Hydrogen molecular sieve, preparation method thereof and application in preparing propylene from methyl alcohol
A hydrogen-type molecular sieve and ammonium hydroxide technology, applied in molecular sieve catalysts, chemical instruments and methods, ethylene production, etc., can solve the problems of short life, fast deactivation of coking, high selectivity of aromatics, etc., and achieve good stability and long life , highly selective effect
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[0032] The invention provides a kind of preparation method of hydrogen type molecular sieve, comprises the following steps:
[0033] (1) Mix silicon source, aluminum source, template agent, crystallization regulator, structure directing agent and water, and age to obtain a precursor; the template agent includes hexamethylenediamine derivatives and organic amine salts; the hexamethylenediamine Amine derivatives include hexaethyl-1,6-hexanediammonium bromide or hydroxylated hexaethyl-1,6-hexanediammonium; the organic amine salts include diethyldipropylammonium bromide, ethyl One of tripropylammonium bromide, diethyldipropylammonium hydroxide and ethyltripropylammonium hydroxide;
[0034] (2) hydrothermal crystallization of the precursor obtained in the step (1) to obtain a crystal;
[0035] (3) roasting the crystal obtained in the step (2) to obtain the former molecular sieve powder;
[0036] (4) performing ion exchange on the molecular sieve former powder obtained in the step...
Embodiment 1
[0062] Mix 35.84g of water and templating agent (4.18g of hexaethyl-1,6-hexanediammonium bromide and 2.52g of ethyltripropylammonium bromide) at 25°C, stir and dissolve; add aluminum source (0.36g of nitric acid Aluminum), crystallization modifier (0.28g ammonium acetate), stirred for 1h; added structure directing agent (0.23g boric acid), stirred for 1h; Aging for 24h to obtain the precursor;
[0063] Transfer the precursor obtained above into a 100mL crystallization kettle, and conduct hydrothermal crystallization at 180°C for 168 hours. After the crystallization is completed, filter, wash, and dry to obtain crystals;
[0064] The XRD test was carried out on the crystallization product on Rigaku MiniFlex II X-ray diffractometer, CuKα radiation, tube voltage 40kV, tube current 15mA, Ni filter, scan rate 2° / min, step width 0.02, to obtain X-ray Diffraction spectrum as figure 1 shown. from figure 1 It can be seen that there are obvious diffraction peaks at 7.0, 7.9, 8.8, 11...
Embodiment 2
[0070]According to the method of Example 1, with 9.73g hexaethyl-1,6-hexammonium hydroxide and 6.31g ethyltripropylammonium hydroxide as template (wherein hexaethyl-1,6-hexammonium hydroxide Both diammonium and ethyltripropylammonium hydroxide are 30wt.% aqueous solution), and hydrogen molecular sieves are prepared.
[0071] Carry out XRD test to the crystal that present embodiment obtains, obtain result as figure 2 . from figure 2 It can be seen that the test results have corresponding diffraction peaks, and the diffraction intensity is strong.
[0072] The chemical formula of the hydrogen-type molecular sieve prepared in this example is SiAl 0.006 B 0.020 o 2.039 .
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