Preparation of transition metal catalyst for preparing oxime through oxidization of amine and application of transition metal catalyst
A transition metal and transition metal salt technology is applied in the field of preparation of transition metal catalysts, which can solve the problems of low final selectivity, numerous side reactions, and unsatisfactory problems, and achieves the prospect of expanding application fields, convenient preparation, and industrialization promotion and application. significant effect
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Embodiment 1
[0016] a. Preparation of high silicon MOR molecular sieve
[0017] 10 g MOR molecular sieve (as SiO 2 The silicon-aluminum ratio is 7.8) mixed with 100 g of hydrochloric acid with a concentration of 6 mol / L, acid-washed at 90 °C for 10 h, and the dealuminated molecular sieves are filtered and washed until neutral to obtain high-silicon MOR Molecular sieve.
[0018] b. Preparation of transition metal catalysts
[0019] Take 0.1 mol of the above-prepared high-silicon MOR molecular sieve and uniformly disperse in the sodium tungstate solution prepared by 3.3 mmol of sodium tungstate (calculated as WO3) and 18g of water, stir at 80°C for 6 h, and then in 100 The moisture was evaporated at ℃, and finally calcined at 550℃ for 6 h to obtain 6.7 g of tungsten-containing MOR mercerized molecular sieves, which are transition metal catalysts for the oxidation of amines to oximes.
Embodiment 2
[0021] a. Preparation of high silicon ZSM-5 molecular sieve
[0022] Mix 10 g of ZSM-5 molecular sieve (calculated as SiO2, silicon-aluminum ratio of 20) with 50 g of nitric acid with a concentration of 13 mol / L, pickle at 100 °C for 5 h, and filter the dealuminized molecular sieve, Wash until neutral to obtain high silicon ZSM-5 molecular sieve.
[0023] b. Preparation of transition metal catalysts
[0024] Take 0.1 mol of the high silicon ZSM-5 molecular sieve prepared above and uniformly disperse in 1 mmol of ammonium tungstate (in WO 3 In the ammonium tungstate solution prepared with 18g of water, stirred at 30°C for 24 hours, then evaporated to dryness at 100°C, and finally roasted at 550°C for 6 hours to obtain 6.2 g of Tungsten ZSM-5 molecular sieves are transition metal catalysts for the oxidation of amines to oximes.
Embodiment 3
[0026] a. Preparation of high silicon Beta molecular sieve
[0027] Mix 10 g of Beta molecular sieve (calculated as SiO2, silicon-aluminum ratio of 10) with 50 g of sulfuric acid with a concentration of 4 mol / L, pickle at 60 °C for 24 h, and filter and wash the dealuminated molecular sieve to Neutral, made of high silicon Beta molecular sieve.
[0028] b. Preparation of transition metal catalysts
[0029] Take 1 mol of the above-prepared high-silicon Beta molecular sieve and uniformly disperse it in a tungsten chloride solution prepared by 5 mmol of tungsten chloride (calculated as WO3) and 36 g of water, stir at 60°C for 1 hour, and then The moisture was evaporated at ℃, and finally calcined at 550℃ for 6 h to obtain 7.1 g of tungsten-containing Beta molecular sieve, which is a transition metal catalyst for the oxidation of amines to prepare oximes.
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