Synthetic method of polynitrogen azole zinc/cadmium framework material
A frame material, polyazole zinc technology, applied in the direction of zinc organic compounds, cadmium organic compounds, etc., can solve the problems of high cost, difficulty in activation, low reaction yield, etc., and achieve rapid reaction, accelerated reaction speed, and post-processing of products simple effect
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[0035] Example 1 Efficient preparation of a small amount of MAF-4 at room temperature
[0036] In a 10mL ground round bottom flask, add 99.4mg Zn(OH) 2 Or 81.4mg ZnO (1.0mmol), 164.2mg Hmim (2.0mmol), 5.0mL reaction solution, capped, stirred at room temperature for 24h and then filtered. The filter cake was washed 3 times with methanol and dried at 120°C to obtain the product with a yield of about 95%. In the initial synthesis, the reaction solution consisted of 4.0 mL of methanol and 1.0 mL of 25 wt% ammonia. The filtrate obtained after each synthesis can be directly used as the reaction solution for the next synthesis, and can be recycled at least 5 times without reducing the purity and yield of the product.
Example Embodiment
[0037] Example 2 Efficient preparation of large amounts of MAF-4 at room temperature
[0038] Add 99.4g Zn(OH) in a 1000mL ground round bottom flask 2 Or 81.4g ZnO (1.0mol), 164.2g Hmim (2.0mol), 500mL reaction solution, capped, stirred vigorously at room temperature for 24h, and then filtered. The filter cake was washed 3 times with methanol and dried at 120°C to obtain the product with a yield of about 95%. In the initial synthesis, the reaction solution consisted of 400 mL of methanol and 100 mL of 25 wt% ammonia. The filtrate obtained after each synthesis can be directly used as the reaction solution for the next synthesis, and can be recycled at least 5 times without reducing the purity and yield of the product.
Example Embodiment
[0039] Example 3 Rapid preparation of MAF-4 by microwave heating
[0040] Add 99.4mg Zn(OH) to 60mL microwave reactor with PTFE substrate 2 Or 81.4mg ZnO (1.0mmol), 164.2mg Hmim (2.0mmol), 5.0mL reaction solution, stir at room temperature for a few minutes, seal, microwave heating to 40°C for 1.5h, cool to room temperature and filter. The filter cake was washed 3 times with methanol and dried at 120°C to obtain the product with a yield of about 95%. In the initial synthesis, the reaction solution consisted of 4.0 mL of methanol and 1.0 mL of 25 wt% ammonia. The filtrate obtained after each synthesis can be directly used as the reaction solution for the next synthesis, and can be recycled at least 5 times without reducing the purity and yield of the product.
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