Preparation method of spherical MFI topological structure all-silicon molecular sieve catalyst containing trace rare earth ions and preparation method of caprolactam
An all-silicon molecular sieve and rare earth ion technology, which is applied in the preparation of caprolactam and the preparation of spherical MFI topology structure of all-silicon molecular sieve catalyst to achieve the effects of improving economy, prolonging catalyst life and high crystallinity
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[0062] A method for preparing a spherical MFI topological structure all-silicon molecular sieve catalyst containing a trace amount of rare earth ions, comprising the following steps:
[0063] a. Mix silicon source, rare earth ion source, organic template and water to obtain a colloidal mixture; wherein, SiO in the colloidal mixture 2 The molar ratio of organic template agent and water is 1:(0.05-0.50):(5-100); in terms of silicon dioxide, the mass ratio of silicon source to rare earth ions is (10000-200000):1.
[0064] b. The colloidal mixture is subjected to two-stage variable temperature hydrothermal crystallization to obtain a crystallized product.
[0065] c. Washing and separating the crystallized product to obtain an all-silicon molecular sieve with an MFI topological structure containing a trace amount of rare earth ions.
[0066] d. The MFI topological structure all-silicon molecular sieve is subjected to roll forming treatment, roasting treatment and post-treatment w...
Embodiment 1
[0098] This example is used to illustrate the preparation method of the spherical MFI topological structure all-silicon molecular sieve catalyst containing a very small amount of rare earth ions provided by the present invention.
[0099] With 208kg tetraethyl orthosilicate, 180kg22.5% by weight of tetrapropylammonium hydroxide, 7.3 grams of Ce (NO 3 ) 4 ·7H 2 O and 220kg of water are mixed, stirred at room temperature for 4 hours to form a colloidal mixture, and the molar ratio of the mixture is SiO 2 :TPAOH:H 2 O=1:0.2:20, SiO 2 with Ce 3+ The mass ratio of 30300:1, the above mixture was transferred to 1M 3 In a stainless steel reaction kettle, first hydrothermally crystallize at 60°C for 1 day, then hydrothermally crystallize at 120°C for 2 days, wash, filter, and dry at 120°C for 24 hours to obtain the all-silicon molecular sieve required for rolling molding in this example. Grind it into the required mesh size for roll forming on the pulverizer.
[0100] The all-si...
Embodiment 2
[0106] This example is used to illustrate the preparation method of the spherical all-silicon molecular sieve catalyst containing a very small amount of rare earth ions provided by the present invention.
[0107] With 208kg orthosilicate ethyl ester, the tetrapropyl ammonium hydroxide of 180kg22.5% by weight, 14 grams of Ce(NO 3 ) 3 ·6H 2 O and 220kg of water are mixed, stirred at room temperature for 3 hours to form a colloidal mixture, and the molar ratio of the mixture is SiO 2 :TPAOH:H 2 O=1:0.2:20, SiO 2 with Ce 3+ The mass ratio of 13500:1, the above mixture was transferred to 1M 3 In a stainless steel reaction kettle, first hydrothermally crystallize at 50°C for 1 day, then hydrothermally crystallize at 100°C for 2 days, wash, filter, and dry at 120°C for 24 hours to obtain the all-silicon molecular sieve required for rolling molding in this example. Grind it into the required mesh size for roll forming on the pulverizer.
[0108] The all-silicon molecular sieve ...
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