Catalyst and preparation method thereof, and method for preparing laurolactam through gas phase rearrangement reaction
A catalyst and fluoride technology, applied in the preparation of lactam, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as equipment corrosion and environmental pollution
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Embodiment 1
[0047] 1) Rare earth-doped fluorine-containing SPEEK / Al 2 o 3 -SiO 2 -ZrO 2 Preparation of composite catalyst
[0048] a) Maintain the system at 0-5°C, dissolve 2g TPAOH in 300g deionized water; at the same time slowly add 0.042g (three) scandium nitrate hexahydrate, 0.008g yttrium trichloride, 10g Al(NO 3 ) 3 9H 2 O, 10gZrOCl 2 ·8H 2 0, 20gTEOS, feeding time 1h; under stirring conditions, slowly add 25% ammonia water dropwise to adjust the solution to pH=10, continue to stir for 2h, stop stirring and age for 1h; vacuum filter, wash with deionized water to neutral properties; the filter cake was dried at 120°C for 28 hours, then roasted at 500°C for 2 hours, ground and sieved to obtain rare earth-doped Al 2 o 3 -SiO 2 -ZrO 2 carrier.
[0049] b) Take 10g of rare earth doped Al 2 o 3 -SiO 2 -ZrO 2 The carrier was added to 30 g of a 1% sodium fluoride aqueous solution, soaked at 50°C for 30 minutes, filtered, washed with deionized water, and dried to obtain a flu...
Embodiment 2
[0066] 1) Rare earth-doped fluorine-containing SPEEK / Al 2 o 3 -SiO 2 -ZrO 2 Preparation of composite catalyst
[0067] a) Maintain the system at 0-5°C, dissolve 3g TPAOH in 300g deionized water; at the same time slowly add 0.09g (three) scandium nitrate hexahydrate, 0.01g yttrium trichloride, 12g Al(NO 3 ) 3 9H 2 O, 10g ZrOCl 2 ·8H 2 0, 25gTEOS, feeding time 1h; under stirring condition, slowly add 25% ammonia solution dropwise to adjust the solution to pH=9, continue to stir for 2h, stop stirring and age for 1h; decompression suction filtration, wash with deionized water to Neutral; the filter cake was dried at 120°C for 24h, then roasted at 550°C for 2h, ground and sieved to obtain rare earth-doped Al 2 o 3 -SiO 2 -ZrO 2 carrier.
[0068] b) Take 10g of rare earth doped Al 2 o 3 -SiO 2 -ZrO 2 The carrier was added to 20 g of a sodium fluoride aqueous solution with a mass fraction of 1%, soaked at 50°C for 30 minutes, filtered, washed with deionized water, and...
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