rho-sapo molecular sieve, its synthesis method and application
A RHO-SAPO, molecular sieve technology, applied in separation methods, molecular sieve catalysts, including molecular sieve catalysts, etc., can solve the problems of low crystallinity of molecular sieve products, increased cost, complexity of steps, and complicated steps, and achieve excellent gas adsorption and separation performance. , the effect of wide chemical composition range and good catalytic performance
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Embodiment 1
[0059] The molar proportions of each raw material, crystallization conditions and elemental composition of the samples are shown in Table 1. The specific batching process is as follows: 40.8g aluminum isopropoxide and 121.2g deionized water are mixed, and after stirring evenly, 36.9g of phosphoric acid (H 3 PO 4 Mass percentage composition 85%), then add dropwise 11.9g silica sol (SiO 2 Mass percentage composition 30.24%). 22.0g N, N'-dimethylethylenediamine was added to the previous mixture, and after stirring evenly, the resulting gel was transferred to a stainless steel reaction kettle containing a polytetrafluoroethylene kettle lining. The molar ratio of each component in the synthesis system is 2.5DMEDA:0.6SiO 2 : 1.0Al 2 o 3 : 1.6P 2 o 5 : 75H 2 O.
[0060] After putting the reactor into an oven, the temperature was programmed to rise to 180°C for dynamic crystallization for 48 hours. After the crystallization, the solid product was centrifuged, washed, and dri...
Embodiment 2-17
[0078] Samples of Examples 2-17 were prepared using the sources of aluminum, phosphorus and silicon described in Table 1 in a similar manner to Examples. The samples obtained in Examples 2-17 are analyzed by XRD, and the results are all close to the data in Table 2 of the samples obtained in Example 1, that is, the diffraction peak positions are the same, and the relative peak intensity of the diffraction peaks is in the range of ± 10% according to the change of synthesis conditions Inner fluctuations show that the samples obtained in Examples 2-17 all have the characteristics of the RHO-SAPO structure.
[0079] The inorganic and organic compositions of the samples obtained in Examples 2-17 were analyzed by XRF and CHN elements, and the element composition analysis results of the products are shown in Table 1.
[0080] Carry out to the former powder sample of embodiment 1-12 13 C MAS NMR analysis by reacting with N,N'-dimethylethylenediamine 13 The CMAS NMR standard spectrum...
Embodiment 18
[0082] The corresponding product that embodiment 1-4 obtains is used for CO as catalyst 2 Synthesis of cyclocarbonate by cycloaddition reaction with epichlorohydrin. The implementation details are as follows: 2 0.2 g of molecular sieve catalyst and 2 mL of epichlorohydrin were sequentially added into a 100 mL stainless steel autoclave. The reaction results are shown in Table 3.
[0083] Catalytic results of table 3 cycloaddition reaction a
[0084] catalyst
Conversion rates(%)
Cyclocarbonate Yield (%)
1
89.6
84.1
2
96.8
93.7
3
86.5
80.7
4
92.7
90.0
[0085] a reaction conditions: epichlorohydrin, 2mL; catalyst, 200mg; CO 2 Pressure, 8bar; temperature, 120°C; reaction time, 4h.
[0086] It can be seen from the results in Table 3 that all the synthesized RHO-SAPO molecular sieves have efficient catalytic effects on the reaction, high selectivity, mild reaction conditions, no need for any organic solvent ...
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