A method for continuous production of ethyl trifluoroacetate
A technology of ethyl trifluoroacetate and trifluoroacetyl chloride, which is applied in the field of continuous preparation of ethyl trifluoroacetate, can solve the problems of high equipment requirements, difficult handling, equipment corrosion, etc., and achieve safe and controllable reaction and short reaction time , the effect of high conversion rate
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Embodiment 1
[0034] optional attachment figure 2 1 piece of corning straight channel module (as premixing preheating module 3), 6 pieces of corning "heart-shaped" microchannel reaction modules, 1 piece of corning straight channel module (as quenching module 10). According to attached image 3 The reaction process shown constitutes a continuous flow microchannel reaction system. Heat transfer oil is used as the reaction heat exchange medium. According to the forced heat transfer principle of the microchannel reactor, only two temperature measuring points are set at the reactor inlet and outlet. Before the reaction, the microchannel reaction system and connecting pipelines were dehydrated and dried, and the air tightness was checked at 1.0MPa. by attaching image 3 1 liquid-phase pump (such as a diaphragm metering pump) in the system continuously and stably adds raw material ethanol to the microchannel reaction system. by attaching image 3 The 2-gas mass flowmeter in the microchannel re...
Embodiment 2
[0038] Use the same Corning microchannel reactor as in Example 1, and follow the same connection and control methods. In this example, the reaction conditions were changed.
[0039] Set the heat exchanger temperature to 60°C, that is, the reaction temperature, and set the reaction pressure to 0 MPa. Raw material ethanol, the feed rate is 0.88g / min, the feed rate of trifluoroacetyl chloride gas is 2.66g / min, the residence time of the reaction is 20s, and the molar ratio of trifluoroacetyl chloride to ethanol is 1.05:1. The reaction raw materials enter the "heart-shaped" micro-channel reaction module 4 after passing through the micro-channel premixing and preheating module 3, and the trifluoroacetyl chloride gas directly enters the "heart-shaped" micro-channel reaction module 4 through the gas mass flow meter. In microchannel reaction modules 4-9, trifluoroacetyl chloride reacts with ethanol. The crude product of the reaction is collected after passing through the quenching mo...
Embodiment 3
[0042] Use the same Corning microchannel reactor as in Example 1, and follow the same connection and control methods. In this example, the reaction conditions were changed.
[0043] Set the heat exchanger temperature to 65°C, that is, the reaction temperature, and set the reaction pressure to 0 MPa. Raw material ethanol, the feed rate is 1.68g / min, the feed rate of trifluoroacetyl chloride gas is 5.31g / min, the residence time of the reaction is 10s, and the molar ratio of trifluoroacetyl chloride to ethanol is 1.1:1. The reaction raw materials enter the "heart-shaped" micro-channel reaction module 4 after passing through the micro-channel premixing and preheating module 3, and the trifluoroacetyl chloride gas directly enters the "heart-shaped" micro-channel reaction module 4 through the gas mass flow meter. In microchannel reaction modules 4-9, trifluoroacetyl chloride reacts with ethanol. The crude product of the reaction is collected after passing through the quenching mod...
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