2-CHLORO-1,1,1,3,3,3-HEXAFLUOROPROPANE synthesis

15synthesis methods

Product Name:2-CHLORO-1,1,1,3,3,3-HEXAFLUOROPROPANE
CAS Number:431-87-8
Molecular formula:C3HClF6
Molecular Weight:186.48

431-52-7
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431-87-8
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Yield:431-87-8 93.7 %Chromat.

Reaction Conditions:

with hydrogen fluoride;copper-substituted α-chromium oxide (99% chromium/1% copper) treated with HF at 320; under 760.051 Torr; for 0.00138889 h;Product distribution / selectivity;Inert atmosphere;Monel nickel alloy tube packed with Monel turnings;

Steps:

2

General Procedure for Fluorination and ChlorofluorinationA weighed quantity of pelletized catalyst was placed in a inch (1.58 cm) diameter Inconel nickel alloy reactor tube heated in a fluidized sand bath: The tube was heated from 50° C. to 175° C. in a flow of nitrogen (50 cc/min; 8.3(10)^-7m³/sec) over the course of about one hour. HF was then admitted to the reactor at a flow rate of 50 cc/min (8.3(10)^-7m³/sec). After 0.5 to 2 hours the nitrogen flow was decreased to 20 cc/min (3.3(10)^-7m³/sec) and the HF flow increased to 80 cc/min (1.3(10)^-6m³/sec); this flow was maintained for about 1 hour. The reactor temperature was then gradually increased to 400° C. over 3 to 5 hours. At the end of this period, the HF flow was stopped and the reactor cooled to 300° C. under 20 sccm (3.3(10)^-7m³/sec) nitrogen flow. CFC-1213xa was fed from a pump to a vaporizer maintained at about 118° C. For fluorinations, the CFC-1213xa vapor was combined with the appropriate molar ratios of HF in a 0.5 inch (1.27 cm) diameter Monel nickel alloy tube packed with Monel turnings. The mixture of reactants then entered the reactor. The HF/1213xa molar ratio was 20 and the contact time was 5 seconds for Examples 1-7. For chlorofluorinations, the CFC-1213xa vapor was combined with the appropriate molar ratios of HF and chlorine. The HF/1213xa/chlorine molar ratio was 20/1/4 for all runs and the contact time was 5 seconds for Examples 8-14 and 30 seconds for Examples 15-16. The reactions were conducted at a nominal pressure of one atmosphere. Analytical data for identified compounds is given in units of GC area %. Small quantities of other unidentified products were present.Examples 1-7Fluorination of 1213xaThe fluorination of CFC-1213xa was carried out at various temperatures using catalysts prepared according to Catalyst Preparation Examples 1-7. The analytical results are shown in Table 1.