Iron-silicon molecular sieve, preparation method thereof, and sulfide oxidation method
A technology of iron-silicon molecular sieve and molecular sieve, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of limited application and poor catalytic performance, and achieve good catalytic effect and modulation selectivity.
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[0042] In the preparation method of the iron-silicon molecular sieve provided by the present disclosure, the micropore pore size distribution of the iron-silicon molecular sieve can be adjusted by adjusting the addition amount of the silicon source in step (2), when SiO 2 Calculate, when the molar ratio of the catalyst containing silicon molecular sieve described in step (1) and the silicon source described in step (2) is 100: (0.1-10), iron silicon molecular sieve can be made to satisfy X 1-1.8 / X 0.4-0.9 =A, 0.3<A<0.9.
[0043] According to the present disclosure, the type of the prepared iron-silicon molecular sieve is jointly determined by factors such as the type of silicon molecular sieve, the type of alkali source, and the ratio of materials. The silicon molecular sieve can be a fresh silicon molecular sieve or an inactivated silicon molecular sieve, which can be obtained commercially or by self-synthesis. The present disclosure has no special limitation on the type o...
Embodiment 1
[0090]At normal temperature (20°C, the rest of the examples are the same as the comparative examples) and normal pressure (0.1MPa, the rest of the examples are the same as the comparative examples), first mix the silicon molecular sieve with 1mol / L aqueous hydrochloric acid for beating, and then mix the mixed slurry at 80 Mix and stir at ℃ for 12 hours; after solid-liquid separation, mix the solid, iron source ammonium hydroxide, organosilicon source tetraethyl orthosilicate and sodium hydroxide aqueous solution (pH 12), and wait for tetraethyl orthosilicate to be hydrolyzed ( The hydrolysis rate is 40%), then the mixture is transferred to a stainless steel sealed reactor, and treated at 170°C for 12 hours, wherein the molar ratio of silicon molecular sieve: iron source: organic silicon source: acid: alkali: water is 100:0.5:2: 10:5:250, silicon molecular sieve and organic silicon source with SiO 2 In terms of acid, H + In terms of alkali in OH - count. The obtained product...
Embodiment 2
[0092] At normal temperature and pressure, first mix silicon molecular sieves with 5mol / L hydrochloric acid solution for beating, then mix and stir the mixed slurry at 60°C for 2 hours; Methyl orthosilicate is mixed with tetrapropylammonium hydroxide aqueous solution (pH 10), and after the methyl orthosilicate is hydrolyzed (hydrolysis rate is 50%), the mixture is transferred to a stainless steel sealed reaction kettle, and treated at 150°C for 12h , wherein, silicon molecular sieve: iron source: organosilicon source: acid: alkali: water molar ratio is 100:1:1:15:15:200, silicon molecular sieve and organosilicon source are SiO 2 In terms of acid, H + In terms of base, in N. The obtained product was filtered, washed with water, dried at 110° C. for 120 minutes, and then calcined at 550° C. for 3 hours to obtain FeSi molecular sieve S-2, whose XRD crystal phase pattern was consistent with that of Example 1.
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