Method for preparing cyclopropanecarboxaldehyde
A technology of cyclopropane and formaldehyde, applied in the field of chemical synthesis of cyclopropane carboxaldehyde, can solve the problems of high reaction temperature, low product yield, low conversion rate, etc., and achieves the effects of high reaction efficiency, easy availability of raw materials and green route.
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Embodiment 1
[0032] Catalyst preparation
[0033] Weigh 10 mg of palladium nitrate in a beaker, add 52 g of deionized water, and mix well. Weigh 31g γ-Al 2 o 3 Add it to the above solution, stir for 24 hours, and then dry it in an oven at 120°C overnight. The above catalyst powder was placed in a tube furnace N 2 Under atmosphere, heat up to 300°C at a rate of 3°C / min and bake for 3h. Catalyst 1 was prepared.
[0034] Place 3g of catalyst 1 in a fixed-bed reactor (such as a fixed-bed reaction tube with an inner diameter of 1.2cm and a length of 40cm, and the catalyst is sieved to a size of 20-40 mesh), with nitrogen as the carrier gas; 2,5-dihydro Furan is preheated to a preheating furnace at 70°C; 2,5-dihydrofuran is preheated for 0.08h -1 The feed space velocity enters the fixed-bed reactor for reaction; the reaction product is received in liquid form after passing through the condensation and gas-liquid separator.
[0035] The product was checked by GC as described in the test ex...
Embodiment 2
[0037] Catalyst preparation
[0038] Weigh 10 mg of chloroplatinic acid into a beaker, add 42 g of deionized water, and mix well. Weigh 24g γ-Al 2 o 3 Add it to the above solution, stir for 24 hours, and then dry it in an oven at 120°C overnight. The above catalyst powder was placed in a tube furnace N 2 Under atmosphere, heat up to 300°C at a rate of 3°C / min and bake for 3h. Catalyst 2 was prepared.
[0039] Except for adjusting the reaction conditions as shown in Table 1 below, other reaction implementations are the same as in Example 1, and the product detection results are shown in Table 1 below.
Embodiment 3
[0041] Weigh 10 g of palladium nitrate in a beaker, add 33 g of deionized water, and mix well. Weigh 31g SiO2 2 Add to the above solution, add dropwise 10wt% sodium hydroxide aqueous solution to the above mixed liquid to adjust the pH to 10, then raise the temperature to 80°C and stir for 1 hour, then filter, and dry the filter cake in an oven at 120°C overnight. The above catalyst powder was placed in a tube furnace N 2 Under atmosphere, heat up to 300°C at a rate of 3°C / min and bake for 3h. Catalyst 3 was prepared.
[0042] Except for adjusting the reaction conditions as shown in Table 1 below, other reaction implementations are the same as in Example 1, and the product detection results are shown in Table 1 below.
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