Preparation method and application of nano SSZ-13 molecular sieve
A molecular sieve and nanotechnology, applied in molecular sieve catalysts, nanotechnology, chemical instruments and methods, etc., can solve the problems of large dosage, unfavorable diffusion, no substantial progress, etc., and achieve the effect of high yield
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Embodiment 1
[0069] Example 1 Sample 1 # preparation
[0070] 0.16g aluminum hydroxide (Al(OH) 3 ≥98wt%) was dissolved in 2.54g (25wt%) N,N,N-trimethyladamantanium aqueous solution, 4.74g deionized water was added, and then 5.90g silica sol (SiO 2 : 30.54 wt%) was added dropwise to the above obtained solution, and continued to stir rapidly for 3 h at room temperature until the mixture was uniform to obtain the initial gel mixture A. The molar ratio of each raw material in the initial gel mixture A is as follows: 30SiO 2 : 2.0Al(OH) 3 : 3TMAdaOH: 597H 2 O. The initial gel mixture A was transferred to a stainless steel reactor with a polytetrafluoroethylene lining, and after dynamic crystallization at 120° C. for 12 h, it was cooled to room temperature to obtain a seed crystal solution B.
[0071] First, 0.34g sodium metaaluminate and 0.066g sodium hydroxide were dissolved in 10.0g deionized water, then 3.13g white carbon black was gradually added to the above obtained clear solution u...
Embodiment 2
[0073] Example 2 Sample 2 # ~10 # preparation
[0074] Sample 2 # ~10 # The types of raw materials, raw material ratio, and crystallization conditions are shown in Table 1, and the batching process is the same as that of Sample 1 in Example 1. # preparation.
[0075] Table 1 Molecular sieve synthesis ingredients and crystallization conditions
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[0078] a : In the initial gel mixture A, the amount of silicon source added is the same as that of SiO 2 The number of moles of aluminum source; the amount of aluminum source added in Al 2 O 3 The number of moles of the template agent R is calculated by the number of moles of the template agent R; the amount of water added is calculated by the number of moles of the water itself.
[0079] b : In the initial gel mixture C, the amount of silicon source added is the same as that of SiO 2 The number of moles of aluminum source; the amount of aluminum source added in Al 2 O 3 The added amount of alkali so...
Embodiment 3
[0084] Example 3 Sample 1 # ~10 # and comparative sample 1 # ~2 # XRD analysis of sample 1 using X-ray diffraction method # ~10 # and comparative sample 1 # ~2 # phase analysis.
[0085] for sample 1 # ~10 # and comparative sample 1 # ~2 # Structural characterization using XRD, typical representatives such as figure 1 Medium sample 1 # XRD pattern of figure 1 is the X-ray diffraction pattern of sample 1#, the results show that sample 1 prepared in Examples 1 and 2 # ~10 # All are SSZ-13 molecular sieves with high purity and high crystallinity. Sample 2 # ~10 # The XRD results of the figure 1 close, that is, the position and shape of the diffraction peaks are basically the same, and the relative peak intensity fluctuates within the range of ±5% depending on the synthesis conditions, indicating that sample 1 # ~10 # It has the characteristics of SSZ-13 structure and no impurities. Comparative Sample 1 # and comparative sample 2 # The XRD patterns of the ...
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