Continuous production method for perfluoro tripropylamine
A technology of perfluorotripropylamine and its production method, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of amino compounds, etc., can solve the problems of many by-products, low yield, complicated perfluorotripropylamine equipment, etc., and achieve The effect of reducing breakage and improving productivity
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Embodiment 1
[0025] In the monel alloy fluorination reactor with an inner diameter of 80 mm and a length of 200 mm, spherical cobalt oxide with a diameter of 3 mm is filled. The fluorination reactor is heated to 300°C, and a mixed gas of 50% fluorine and 50% nitrogen is introduced for fluorination, so that cobalt oxide is completely converted into cobalt trifluoride. Then maintain the temperature of the fluorination reactor at 230°C; continuously feed 20% fluorine-nitrogen mixed gas and 10% tripropylamine-nitrogen mixed gas in the ratio of 10:1 molar ratio of fluorine gas to tripropylamine for reaction, and control the residence time for 5 Second. After 3 hours, neutralize the collected reaction product with 20% potassium hydroxide aqueous solution until the pH value is neutral, let it stand, after layering, take the organic phase and wash it with deionized water three times, separate the organic phase and wash it with anhydrous sodium sulfate After drying, carry out rectification and sep...
Embodiment 2
[0027] Using the same equipment as in Example 1, the fluorination reactor was heated to 300°C, and a 50% fluorine-50% nitrogen mixed gas was introduced for fluorination, so that cobalt oxide was completely converted into cobalt trifluoride. Then maintain the temperature of the fluorination reactor at 200°C; continuously feed 20% fluorine-nitrogen mixed gas and 15% tripropylamine-nitrogen mixed gas in the ratio of 12:1 molar ratio of fluorine gas to tripropylamine to react, and control the residence time for 5 Second. After 3 hours, neutralize the collected reaction product with 20% potassium hydroxide aqueous solution until the pH value is neutral, let it stand, after layering, take the organic phase and wash it with deionized water three times, separate the organic phase and wash it with anhydrous sodium sulfate After drying, carry out rectification and separation, take the boiling point of 127 ~ 128 ℃ for fractionation, and obtain perfluorotripropylamine with a purity of 98%...
Embodiment 3
[0029] Using the same equipment as in Example 1, the fluorination reactor was heated to 260°C, and a 50% fluorine-50% nitrogen mixed gas was introduced for fluorination, so that cobalt oxide was completely converted into cobalt trifluoride. Then the temperature of the fluorination reactor is maintained at 260°C; 30% fluorine-nitrogen mixed gas and 20% tripropylamine-nitrogen mixed gas are continuously fed into the reaction according to the molar ratio of fluorine gas to tripropylamine 16:1, and the residence time is controlled for 5 Second. After 3 hours, neutralize the collected reaction product with 20% potassium hydroxide aqueous solution until the pH value is neutral, let it stand, after layering, take the organic phase and wash it with deionized water three times, separate the organic phase and wash it with anhydrous sodium sulfate After drying, carry out rectification and separation, take the boiling point of 127 ~ 128 ℃ for fractionation, and obtain perfluorotripropylam...
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