A kind of ecr-40 molecular sieve and preparation method thereof
A technology of ECR-40 and molecular sieve, applied in the field of molecular sieve, can solve the problems of difficult industrial production, long crystallization time and high energy consumption, and achieve the effects of simple operation, short time consumption and low energy consumption
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Embodiment 1
[0062] A kind of preparation method of ECR-40 molecular sieve: pseudo-boehmite (Al 2 o 3 Mass percentage content 77%, aluminum source) and diethylethanolamine (mass percentage content 99%, R1) mix and stir, then add silica sol (SiO 2 Mass percent composition 30.04%, silicon source), after stirring for 10min, add phosphoric acid (H 3 PO 4 mass percent content 85%, phosphorus source), stirred for 15min, finally added water, hydrofluoric acid (HF mass percent composition 40%) and butyltrimethylammonium chloride (R2), after stirring for 30min, the gel Transfer to a stainless steel reaction kettle. Put the reaction kettle into an oven, and rotate and crystallize at 200°C for 48h. After the crystallization, the solid product was centrifuged, washed, and dried in air at 100°C to obtain an ECR-40 molecular sieve sample.
[0063] Dynamic crystallization is to stir the synthetic gel evenly through the rotation of the reactor body. The rotation of the reactor is driven by a motor pl...
Embodiment 2-12
[0070] Embodiment 2-12 concrete batching ratio and crystallization condition are different from embodiment 1, see table 2:
[0071] Table 2 Molecular sieve synthesis ingredients and crystallization conditions*
[0072]
[0073]
[0074] The substance type in Table 1 is A+B, and its corresponding molar content is a+b mol, which means that the molar content of A is amol, and the molar content of B is b mol.
[0075] The molecular sieve samples prepared in Examples 2-12 were analyzed by XRD, and the data results were close to those in Table 1, that is, the peak positions and shapes were the same, and the relative peak intensity of the peaks fluctuated in the range of ±10% according to the change of synthesis conditions, indicating that the prepared molecular sieves had ECR Features of -40 structures.
Embodiment 13
[0080] The CHN elemental analysis of the raw powder samples of Examples 1-12 shows that the C / N molar ratio fluctuates at 6.0±0.05. The bulk element composition of the molecular sieve product was analyzed by XRF, and the elemental composition of Al, P and Si in the molecular sieve product was determined. The CHN elemental analysis results were normalized with the inorganic element composition determined by XRF, and the anhydrous chemical composition of the molecular sieve product was obtained as Table 3.
[0081] The anhydrous chemical composition of table 3 molecular sieve product
[0082]
[0083]
[0084] Carry out to the molecular sieve former powder sample prepared by embodiment 1-12 13 C MAS NMR analysis, 13 In the C MAS NMR spectrum, there are carbon resonance peaks belonging to TMA and DEEA, but there is no characteristic carbon resonance peak belonging to BTMACl. Therefore, BTMAC1 is decomposed into TMA and enters into the prepared molecular sieve product.
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Abstract
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