluorinated ethane is tetrafluoroethane.

9. The process according to claim 8 wherein the tetrafluoroethane is 1,1,1,2-tetrafluoroethane (134a).

10. The process according to claim 1 wherein the contacting step is performed, at least in part, at a temperature of from about 0° C. to about 200° C.

11. The process according to claim 1 wherein the contacting step is conducted at a pressure of from about 0.1 MPa to the saturation pressure.

12. The process according to claim 11 wherein the adsorbent treatment step comprises an exposure step comprising exposing the adsorbent to one or more inert gases.

13. The process according to claim 1 further comprising an adsorbent treatment step prior to the contacting step.

14. The process according to claim 13 wherein the adsorbent treatment step comprises a heat treatment step comprising heating the adsorbent to a maximum temperature of at least 150° C.

15. The process according to claim 14 wherein the heat treatment step comprises heating the adsorbent to the maximum temperature at a rate of from 1° C./minute to 100° C./minute.

16. The process according to claim 14 wherein the heat treatment step comprises maintaining the adsorbent at or around the maximum temperature for a time of from 1 second to 1 hour.

17. The process according to claim 1 wherein the process removes at least 50% by weight of the halogenated ethane.

18. The process according to claim 17 wherein the process reduces the concentration of the halogenated ethane to levels at, around or below the limit of detection by gas chromatography.

19. The process according to claim 1 wherein the adsorbent is dried before use.

20. The process according to claim 1 further comprising a step of regenerating the adsorbent after it has been contacted with the composition.

21. The process according to claim 20 wherein the regenerating step comprises contacting the adsorbent with a heated stream of inert gas and/or heating the adsorbent whilst the or an inert gas is passed over it.

22. The process according to claim 20 wherein the regenerating step comprises subjecting the adsorbent to a change in pressure.

23. The process according to claim 1 further comprising one or more additional purifying steps, which may be conducted before and/or after the contacting step.

24. The process according to claim 1 which is carried out, at least in part, in the gas or liquid phase.

25. A process for treating a composition comprising one or more desired tetrafluoropropenes and one or more undesired halogenated ethanes, so as to reduce the concentration of at least one undesired halogenated ethane, the process comprising contacting the composition with an adsorbent comprising pores having openings which have a size across their largest dimension of about 6 Å or less, wherein the moisture content of the adsorbent is less than about 1.5% by weight.

26. A method for recovering a desired component of a spent refrigerant, the method comprising removing a spent refrigerant comprising a desired component and an undesired component from a refrigerant system and contacting the spent refrigerant with an adsorbent comprising pores having a size opening across their largest dimension of 6 Å or less to remove or reduce the concentration of one or more undesired components, the desired component comprising a tetrafluoropropene, the undesired component comprising a halogenated ethane.

27. The method according to claim 26 wherein the tetrafluoropropene comprises at least 10 wt % of the spent refrigerant.

28. A kit for recovering a desired component of a spent refrigerant, the kit comprising an apparatus comprising an adsorbent comprising pores having a size opening across their largest dimension of 6 Å or less and instructions for removing a spent refrigerant comprising a desired component and an undesired component from a refrigerant system and contacting the spent refrigerant with the apparatus to remove or reduce the concentration of one or more undesired components, the desired component comprising a tetrafluoropropene, the undesired component comprising a halogenated ethane.

Assignees

• Mexichem Fluor Sa De Cv

Inventors

• Sharratt Andrew
• Low Robert

Classifications

• F25B43/003

  Filters · CPC title

• C09K2205/126

  Unsaturated fluorinated hydrocarbons · CPC title

• C09K5/045

  containing only fluorine as halogen · CPC title

• C07C17/389 Primary

  by adsorption on solids · CPC title

• B01D2259/402

  using two beds · CPC title