Catalytic gas phase fluorination
View Patent ↗The present invention relates to a fluorination process, comprising: an activation stage comprising contacting a fluorination catalyst with an oxidizing agent-containing gas flow for at least one hour; and at least one reaction stage comprising reacting a chlorinated compound with hydrogen fluoride in gas phase in the presence of the fluorination catalyst, so as to produce a fluorinated compound.
1. A fluorination process, comprising:
an activation stage comprising the following steps, in succession:
i. reacting a chlorinated compound selected from the group consisting of 2-chloro-3,3,3-trifluoro-1-propene, 1,1,1,2,3-pentachloropropane, 1,1,2,2,3-pentachloropropane, 2,3-dichloro-1,1,1-trifluoropropane, 2,3,3,3-tetrachloro-1-propene and 1,1,2,3-tetrachloro-1-propene with hydrogen fluoride in gas phase in the presence of a chromium-based fluorination catalyst, and
ii. contacting the chromium-based fluorination catalyst with a first oxidizing agent-containing gas flow comprising an oxidizing agent and hydrogen fluoride;
at least one reaction stage comprising reacting the chlorinated compound with hydrogen fluoride in gas phase in the presence of the fluorination catalyst, so as to produce a fluorinated compound; and
at least one regeneration stage comprising contacting the fluorination catalyst with a second oxidizing agent-containing gas flow.
2. The process of claim 1 , wherein the first and/or second oxidizing agent-containing gas flows comprise an oxygen-containing gas flow.
3. The process of claim 1 , wherein the activation stage and/or the at least one regeneration stage comprise contacting the fluorination catalyst with the first and/or second oxidizing agent-containing gas flows for at least 2 hours.
4. The process of claim 1 , wherein the second oxidizing agent-containing gas flow contains hydrogen fluoride in addition to the oxidizing agent, and wherein the proportion of oxidizing agent in the second oxidizing agent-containing gas flow is from 2 to 98 mol %, relative to the total amount oxidizing agent and hydrogen fluoride.
5. The process of claim 1 , wherein the second oxidizing agent-containing gas flow does not contain hydrogen fluoride.
6. The process of claim 1 , wherein the first and/or second oxidizing agent-containing gas flow comprise air.
7. The process of claim 1 , wherein the activation stage and/or the at least one regeneration stage comprise contacting the fluorination catalyst with a hydrogen fluoride gas flow, either:
before contacting the fluorination catalyst with the oxidizing agent-containing gas flow; or
after contacting the fluorination catalyst with the oxidizing agent-containing gas flow.
8. The process of claim 1 , wherein the first and/or second oxidizing agent-containing gas flow is/are contacted with the fluorination catalyst at a temperature of from 250 to 500° C.
9. The process of claim 1 , wherein the fluorinated compound is a fluoroolefin.
10. The process of claim 1 , wherein the fluorination catalyst is a supported catalyst.
11. The process of claim 1 , wherein the fluorination catalyst is an unsupported catalyst.
12. The process of claim 1 , wherein the fluorination catalyst further comprises a co-catalyst selected from the group consisting of Co, Zn, Mn, Mg, V, Mo, Te, Nb, Sb, Ta, P, Ni and mixtures thereof.
13. The process of claim 12 , wherein the co-catalyst is present in an amount from about 1-10 wt % of said fluorination catalyst.
14. The process of claim 1 , wherein the fluorination catalyst is a mixed chromium/nickel catalyst.
15. The process of claim 1 , wherein the chlorinated compound is 2-chloro-3,3,3-trifluoro-1-propene.
16. The process of claim 1 , wherein the at least one reaction stage is carried out at a pressure of from 1 to 20 bars.
17. The process of claim 1 , wherein the at least one reaction stage is carried out at a temperature of from 200 to 450° C.
18. The process of claim 1 , wherein the contact time between hydrogen fluoride and the chlorinated compound during the at least one reaction stage is from 6 to 100 s.
19. The process of claim 1 , wherein the at least one reaction stage is carried out in the presence of an oxidizing agent.