Inorganic microporous nickle and cobalt phosphate molecular sieves materials and their synthesis method
A nickel-cobalt phosphate, molecular sieve-like technology, used in molecular sieve catalysts, molecular sieves and alkali-exchanged phosphates, chemical instruments and methods, etc., can solve the problems of high crystallization temperature, unfavorable industrial production, long crystallization time, etc. Synthesis conditions, the effect of shortening the synthesis time
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Embodiment 1
[0023] Example 1Co mole fraction is 31% CoVSB-1
[0024] Dissolve 3.23g of nickel chloride and 1.38g of cobalt chloride in 14mL of distilled water, and add 2.24mL of orthophosphoric acid dropwise while stirring; then, add 0.97mL of hydrofluoric acid; finally add 1.18mL of ethylenediamine template, and stir for 0.5 After mixing evenly for 1 hour, the mixed material was moved into a polytetrafluoroethylene-lined stainless steel synthesis kettle and sealed, and the filling capacity was 70% (V). Crystallize at 170°C for 2 hours under autogenous pressure, wash the solid product three times with deionized water, and dry it in air at 60°C to obtain CoVSB-1. The XRD analysis is shown in Figure 2. Its unit cell parameters are: a=b=19.935(3) Ȧ; c=5.0476(1) Ȧ; V=1737.28 Ȧ 3 . The unit cell parameters of VSB-1 reported in the literature a=b=19.834(1) Ȧ; c=5.0379(1) Ȧ; V=1716.33 Ȧ 3 Compared with that, it has increased, indicating that cobalt atoms have entered the framework. The main ...
Embodiment 2
[0025] Embodiment 2Co mole fraction is 52% CoVSB-1
[0026] In Example 1, (3.23g NiCl 2 ·6H 2 O+1.38g CoCl 2 ·6H 2 O) was changed to (2.31g NiCl 2 ·6H 2 O+2.30g CoCl 2 ·6H 2 O), the rest of the synthesis conditions and synthesis steps are unchanged, the unit cell parameters of the CoVSB-1 product obtained are: a=b=19.960 (2) Ȧ; c=5.053 (1) Ȧ; V=1743.49 Ȧ 3 . The main component content of this product is: Co (22.06wt%), Ni (20.34wt%), P (14.32wt%), calculate its cobalt mole fraction [n Co / (n Co +n Ni )] at 52%.
Embodiment 3
[0027] Embodiment 3 Co mole fraction is 52% CoVSB-1
[0028] In Example 2, the components of the reaction mixture and other synthesis steps are kept unchanged, the crystallization temperature is changed to 150° C., and the crystallization time is changed to 4 hours, and the product of Example 2 can also be prepared.
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