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 with hydrogen fluoride in gas phase in the presence of the fluorination catalyst, wherein the fluorination catalyst is a chromium-based catalyst further comprising a co-catalyst selected from the group consisting of Co, Ni, Zn, and Mn and mixtures thereof, said catalyst being supported on alumina, activated alumina or aluminum derivatives, and
ii. contacting a fluorination catalyst with an oxidizing agent-containing gas flow for at least one hour;
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; and
at least one regeneration stage comprising contacting the fluorination catalyst with an oxidizing agent-containing gas flow, wherein conversion percentage to the fluorinated compound is higher after the at least one regeneration stage than conversion percentage after the initial activation stage;
wherein the said chlorinated compound is selected from the group consisting of hydrochlorocarbons, hydrochlorofluorocarbons and hydrochlorofluoroolefins.
2. The process of claim 1 , wherein the oxidizing agent-containing gas flow of the activation stage and/or the at least one regeneration stage is 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 oxidizing agent-containing gas flow for at least 2 hours.
4. The process of claim 1 , wherein the oxidizing agent-containing gas flow of the activation stage and/or the at least one regeneration stage contains hydrogen fluoride in addition to the oxidizing agent, and wherein the proportion of oxidizing agent in the oxidizing agent-containing gas flow of the activation stage and/or the at least one regeneration stage is preferably from 2 to 98 mol %, relative to the total amount oxidizing agent and hydrogen fluoride.
5. The process of claim 1 , wherein the oxidizing agent-containing gas flow of the activation stage and/or the at least one regeneration stage does not contain hydrogen fluoride.
6. The process of claim 1 , wherein the oxidizing agent-containing gas flow of the activation stage and/or the at least one regeneration stage is 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 oxidizing agent-containing gas flow is contacted with the fluorination catalyst during the activation stage and/or the at least one regeneration stage 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 co-catalyst is present in an amount from about 1-10 wt % of said fluorination catalyst.
11. The process of claim 1 , wherein the fluorination catalyst is a mixed chromium/nickel catalyst.
12. The process of claim 1 , wherein the chlorinated compound is 2-chloro-3,3,3-trifluoro-1-propene.
13. The process of claim 1 , wherein the at least one reaction stage is carried out at a pressure of from 1 to 20 bars.
14. The process of claim 1 , wherein the at least one reaction stage is carried out at a temperature of from 200 to 450° C.
15. 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.
16. The process of claim 1 , wherein the at least one reaction stage is carried out in the presence of an oxidizing agent.