Method for preparing dibutoxymethane from dimethoxymethane and n-butyl alcohol
A technology for dimethoxymethane and dibutoxymethane, which is applied in the field of preparing dibutoxymethane, can solve the problems of difficult product separation, high energy consumption, short reaction time and the like, and achieves good application prospects and simple process operation. , the effect of high selectivity
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Embodiment 1
[0038] Add 30g of dimethoxymethane, 64g of n-butanol and 3g of catalysts into a 200mL autoclave. The catalysts are KAD302 (Beijing Kairui Environmental Protection), KC107 (Tianjin Yunkai), NKC-9 (Tianjin Bohong), DA -330 (Jiangsu Tehua), D009B (Dandong Pearl), Amberlyst-15 (Jiangsu Sekesaisi), D072H (Tianjin Yunkai). use N 2 Replace the air in the kettle three times under the condition of 1.0MPa, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0MPaN again 2 , let it stand for 30 minutes, and use it to test the leak of the reactor to ensure that the device is airtight and then empty the gas in the kettle. 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 type are shown in Table 1.
[0039] Table 1. Effects of differe...
Embodiment 2
[0043] In a 200mL autoclave, the ratio of the amount of raw material dimethoxymethane and n-butanol is 2:1, 1:1, 1:2, 1:3, 1:4 and 3gAmberlyst-15 catalyst, at room temperature Next use N 2Replace the air in the kettle three times under the condition of 1.0MPa, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0MPaN again 2 , let it stand for 30 minutes, and use it to test the leak of the reactor to ensure that the device is airtight and then empty the gas in the kettle. Under the condition of ensuring no air leakage, the temperature was raised 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.
[0044] Table 2. The effect of different raw material ratios on the reaction activity and product selectivity.
[0045]
[0046] As can be seen from T...
Embodiment 3
[0048] In 200mL autoclave, add 30g dimethoxymethane, 64g n-butanol, 3gAmberlyst-15 catalyst, use N at room temperature 2 Replace the air in the kettle three times under the condition of 1.0MPa, so that the remaining air content in the kettle is less than 0.1%, and then pass 2.0MPaN again 2 , let it stand for 30 minutes, and use it to test the leak of the reactor to ensure that the device is airtight and then empty the gas in the kettle. Under the condition of ensuring no air leakage, heat up under normal pressure, the stirring speed of the reactor is 500 rpm, the reaction time is 6 hours, the reaction pressure is 3.0MPa, and the reaction temperatures are 25°C, 40°C, 60°C, and 80°C respectively , 100°C, 120°C, 130°C, 140°C, 150°C, 160°C, the reaction results under different reaction temperature conditions are shown in Table 3.
[0049] Table 3. Effect of Amberlyst-15 catalyst on the reactivity and product selectivity of dimethoxymethane and n-butanol at different reaction temp...
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