Method of preparing tetrahydrofuran
A technology of tetrahydrofuran and butanediol, applied in chemical instruments and methods, organic chemistry, physical/chemical process catalysts, etc., can solve the problems of low tetrahydrofuran yield, dangerous methods, etc., and achieve the effect of excellent reactivity
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Embodiment 1
[0025] A fixed bed reactor with a diameter of 20 mm and a length of 520 mm was used for the gas phase catalytic reaction. First, 2 g of aluminum sulfate catalyst was charged into the reactor, and the catalyst was activated with helium at 370° C. for 2 hours. Using a syringe pump, 1,4-butanediol at a flow rate of 0.5 cc / min was mixed with helium and fed into the reactor at a constant flow rate of 5.0 liters / hour. The reaction was carried out at 200° C. under one atmospheric pressure, and the reaction products were analyzed on-line using a Poropak QS column and a gas chromatograph equipped with a flame ionization detector (FID). After the reaction reached a steady state, the products passing through the reactor were analyzed. The yield of tetrahydrofuran was 98.5%.
Embodiment 2
[0027] The liquid-phase catalytic reaction was carried out in a 500 ml three-necked round bottom reactor equipped with a magnetic stirrer and reflux device. Before the reaction, the catalyst was activated with helium gas at 300° C. for 2 hours, and 0.5 g of pretreated aluminum sulfate and 100 g of 1,4-butanediol were added to the reactor. The reaction was carried out at a temperature of 200° C. for 1 hour, and the reaction product was condensed using a condenser. The condensed product was then distilled to separate residual 1,4-butanediol and analyzed using a gas chromatograph as described in Example 1. As a result, 98.5% tetrahydrofuran was obtained.
Embodiment 3-5
[0029] Except using one of transition metal sulfate catalysts such as nickel sulfate, ferrous sulfate and chromium sulfate of 1g and 100g of 1,4-butanediol respectively, all the other are in the same manner as described in Example 2 The preparation process of tetrahydrofuran was carried out. The yields for each reaction are listed in Table 1.
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