Organic silicon micro-pore zeolite, synthesizing method and its application
A technology of microporous zeolite and synthesis method, applied in the directions of crystalline aluminosilicate zeolite, organic chemistry, chemical instruments and methods, etc., to achieve the effect of good technical effect
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Embodiment 1
[0024] Sodium aluminate (Al 2 o 3 42.0% by weight) 6.1 grams are dissolved in 288 grams of water, add 1.0 grams of sodium hydroxide to make it dissolve, then add 34.0 grams of hexahydropyridine under stirring, then add 60 grams of solid silicon oxide, and 5.5 grams of trimethylchlorosilane , the material ratio (molar ratio) of reactant is:
[0025] SiO 2 / Al 2 o 3 =40
[0026] NaOH / SiO 2 =0.025
[0027] Chlorotrimethylsilane / SiO 2 =0.05,
[0028] Hexahydropyridine / SiO 2 =0.50
[0029] h 2 O / SiO 2 =16
[0030] After the reaction mixture was evenly stirred, it was put into a stainless steel reaction kettle, and crystallized at 135° C. for 50 hours while stirring. After taking out, it is filtered, washed and dried. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 42.1.
[0031] After drying the sample was determined, its Si29 The NMR solid-state nuclear magnetic spectrum peak appears at 15.1ppm. Its X-ray diffraction data are shown in Tabl...
Embodiment 2
[0035] Sodium aluminate (Al 2 o 3 42.0% by weight) 8.0 grams are dissolved in 360 grams of water, add 4.0 grams of sodium hydroxide to make it dissolve, then add 34.0 grams of hexahydropyridine under the situation of stirring, then add 150 grams of silica sol (silicon oxide content 40% by weight), Dimethyldichlorosilane 3.9 grams, the material ratio (mol ratio) of reactant is:
[0036] SiO 2 / Al 2 o 3 =30
[0037] NaOH / SiO 2 =0.05
[0038] Dimethyldichlorosilane / SiO 2 =0.03,
[0039] Hexahydropyridine / SiO 2 =0.40
[0040] h 2 O / SiO 2 =20
[0041] After the reaction mixture was stirred evenly, it was put into a stainless steel reaction kettle, and crystallized at 150° C. for 55 hours while stirring. After taking out, it is filtered, washed and dried. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 28.6.
[0042] After drying the sample was determined, its Si 29 NMR solid-state nuclear magnetic spectrum peaks appear at 5.7ppm and -16.4p...
Embodiment 3
[0046] Dissolve 3.0 grams of aluminum oxide in 450 grams of water, add 16.0 grams of sodium hydroxide to dissolve it, then add 34.7 grams of hexamethyleneimine while stirring, then add 60 grams of solid silicon oxide, dimethyldiethyl Oxygensilane 5.9 grams, the material ratio (mol ratio) of reactant is:
[0047] SiO 2 / Al 2 o 3 =30
[0048] NaOH / SiO 2 =0.2
[0049] Dimethyldiethoxysilane / SiO 2 =0.04,
[0050] Hexamethyleneimine / SiO 2 =0.35
[0051] h 2 O / SiO 2 =25
[0052] After the reaction mixture was stirred evenly, it was put into a stainless steel reaction kettle, and crystallized at 145° C. for 70 hours while stirring. After taking out, it is filtered, washed and dried. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 30.1.
[0053] After drying the sample was determined, its Si 29 NMR solid-state nuclear magnetic spectrum peaks appeared at 5.8ppm and -15.9ppm. Its X-ray diffraction data are shown in Table 3.
[0054] table 3
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