Reactor and agitator useful in a process for making 1-chloro-3,3,3-trifluoropropene
View Patent ↗Disclosed is a reactor and agitator useful in a high pressure process for making 1-chloro-3,3,3-trifluoropropene (1233zd) from the reaction of 1,1,1,3,3-pentachloropropane (240fa) and HF, wherein the agitator includes one or more of the following design improvements: (a) double mechanical seals with an inert barrier fluid or a single seal; (b) ceramics on the rotating faces of the seal; (c) ceramics on the static faces of seal; (d) wetted o-rings constructed of spring-energized Teflon and PTFE wedge or dynamic o-ring designs; and (e) wetted metal surfaces of the agitator constructed of a corrosion resistant alloy.
1. A process for the manufacture of 1233zd comprising the steps of:
(a) reacting 240fa and HF without a catalyst in an agitator stirred reactor, wherein the agitator comprises wetted metal surfaces and two spaced-apart sets of agitator blades mounted on an agitator shaft, wherein the wetted metal surfaces of the agitator comprise a corrosion resistant alloy selected from the group consisting of Alloy 020, the Hastelloy alloys and the Inconel alloys, and the reactor is operated at a pressure range of 350 psig to 450 psig and at a temperature range of from 90° C. to 145° C. to produce a product stream comprising 1233zd, HCl, HF, and other byproducts;
(b) distilling the product stream from step (a) into a first overhead product and a first bottoms product rich in HF;
(c) distilling the first overhead product from step (b) to form a second overhead product containing HCl and a second bottoms product containing organic components and HF;
(d) phase separating the second bottoms product from step (c) to separate the HF from the organic components; and
(e) scrubbing, drying, and distilling the organic components from step (d) to provide purified 1233zd.
2. The process of claim 1 , wherein the HF from step (b) is recycled to the reactor.
3. The process of claim 1 , wherein the HCl from step (c) is scrubbed with water and optionally recovered as an aqueous solution.
4. The process of claim 1 , wherein the HF from the phase separation in step (d) is recycled back to the reactor.
5. A process for the manufacture of 1233zd comprising the steps of:
(a) reacting 240fa and HF with a catalyst in an agitator stirred reactor, wherein the agitator comprises wetted metal surfaces and two spaced-apart sets of agitator blades mounted on an agitator shaft, wherein the wetted metal surfaces of the agitator comprise a corrosion resistant alloy selected from the group consisting of Alloy 020, the Hastelloy alloys and the Inconel alloys, and the reactor is operated at a pressure range of 350 psig to 450 psig and at a temperature range of from 90° C. to 145° C. to produce a product stream comprising 1233zd, HCl, HF, and other byproducts;
(b) distilling the product stream from step (a) into a first overhead product and a first bottoms product rich in HF;
(c) distilling the first overhead product from step (b) to form a second overhead product containing HCl and a second bottoms product containing organic components and HF;
(d) phase separating the second bottoms product from step (c) to separate the HF from the organic components; and
(e) scrubbing, drying, and distilling the organic components from step (d) to provide purified 1233zd.
6. The process of claim 5 , wherein the catalyst comprises one or more Lewis acid catalysts.
7. The process of claim 6 , wherein the Lewis Acid catalyst is selected from the group consisting of TiCl 4 , SbCl 5 , and mixtures thereof.
8. The process of claim 7 , wherein the catalyst is TiCl 4 .