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] A kind of preparation method of core-shell type metal hybrid silicate-1 / SAPO-5 composite molecular sieve ceramic membrane proposed by the present invention comprises the following steps:
[0034] 1. Preparation of silicate-1 molecular sieve synthesis liquid: using silicon source, organic template, transition metal salt and water as raw materials, the molar composition of raw materials in the reaction system is calculated as oxides: 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 (Template) is selected from tetrapropyl hydrogen Ammonium oxide (TPAOH), tetrapropylammonium bromide (TPABr), triphenylamine (TPA) or triethylamine (TEA), the silicon source is selected from tetraethyl orthosilicate, silica sol, silicic acid or water glass.
[0035] According to the above ratio and dosage, in the stirring state, add the weighed silicon source dropwise into t...
Embodiment 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 Prepare Co hybrid silicate-1 molecular sieve synthetic liquid with a material ratio of (mol), the silicon source is tetraethyl orthosilicate, according to the above-mentioned ratio of materials, add tetraethyl orthosilicate under stirring conditions, and stir and dissolve for 5 hours , to make it completely hydrolyzed to obtain an aqueous solution of ethyl orthosilicate, and after the aqueous solution of ethyl orthosilicate is clarified, add Co(NO 3 ) 3 and TPABr, stirring and dissolving for 3 hours, and after the substances are completely dissolved, adjust the pH of the reaction solution between 10 and 12 to obtain a Co hybrid silicate-1 molecular sieve synthetic solution.
[0047] (2) Preparation of Co hybridized SAPO-5 molecular sieve synthesis solution
[0048] According to Al 2 o 3 :1.3P 2 o 5 :0.5SiO2 2 :3TPABr:1000H ...
Embodiment 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] It is basically the same as Example 1, except that during the preparation of the 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, the material formula is Al 2 o 3 :0.8P 2 o 5 :0.05SiO2 2 :0.75TPA:45H 2 O:0.3FeCl 3 .
[0068] (3) Preparation of Fe hybrid core-shell silicate-1 / SAPO-5 composite molecular sieve seed crystals
[0069] The reaction temperature of Fe hybrid silicate-1 molecular sieve synthesis solution was ...
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