Process for producing 2,3,3,3-tetrafluoropropene
View Patent ↗The present invention relates, in part, to the discovery that the presence of impurities in a reactor for dehydrochlorinating HCFC-244bb to HFO-1234yf results in selectivity changeover from HFO-1234yf to HCFO-1233xf. By substantially removing such impurities, it is shown that the selectivity to HFO-1234yf via dehydrochlorination of HCFC-244bb is improved.
1. A process for removing impurities from a reactor comprising an inner metal alloy surface such that the reactor is substantially free of impurities comprising the steps of:
(a) purging the reactor with an inert gas;
(b) optionally, oxidizing the impurities in the reactor by introducing an oxidizing agent into the reactor under conditions effective to oxidize the impurities;
(c) reducing the impurities in the reactor by introducing a reducing agent into the reactor under conditions effective to reduce the impurities;
(d) cooling the reactor to an ambient temperature while passing the reducing agent and/or inert gas through the reactor; and
(e) maintaining a positive pressure in the reactor with the reducing agent and/or the inert gas.
2. The process of claim 1 , wherein the impurities in the reactor are selected from the group consisting of metal halides, metal oxides, and carbonaceous materials.
3. The process of claim 2 , wherein the metal halides comprise halides of Ni, Cr, Fe, Mo, Nb, Cu, or Co.
4. The process of claim 1 , wherein the inert gas introduced into the reactor in the purging step comprises a gas selected from the group consisting of He, Ar, N 2 , and combinations of these.
5. The process of claim 4 , wherein the inert gas is N 2 .
6. The process of claim 4 , wherein the purging step is carried out at a temperature of from about 100° C. to about 700° C.
7. The process of claim 4 , wherein the purging step is carried out at a temperature of from about 200° C. to about 600° C.
8. The process of claim 4 , wherein the purging step is carried out at a temperature of from about 300° C. to about 500° C.
9. The process of claim 4 , wherein the purging step is carried out at a temperature of from about 400° C. to about 500° C.
10. The process of claim 2 , wherein the oxidizing agent is introduced into the reactor under conditions effective to burn off the carbonaceous materials in the reactor.
11. The process of claim 10 , wherein the oxidizing agent introduced into the reactor in the oxidizing step comprises a gas selected from the group consisting of H 2 O, CO 2 , O 2 , air, O 3 , Cl 2 , N 2 O, and combinations of these.
12. The process of claim 11 , wherein the oxidizing gas comprises is air.
13. The process of claim 11 , wherein the oxidizing step is carried out at a temperature of from about 100° C. to about 700° C.
14. The process of claim 11 , wherein the oxidizing step is carried out at a temperature of from about 200° C. to about 600° C.
15. The process of claim 11 , wherein the oxidizing step is carried out at a temperature of from about 400° C. to about 500° C.
16. The process of claim 2 , wherein the reducing agent is introduced into the reactor under conditions effective to convert any metal halides or metal oxides into metallic metals.
17. The process of claim 16 , wherein the reducing agent introduced into the reactor in the reducing step comprises a gas selected from the group consisting of H 2 , NH 3 , and C 1 -C 12 hydrocarbons.
18. The process of claim 17 , wherein the reducing gas is H 2 .
19. The process of claim 17 , wherein the reducing step is carried out at a temperature of from about 100° C. to about 700° C.
20. The process of claim 17 , wherein the reducing step is carried out at a temperature of from about 200° C. to about 600° C.
21. The process of claim 17 , wherein the reducing step is carried out at a temperature of from about 400° C. to about 500° C.
22. A process for preparing 2,3,3,3-tetrafluoropropene comprising:
(a) removing impurities from a reactor such that the reactor is substantially free of impurities comprising the steps of:
(i) purging the reactor with an inert gas;
(ii) optionally, oxidizing the impurities in the reactor by passing an oxidizing agent through the reactor at a temperature that is sufficiently high to oxidize the impurities;
(iii) reducing the impurities in the reactor by passing a reducing agent through the reactor at a temperature that is sufficiently high to reduce the impurities;
(iv) cooling the reactor to an ambient temperature while passing the reducing agent and/or inert gas through the reactor; and
(v) maintaining a positive pressure in the reactor with the reducing agent and/or the inert gas;
(b) providing a starting composition comprising 2-chloro-1,1,1,2-tetrafluoropropane in the reactor; and
(c) contacting the starting composition in the reactor under conditions effective to produce a final composition comprising 2,3,3,3-tetrafluoropropene.