Method for preparing benzalacetone under supercritical condition
A benzylidene acetone and supercritical technology, applied in the field of synthesizing benzylidene acetone, can solve the problems of long reaction time, low empty yield, large energy consumption, etc., and achieve shortened reaction time, improved reaction temperature and pressure, and reaction selectivity. high effect
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Embodiment 1
[0017] Example 1 (eg figure 1 ): Turn on high-pressure metering pump 1, pump acetone A at a constant rate of 7ml / min, turn on high-pressure metering pump 2, pump benzaldehyde B at a constant rate of 1ml / min, set the temperature of preheater 3 at 250°C, and exceed The temperature of the critical pipeline reactor 4 is set at 350°C, the high-precision reverse pressure controller 6 behind the condenser 5 is adjusted, the pressure is controlled at 25±1MPa, and the reaction residence time is 20min. After the reaction was completed, the reaction solution was collected and analyzed by gas chromatography. With ethyl benzoate as the internal standard, the content of the calibrated benzylidene acetone was 20.3%, and the calculated selectivity of the benzylidene acetone was 96.3%.
Embodiment 2-6
[0019] According to embodiment 1, by changing the flow rate of pump 1, to change the molar ratio of benzaldehyde and acetone, keeping the conditions such as reaction temperature, preheater temperature, reverse pressure constant, the following results are obtained after the reaction (Table 1):
[0020] Table 1, the influence of raw material ratio on reaction
[0021]
Embodiment 7-12
[0023] According to Example 1, only the temperature of the pipeline reactor was changed, and the conditions such as pump flow rate, preheater temperature and reverse pressure were kept constant, and the following results were obtained after the reaction (Table 1):
[0024] Table 2. Effect of temperature on reaction
[0025] Example temperature Benzylidene acetone selectivity 7 300℃ 92.2% 8 320℃ 93.8% 9 340℃ 95.7% 10 360℃ 96.4% 11 390℃ 96.0% 12 420℃ 94.7% 13 450℃ 93.4%
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