A method for preparing dibutoxymethane with liquid acid and loaded solid acid as catalyst
A technology of dibutoxymethane and dimethoxymethane, applied in the field of dibutoxymethane preparation, can solve the problems of short reaction time, difficult separation of products, high energy consumption, etc., and achieve high selectivity, good application prospects, The effect of simple process operation
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Embodiment 1
[0048] Add 30 g of dimethoxymethane, 64 g of n-butanol and 3 g of catalyst into a 200 mL autoclave. The catalysts are sulfuric acid (Shandong Jiuding) with a mass fraction of 98% and hydrochloric acid with a mass fraction of 38% ( Hebei Yongfei), nitric acid with a mass fraction of 50% (Hebei Yongfei), and hydrofluoric acid with a mass fraction of 45% (Shandong Jiuding). use N 2 Replace the air in the kettle three times under the condition of 1.0 MPa, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0 MPa N 2 , let it stand for 30 minutes, and use it for leak testing of the reactor to ensure that the device is airtight and then evacuate the gas in the reactor. Under the condition of ensuring no air leakage, the reaction was heated and heated. The stirring speed of the reactor was 500 rpm, the reaction temperature was 120 °C, the reaction pressure was 3.0 MPa, and the reaction time was 6 hours. The results of controlling the catalyst types are...
Embodiment 2
[0053] Add raw material dimethoxymethane and n-butanol in 200 mL autoclave The ratio of the amount of substance is 2:1, 1:1, 1:2, 1:3, 1:4 and 3 g hydrofluoric acid catalyst, at room temperature with N 2 Replace the air in the kettle three times under the condition of 1.0 MPa, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0 MPa N 2 , let it stand for 30 minutes, and use it for leak testing of the reactor to ensure that the device is airtight and then evacuate the gas in the reactor. Under the condition of ensuring no air leakage, heating was carried out under normal pressure, the stirring speed of the reactor was 500 rpm, the reaction temperature was 120 °C, the reaction pressure was 3.0 MPa, and the reaction time was 6 hours. The results of controlling the ratio of raw materials are shown in Table 2.
[0054] Table 2. The effect of different raw material ratios on the reaction activity and product selectivity.
[0055]
[0056] As can...
Embodiment 3
[0058] Table 3.H 2 SO 4 / SiO 2 Effects of catalysts on the reactivity and product selectivity of dimethoxymethane and n-butanol at different reaction temperatures.
[0059]
[0060] Preparation of sulfuric acid with a mass fraction of 20% H 2 SO 4 / SiO 2 Supported catalyst, the preparation process is as follows: first, put silica into a muffle furnace and roast at 500°C for 4 hours to remove the water adsorbed in silica, take 80 g of calcined silica as a carrier; take 20 g of 98 % concentrated sulfuric acid was diluted into a 49% sulfuric acid solution, and 40 g of the sulfuric acid solution was impregnated into 80 g of silica carrier pores in an ultrasonic environment; the impregnated catalyst precursor was dried in an oven at 110 °C for 10 hours , baked in an oven at 350 °C for 3 hours to produce H 2 SO 4 / SiO 2 supported catalyst. Add 30 g dimethoxymethane, 64 g n-butanol, 3 g H 2 SO 4 / SiO 2 catalyst, at room temperature with N 2 Replace the air in the kett...
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