Metal hetero-element modified titanium nitride-polyaniline catalyst, preparation method and application thereof in synthesis of p-hydroxyanisole
A technology of heteroelements and catalysts, applied in the field of titanium nitride-polyaniline catalyst and its preparation, can solve the problems of easy deactivation, decreased catalyst activity, low low temperature efficiency, etc., and achieves the effect of good stability
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Embodiment 1
[0044] Zinc modified titanium nitride-polyaniline composite catalyst, the preparation method is as follows:
[0045] (1) Solution A: Add 180 g of colloidal silica solution, 126 g of cyanamide, 816 g of n-butyl titanate, 268 g of zinc nitrate (hexahydrate) and 205 g of ammonium persulfate into 630 g of ethanol, and fully stir at 40°C for 12 hours;
[0046] (2) Solution B: Add 84g of aniline to 837g of 1mol / L hydrochloric acid solution, and fully stir at 30°C for 6h;
[0047] (3) Add solution A to solution B, fully stir at 20°C for 9 hours, evaporate to dryness at 120°C to obtain block. Take 300g block and calcinate at 900°C under nitrogen atmosphere for 8h, the heating rate is 3°C / min, then place in 4500g ammonium bifluoride aqueous solution (5wt%) and stir for 36h to remove the silica template, filter, wash with distilled water, and dry at 120°C for 36h Finally, the composite catalyst was obtained with a specific surface area of 324m 2 / g, the pore diameter is about 29nm. ...
Embodiment 2
[0051] Cesium modified titanium nitride-polyaniline composite catalyst, the preparation method is as follows:
[0052] (1) Add 120g of colloidal silica solution, 180g of urea, 684g of titanium tetrachloride, 59g of cesium nitrate and 137g of ammonium persulfate into 540g of ethanol, and fully stir for 9 hours at 30°C;
[0053] (2) Solution B: add 56 g of aniline to 837 g of 2mol / L hydrochloric acid solution, and stir fully at 40°C for 9 hours;
[0054] (3) Add solution A to solution B, fully stir at 40°C for 6 hours, and evaporate to dryness at 105°C to obtain a lump. Take 300g block and calcinate at 600°C for 4h under nitrogen atmosphere, the heating rate is 1°C / min, then place in 3000g ammonium bifluoride aqueous solution (2wt%) and stir for 60h to remove the silica template, filter, wash with distilled water, and dry at 100°C for 60h Finally, a composite catalyst is obtained with a specific surface area of 468m 2 / g, the pore diameter is about 33nm.
[0055] The compos...
Embodiment 3
[0058] Manganese modified titanium nitride-polyaniline composite catalyst, the preparation method is as follows:
[0059] (1) Add 240g of colloidal silica solution, 252g of dicyandiamide, 1020g of n-butyl titanate, 151g of manganese nitrate (tetrahydrate) and 274g of ammonium persulfate into 1764g of ethanol, and fully stir for 6 hours at 20°C;
[0060] (2) Solution B: 112g of aniline was added to 2232g of 3mol / L hydrochloric acid solution, and fully stirred at 20°C for 12h;
[0061] (3) Add solution A to solution B, fully stir at 30°C for 12 hours, and evaporate to dryness at 90°C to obtain lumps. Take 300g block and calcinate at 1200°C for 6h under nitrogen atmosphere, the heating rate is 6°C / min, then place in 6000g ammonium bifluoride aqueous solution (10wt%) and stir for 12h to remove the silica template, filter, wash with distilled water, and dry at 150°C for 12h Finally, the composite catalyst is obtained, and the specific surface area is 210m 2 / g, the pore diameter ...
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