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One-step preparation method of perfluoroalkyl iodide

A technology of perfluoroalkyl iodide and one-step method is applied in the field of preparing perfluoroalkyl iodide by one-step method to achieve the effects of reducing production investment, simplifying production process and equipment, and improving reaction effect.

Inactive Publication Date: 2011-11-16
山东中氟化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This requires the use of two sets of reaction equipment and two sets of rectification equipment for synthesis, which increases the production process steps, increases equipment investment, and increases production costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] In a 2L stainless steel 316L pressure-resistant reactor, add 762g (3mol) of elemental iodine, 333g (1.5mol) of iodine pentafluoride, 11g of antimony pentafluoride, and 11g of titanium-nickel alloy powder (titanium / nickel=30 / 70) . The inside of the reaction kettle was evacuated to -0.095MPa, and the high-purity nitrogen was replaced for several times, so that the water content in the kettle was less than or equal to 100ppm, and the oxygen content was less than or equal to 30ppm. Start stirring, heat up to 60°C, add tetrafluoroethylene in stages, keep the pressure in the kettle at 0.5~0.7MPa, and add 15~40g each time. When the pressure no longer dropped after the tetrafluoroethylene was introduced, the reaction temperature was raised to 130°C, and the tetrafluoroethylene pressure was raised to 2.8MPa. When the whole reaction continued for 12 hours, a total of 1050g (10.5mol) of tetrafluoroethylene was added to stop the reaction, the temperature was lowered to -5°C, the r...

Embodiment 2

[0040] The amount and parameters of each raw material are the same as in Example 1, except that the total reaction time is extended to 16 hours, and 1360 g (13.6 mol) of tetrafluoroethylene are added. After rectifying C2 and C4, vacuum distillation is performed to obtain long-chain perfluoroethylene. Alkyl iodide mixture 425g. The test results of each component content are shown in Table 3.

[0041] Table 3 Contents of perfluoroalkyl iodine components

[0042] number of carbon atoms ≤C4 C6 C8 C10 C12 ≥C14 content(%) 1.1 38.2 27.7 16.9 8.5 6.6

Embodiment 3

[0044] In a 10L stainless steel 316L pressure-resistant reactor, add 3810g (15mol) of elemental iodine, 1665g (7.5mol) of iodine pentafluoride, 73g of antimony pentafluoride, and 110g of titanium-nickel alloy (titanium / nickel=30 / 70). Evacuate to -0.095MPa, and replace it with high-purity nitrogen for several times, so that the water content in the kettle is less than or equal to 100ppm and the oxygen content is less than or equal to 30ppm. Start stirring, heat up to 80°C, add tetrafluoroethylene in stages, keep the pressure in the kettle at 0.5~0.7Mpa, and add 15~40g each time. When the pressure no longer drops after the tetrafluoroethylene is introduced, the reaction temperature is raised to 150° C., and the tetrafluoroethylene pressure is raised to 2.8 MPa to continue the reaction. After 12 hours, a total of 5088 g (50.88 mol) of tetrafluoroethylene was added, the reaction was stopped, the temperature was lowered to -5°C, the reaction material was released, washed with KOH s...

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PUM

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Abstract

The invention relates to a one-step preparation method of perfluoroalkyl iodide, belonging to the field of fluoride product intermediates. The preparation method comprises the following steps: adding iodine, iodine pentafluoride and a composite catalyst into a reaction vessel, vacuumizing to -0.095 MPa, replacing air in the reaction vessel with high-purity nitrogen gas for times until the water content is not more than 100 ppm and the oxygen content is not more than 30 ppm, heating the reaction vessel until the internal temperature is 60-80 DEG C, adding tetrafluoroethylene, and maintaining the pressure at 0.5-0.7 MPa for reaction; and raising the reaction temperature to 130-150 DEG C when the pressure does not decrease after adding tetrafluoroethylene, continuing introducing tetrafluoroethylene, and controlling the pressure at 2.8 MPa for reaction to obtain the perfluoroalkyl iodide. In the preparation method, the perfluoroalkyl iodide is synthesized by one-step reaction from iodine pentafluoride, two-step reaction is continuously carried out in the reaction vessel, and the reaction effect is greatly enhanced by using the composite catalyst; and the original two-step reaction is changed into a one-step reaction, thus reducing the production steps, simplifying the production process and equipment and lowering the production investment.

Description

technical field [0001] The invention relates to the field of fluorine product intermediates, in particular to a method for preparing perfluoroalkyl iodide in one step. Background technique [0002] At present, the method for preparing perfluoroalkyl iodide is mainly carried out in two steps: first, pentafluoroiodoethane is synthesized with iodine pentafluoride, iodine and tetrafluoroethylene under the action of a catalyst, and then separated and purified to obtain pentafluoroiodoethane alkane; then pentafluoroiodoethane and tetrafluoroethylene synthesize perfluoroalkyl iodides containing many carbon numbers under the action of another catalyst. [0003] This method is the method commonly used by everyone at present. In the method, pentafluoroiodoethane is first synthesized, and then pentafluoroiodoethane and tetrafluoroethylene are used to synthesize perfluoroalkyl iodides containing multiple carbon numbers. The synthesis process needs to be completed in two steps. This ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/16C07C17/04B01J27/135
Inventor 何日兴肖玉岭张立亭毛震
Owner 山东中氟化工科技有限公司
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