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ChemicalBook CAS DataBase List Perfluoro-1-iodohexane
355-43-1

Perfluoro-1-iodohexane synthesis

8synthesis methods
To an autoclave (stainless steel, volume:1L) equipped with a mixing tank and a stirrer, C4F9I which compound (1) flow rate 25mL/min, CF2=CF2 (tetrafluoroethylene) which compound (2) flow rate 0.37g/min, (C2F5COO)2 (10 and half hour life temperature: 31°C) which compound (4) flow rate 0.052 mmol/min were supplied, the mixture was prepared by mixing at stirrer. Temperature in the autoclave was 10°C, residence time of the mixture in the autoclave was 10 minutes. The molar ratio (C4F9I/CF2=CF2)of C4F9I and CF2=CF2 in the mixed solution was 41, the amount of (C2F5COO)2 with respect to C4F9I was 0.034 mol%. Only the mixture from the bottom of the autoclave was withdrawn in the absence of gas phase, the mixture was fed to the bottom of tubular reactor (Tankan-shiki, volume: 0.5L). The mixture was not seperated by gas-liquid separation, the mixture was flow towards the outlet from the inlet of the reaction tube in the tube reactor. The temperature of the reaction tube, and a 70°C, the residence time of the mixture in the tubular reactor was set to 20 minutes. The mixture containing a compound Perfluoro-1-iodohexane C6F13I was obtained.
synthesis of Perfluoro-1-iodohexane
-

Yield:-

Reaction Conditions:

with bis(pentafluoropropionyl)peroxide at 28 - 70; for 0.333333 h;Concentration;Temperature;Time;

Steps:

1

Into an autoclave 1 (made of stainless steel, capacity: 1 L) having a stirrer, C4F9I as the compound (1) was supplied at a flow rate of 25 mL/min, CF2=CF2 (tetrafluoroethylene) was supplied at a flow rate of 0.10 g/min, and (C2F5COO)2 (10 hour half-life temperature: 28°C) was supplied at a flow rate of 0.0065 mmol/min, and they were mixed by the stirrer to prepare a mixed solution. The temperature in the autoclave was set to be 70°C, and the retention time of the mixed solution in the autoclave was set to be 20 minutes. The obtained reaction mixture (1) contained C6F13I as the compound (2). The amounts of tetrafluoroethylene and (C2F5COO)2 were 0.65 mol% and 0.00425 mol%, respectively, to C4F9I.[0071] From the bottom of the autoclave 1, the reaction mixture (1) was withdrawn and supplied into an autoclave 2 (made of stainless steel, capacity: 1 L) having a stirrer, at a flow rate of 25 mL/min, CF2=CF2 (tetrafluoroethylene) was supplied at a flow rate of 0.10 g/min, and (C2F5COO)2 (10 hour half-life temperature: 28°C) was supplied at a flow rate of 0.0065 mmol/min, and they were mixed by the stirrer to prepare a mixed solution. The temperature in the autoclave was set to be 70°C, and the retention time of the mixed solution in the autoclave was set to be 20 minutes to obtain a reaction mixture (2) containing C6F13I as the compound (2). The amounts of tetrafluoroethylene and (C2F5COO)2 supplied, were 0.65 mol% and 0.00425 mol%, respectively, to the total of telomers in the mixed solution.[0072] From the bottom of the autoclave 2, the reaction mixture (2) was withdrawn, and an analysis of the composition was carried out to obtain the C4F9I conversion and C8+/C6 (%). The results are shown in Table 1.

References:

EP2578560,2013,A1 Location in patent:Paragraph 0070; 0071; 0072

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