Core-shell metal hybrid silicate-1/SAPO-5 composite molecular sieve ceramic membrane and preparation method thereof
A SAPO-5, composite molecular sieve technology, applied in catalyst activation/preparation, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of long time, low film formation rate, high energy consumption, delay deactivation, reduce preparation cost, the effect of improving completeness
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[0033] The preparation method of a core-shell metal hybrid silicate-1 / SAPO-5 composite molecular sieve ceramic membrane provided by the present invention includes the following steps:
[0034] 1. Preparation of silicate-1 molecular sieve synthesis solution: using silicon source, organic template, transition metal salt and water as raw materials, the molar composition of the raw materials of the reaction system is calculated as oxide: SiO 2 : ATemplate: bH 2 O: cX, a=0.001~0.03, b=40~1000, c=0.015~0.1, X is a transition metal salt, the transition metal is selected from Fe, Co or Ni; the organic template is selected from tetrapropyl hydrogen Ammonium oxide (TPAOH), tetrapropylammonium bromide (TPABr), triphenylamine (TPA) or triethylamine (TEA), and the silicon source is selected from ethyl orthosilicate, silica sol, silicic acid or water glass.
[0035] According to the above-mentioned ratio and dosage, under stirring, add the weighed silicon source dropwise to water and stir until i...
Example Embodiment
[0044] Example 1
[0045] (1) Preparation of Co hybrid silicate-1 molecular sieve synthesis solution
[0046] According to SiO 2 :0.001TPABr:40H 2 O:0.1Co(NO 3 ) 3 (mol) material ratio to prepare Co hybrid silicate-1 molecular sieve synthesis solution, silicon source is ethyl orthosilicate, according to the above material ratio, add ethyl orthosilicate under stirring conditions, and stir to dissolve for 5 hours , It is completely hydrolyzed to obtain the ethyl orthosilicate aqueous solution, after the ethyl orthosilicate aqueous solution is clarified, add Co(NO 3 ) 3 And TPABr, stirring and dissolving for 3 hours, after the substances are completely dissolved, adjust the pH of the reaction solution to between 10-12 to obtain the Co hybrid silicate-1 molecular sieve synthesis solution.
[0047] (2) Preparation of Co hybrid SAPO-5 molecular sieve synthesis solution
[0048] Follow Al 2 O 3 :1.3P 2 O 5 :0.5SiO 2 :3TPABr:1000H 2 O:0.075Co(NO 3 ) 3 (mol) of the material ratio to prepare th...
Example Embodiment
[0063] Example 2
[0064] (1) Preparation of Fe hybrid silicate-1 molecular sieve synthesis solution
[0065] It is basically the same as Example 1, except that in the process of preparing silicate-1 molecular sieve, the silicon source used is silica sol, and the material formula of the synthetic liquid is SiO 2 : 0.03TPAOH: 1000H 2 O: 0.015FeCl 3 .
[0066] (2) Preparation of Fe hybrid SAPO-5 molecular sieve synthesis solution
[0067] Basically the same as Example 1, except that during the preparation process of Fe hybrid SAPO-5 molecular sieve synthesis solution, the aluminum source, silicon source, organic template and active metal used are sodium aluminate, silica sol, TPA and Ferric chloride, material formula is Al 2 O 3 :0.8P 2 O 5 :0.05SiO 2 :0.75TPA:45H 2 O:0.3FeCl 3 .
[0068] (3) Preparation of Fe hybrid core-shell silica-1 / SAPO-5 composite molecular sieve seeds
[0069] The reaction temperature of Fe hybrid silicate-1 molecular sieve synthesis solution is set to 200℃, and th...
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