Method for preparing rare earth-containing MCM-49 molecular sieve
A MCM-49, molecular sieve technology, applied in molecular sieve compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of difficult exchange, large radius of hydrated ions, unsatisfactory exchange product uniformity, etc. Stability, the effect of reducing the cost of synthesis
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Embodiment 1
[0015] Select the molar ratio of the reaction mixture as: SiO 2 / Al 2 o 3 =30,OH - / SiO 2 =0.20, (HMI+CHA) / SiO 2 = 0.3, La 2 o 3 / Al 2 o 3 =0.015,H 2 O / SiO 2 =32. The operation steps are: under the condition of constant stirring, 5.1g of sodium metaaluminate solution [containing 15.0% (w) Al 2 o 3 , 27.0% (w) NaOH, the same below], 0.44g sodium hydroxide (96% NaOH), 2.3g hexamethyleneimine, 4.3g cyclohexylamine, 56.0g silica sol [containing 24.1% (w) SiO 2 , the same below], 0.1g La(NO 3 ) 3 ·6H 2 O and 84.1 g of deionized water were sequentially added into a stainless steel reactor and mixed evenly, then the reactor was sealed and crystallized at 166° C. for 48 h. After the reaction kettle is cooled, the solid and the mother liquor are centrifuged, the solid is washed with deionized water to pH 8-9, and dried at 100°C in the air for 8 hours to obtain the original molecular sieve powder, which is tested by powder X-ray diffraction (XRD) The result is MCM-49 mo...
Embodiment 2
[0017] In embodiment 1, the add-on of sodium metaaluminate solution is changed into 255g, the add-on of sodium hydroxide is changed into 22g, the add-on of hexamethyleneimine is changed into 115g, and the add-on of cyclohexylamine is changed into 215g, the addition of silica sol is changed into 2800g, La(NO 3 ) 3 ·6H 2 The addition of O was changed to 5g, the addition of deionized water was changed to 4204g, and the raw material composition was unchanged. The raw material mixture was first aged at 40°C for 12 hours, and then crystallized at 172°C for 38 hours. The product was MCM-49 molecular sieve, and the La in the molecular sieve was measured by XRF. 2 o 3 The weight content is 0.21%.
Embodiment 3
[0019] In embodiment 1, the add-on of sodium hydroxide is changed into 0.67g, the add-on of hexamethyleneimine is changed into 3.5g, the add-on of cyclohexylamine is changed into 6.5g, the add-on of silica sol is changed into 28.0g, La(NO 3 ) 3 ·6H 2 The addition of O was changed to 0.13g, the addition of deionized water was changed to 97.3g, and the rest of the raw materials were unchanged; the molar ratio of the reaction mixture was: SiO 2 / Al 2 o 3 =15,OH - / SiO 2 =0.45, (HMI+CHA) / SiO 2 = 0.9, La 2 o 3 / Al 2 o 3 =0.02,H 2 O / SiO 2 =60. The raw material mixture was first aged at 85°C for 6 hours, and then crystallized at 148°C for 70 hours. The product was MCM-49 molecular sieve, and the La in the molecular sieve was measured by XRF. 2 o 3 The weight content is 0.28%.
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