Metallic copper catalyst for polyfluoroalkylethyl iodide production and process for producing polyfluoroalkylethyl iodide
A technology of polyfluoroalkylethyl and polyfluoroalkyl, applied in the field of manufacturing polyfluoroalkylethyl iodide
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Embodiment 1
[0104] Embodiment 1 (ethylene addition reaction)
[0105] Add perfluoroethyl iodide (CF 3 CF2 1) 138.6 g, 8.21 g of copper powder (average particle diameter 45 μm, manufactured by Mitsui Kinzoku Co., Ltd.), degassed, heated to 80° C., introduced ethylene, and made the autoclave internal pressure 1.0 MPa. When perfluoroethyl iodide is consumed, the pressure decreases and the partial pressure of ethylene in the gas phase increases, so ethylene is introduced while paying attention to the pressure of ethylene, and the internal pressure is kept at the above-mentioned pressure. The time point when the pressure drop of ethylene was not observed was set as the end point of the reaction. The reaction time was 80 minutes. After cooling the reaction mixture, the product was analyzed by gas chromatography.
[0106] The conversion rate of perfluoroethyl iodide was 99.5%, and the selectivity of the produced ethylene adduct (ethylene one-molecule adduct) was 99.8%.
[0107]
[0108] ...
Embodiment 2-6
[0119] Embodiment 2-6 (ethylene addition reaction)
[0120] Instead of perfluoroethyl iodide, use 1-iodoperfluorooctane (n-C 8 f 17 Except for 1), the others were processed in the same manner as in Example 1.
[0121] After cooling the reaction mixture, the product was analyzed by gas chromatography. The results are shown in Table 1.
Embodiment 7
[0129] Embodiment 7 (telomerization-ethylene addition reaction)
[0130] (1) Add 1-iodoperfluorobutane (n-C 4 h 9 I) 100 g and 4 g of copper powder (325 mesh, manufactured by Kishida Chemical Co., Ltd.), heated to 110° C. Tetrafluoroethylene was introduced into the reactor at the same temperature, and the pressure was increased to 0.38 MPa. As the reaction progressed, tetrafluoroethylene was consumed, so the internal pressure was checked, and tetrafluoroethylene was continuously introduced to maintain the above-mentioned pressure. After introducing a total of 18 g of tetrafluoroethylene, the reaction was stopped.
[0131] An analysis sample of the reaction mixture was taken out from the reaction vessel, and the product was analyzed by gas chromatography. The results are shown in Table 2. The conversion rate at this time was 40.0%.
[0132] Product distribution: CF 3 CF 2 CF 2 CF 2 (CF 2 CF 2 ) n -I
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