Titanium-containing silica catalyst, preparation method and use thereof
A technology of silica and catalysts, applied in physical/chemical process catalysts, chemical instruments and methods, organic chemistry, etc., can solve the problems of low catalyst activity, selectivity, and poor stability
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Embodiment 1
[0047] Slowly add 350g of n-hexadecylamine to a mixed solution of 3200g deionized water and 1600g ethanol under stirring at 45°C to form a transparent solution A; simultaneously add 43g of trimethyl methyl silicate and 35g of tetrabutyl titanate to In a mixed solution composed of 300g isopropanol and 600g tetraethyl orthosilicate, stir for 60min to form solution B; slowly add solution B to solution A, stir for 24h, filter, wash, dry at 120°C for 12h, and then The solution containing ethanol was refluxed for 2 hours to remove the residual template agent, filtered, washed, and filtered three times. The filtered sample was dried at 120°C for 24 hours, and heated at 200°C for 6 hours under a nitrogen atmosphere to obtain a white solid powder.
[0048] Wherein, the reaction mixture has the following molar ratios: Ti / Si=0.0322, n-hexadecylamine / Si=0.4544, (water+ethanol+isopropanol) / Si=68.0790, trimethylmethylsilicate / tetraorthosilicate Ethyl ester = 0.1096.
[0049] Add 100 g of t...
Embodiment 2
[0052] Except that the 350g n-hexadecylamine in [Example 1] is replaced by 270g n-Dodecylamine, all the other conditions are the same as [Example 1].
[0053] Wherein, the reaction mixture has the following molar ratios: Ti / Si=0.0322, n-dodecylamine / Si=0.4567, (water+ethanol+isopropanol) / Si=68.0790, trimethylmethylsilicate / tetraorthosilicate Ethyl esters = 0.1096.
[0054]Measure the ultraviolet-visible spectrum of the prepared catalyst, and its spectrogram has an absorption peak at 218 nm; measure the infrared spectrum of the prepared catalyst, and its spectrogram has an absorption peak at a wavenumber of 955 cm -1 There is an absorption peak; measure the solid of the prepared catalyst 29 Si nuclear magnetic resonance spectrum, its spectrogram has absorption peak at 14.5ppm place; Measure the solid of catalyst 13 C nuclear magnetic resonance spectrum, its spectrum has an absorption peak at -0.7 ppm.
Embodiment 3
[0056] Except that 43g of trimethyl methylsilicate in [Example 1] was replaced by 40g of dimethyl dimethylsilicate, other conditions were the same as in [Example 1].
[0057] Wherein, the reaction mixture has the following molar ratio: Ti / Si=0.0320, n-hexadecylamine / Si=0.4520, (water+ethanol+isopropanol) / Si=67.7061, dimethyl dimethyl silicate / orthosilicate Tetraethyl ester=0.1157.
[0058] Measure the ultraviolet-visible spectrum of the prepared catalyst, and its spectrogram has an absorption peak at 220 nm; measure the infrared spectrum of the prepared catalyst, and its spectrogram has an absorption peak at a wavenumber of 960 cm -1 There is an absorption peak; measure the solid of the prepared catalyst 29 Si nuclear magnetic resonance spectrum, its spectrogram has absorption peak at 15.0ppm place; Measure the solid of catalyst 13 C nuclear magnetic resonance spectrum, its spectrum has an absorption peak at -0.9 ppm.
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