A kind of method for preparing keggin polycation chloride crystal
A chloride, polyaluminum chloride technology, applied in chemical instruments and methods, crystal growth, single crystal growth and other directions, can solve the problems of difficult preparation of Keggin structure polycationic chloride crystals, and achieve the effect of simple preparation
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Embodiment 1
[0030] (1) PAC solid-phase synthesis reaction: at 80°C, slowly dissolve 3.7g of aluminum powder into 87ml of C=5mol / lAlCl 3 In the solution, the degree of alkalization was set to 0.8. After all the aluminum powder had reacted, the solution was filtered and evaporated at room temperature to obtain a solid that was washed with isopropanol to obtain a PAC solid, which was dried in an oven for use.
[0031] (2) Keggin-GaAl 12 Chloride synthesis reaction: Dissolve 4.5g of the above-mentioned PAC solid in 25ml of methanol, sonicate in an ultrasonic instrument for about 10min, and after the solid is completely dissolved, dissolve the solid GaCl 3 Dissolve in the solution to make n(Al) / n(Ga)=1.6, evaporate and crystallize at room temperature. 15 days to get pure Keggin-GaAl 12 Chloride crystals.
Embodiment 2
[0033] (1) PAC solid-phase synthesis reaction: 2.6g of pure Al(OH) 3 Slowly dissolve in 12ml C=5.1mol / l HCl solution, after it is completely dissolved, add 50ml of water to make the degree of alkalization 1.2. Under the condition of 80°C, after all the solids have reacted, the solution was filtered and evaporated at room temperature, and the obtained solids were washed with isopropanol to obtain PAC solids, which were dried in an oven for future use.
[0034] (2) Keggin-GaAl 12Chloride synthesis reaction: Dissolve 4.5g of PAC solid in 25ml of methanol, sonicate in an ultrasonic instrument for about 10min, after the solid is completely dissolved, dissolve the solid GaCl 3 Dissolve in the solution to make n(Al) / n(Ga)=6.4, evaporate and crystallize at room temperature. 15 days to get pure Keggin-GaAl 12 Chloride crystals.
Embodiment 3
[0036] (1) PAC solid-phase synthesis reaction: at 80°C, slowly add 19.3g of aluminum powder to 103ml of C=5.3mol / l AlCl 3 In the solution, the degree of alkalinity was set to 1.3. After all the aluminum powder had reacted, the solution was filtered and evaporated at room temperature to obtain a solid that was washed with isopropanol to obtain a PAC solid, which was dried in an oven for future use.
[0037] (2) Keggin-GaAl 12 Chloride synthesis reaction: Dissolve 4.5g of PAC solid in 25ml of methanol, sonicate in an ultrasonic instrument for about 10min, after the solid is completely dissolved, dissolve the solid GaCl 3 Dissolve in the solution to make n(Al) / n(Ga)=26, evaporate and crystallize at room temperature. 15 days to get pure Keggin-GaAl 12 Chloride crystals.
[0038] In the above cases, single crystal particles with a size of about 3mm and polycrystalline powder can be obtained. The analysis results are shown in the attached figure 1 , 2, 3.
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