Preparation for composite titanium oxide catalyst of ester interchange synthetic phenyl ester oxalate
A technology of phenyl oxalate and catalyst, which is applied in the field of preparation of composite oxide catalysts, can solve problems such as not seen, and achieve the effects of low cost, mild operating conditions, conversion rate and product selectivity
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Embodiment 1
[0015] [Example 1] Preparation and Activity Investigation of Composite Titanium Silicon Oxide Catalyst
[0016] The present invention prepares phenol and dimethyl oxalate transesterification and synthesizes phenyl oxalate with composite titanium silicon oxide catalyst implementation investigation. Add 0.05 g of acetylacetone dropwise into an absolute ethanol solution containing 0.26 g of tetrabutyl titanate, and stir thoroughly to obtain solution A. Prepare an ethanol solution containing 20.82 g of ethyl silicate, add 5 ml of glacial acetic acid and 10 ml of deionized water, and stir thoroughly to obtain solution B. Slowly drop solution B into solution A in a nitrogen flow, stir well to obtain a miscible solution, let stand in a nitrogen flow at room temperature for 24 to 72 hours, precipitate to form a gel, and vacuum dry the gel at 60 to 80°C After 2 to 6 hours, after crushing and grinding, put it into a muffle furnace and bake at 550° C. for 5 hours to prepare a titanium-s...
Embodiment 2-5
[0019] The catalyst was changed to composite TiO 2 -SiO 2 A series of catalysts, wherein the content of titanium oxide is respectively 2.5%, 5%, 10%, 20%, under the situation that other conditions are exactly the same as in Example 1, carry out transesterification reaction, respectively form embodiment 2-5, investigate reaction result.
[0020] Table 1: TiO 2 -SiO 2 Series catalyst transesterification results (weight percentage)
[0021] Titanium Oxide Containing DMO Selectivity, % Yield, %
Embodiment
[0023] Amount, wt% Conversion % Anisole MPO DPO MPO DPO
[0024] 1 1 43.5 0.2 83.4 16.1 36.3 7.0
[0025] 2 2.5 39.7 0.4 78.2 21.4 31.1 8.5
[0026] 3 5 29.5 0.7 86.3 12.9 25.5 3.8
[0027] 4 10 27.3 0.8 85.0 14.1 23.2 3.9
[0028] 5 20 49.6 0.2 77.0 22.6 38.2 11.2
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