Method for preparing allyl acetate
A technology of allyl acetate and acetic acid, which is applied in the field of preparation of allyl acetate, can solve the problems of low space-time yield and selectivity, and achieve improved space-time yield and selectivity, good technical effects, and selectivity Improved effect
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Embodiment 1
[0010] (1) Catalyst preparation
[0011] Step (a): Take 1200ml of liquid carbon dioxide solution containing palladium(II) hexafluoroacetylacetonate and copper(II) hexafluoroacetylacetonate as the impregnating solution, the palladium content of the impregnating solution is 2.75g / L, and the copper content is 0.625g / L , impregnating 1100 ml of spherical silica carriers with a diameter of 4 to 6 mm at an impregnation pressure of 69 MPa and an impregnation temperature of 28° C. to obtain a catalyst precursor I;
[0012] Step (b): Then reduce the pressure and evaporate the liquid carbon dioxide in the catalyst precursor I at a rate of 0.3ml (liquid carbon dioxide) / min until the liquid carbon dioxide evaporates completely to obtain the catalyst precursor II;
[0013] Step (c): reducing the catalyst precursor II in a hydrogen atmosphere, the hydrogen flow rate is 0.2ml / min, and the reduction temperature is 75°C to obtain the catalyst precursor III;
[0014] Step (d): soak the catalys...
Embodiment 2
[0029] Except that the roasting step is added between step (c) and step (d), other steps are all the same as in Example 1. Wherein the roasting step is: the catalyst precursor III is roasted under a nitrogen / acetic acid atmosphere, wherein the partial pressure of acetic acid accounts for 5% of the total pressure, the roasting temperature is 250°C, and the roasting time is 24hr. For the convenience of comparison, the preparation conditions of the catalyst are listed in Table 1, the physical property data of the catalyst are listed in Table 2, and the evaluation conditions, space-time yield and selectivity data of the catalyst are listed in Table 3.
Embodiment 3~14
[0031] In addition to changing the concentration of palladium copper in the liquid carbon dioxide impregnation solution, the type of palladium copper compound, the concentration of potassium acetate solution, impregnation pressure, impregnation temperature, reducing gas, reduction temperature, molar ratio of reaction raw materials, space velocity of raw material gas, reaction pressure and reaction Except temperature, other operation steps are all identical with embodiment 2. For the convenience of comparison, the preparation conditions of the catalyst are listed in Table 1, the physical property data of the catalyst are listed in Table 2, and the evaluation conditions, space-time yield and selectivity data of the catalyst are listed in Table 3.
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