Preparation method and application of a zirconium-based metal-organic framework material
An organic framework and metal-based technology, applied in the field of adsorption and separation of nicotinamide and nicotinic acid, can solve the problems of template molecule elution, difficult separation, limited application, etc., and achieve the effect of high-efficiency separation
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Embodiment 1
[0031] Example 1 Synthesis of zirconium-based metal-organic framework material DUT-67
[0032] A method for preparing a zirconium-based metal-organic framework material (DUT-67), comprising the following steps:
[0033] S1. Mix dimethylformamide and N-methyl-2-pyrrolidone at a volume ratio of 1:1 to obtain 150mL mixed solution A; weigh 1.38g of zirconium chloride with a substance amount of 6mmol and a substance amount of 4mmol 0.66g of thiophenedicarboxylic acid, the zirconium chloride and thiophenedicarboxylic acid were added into the mixed solution A prepared together, and then 26.8mL of formic acid solution was added to the mixed solution to obtain the mixed solution B;
[0034] S2, the mixed solution B prepared in step S1 was stirred for 5 minutes, then transferred to a 100mL polytetrafluoroethylene-lined stainless steel autoclave, and heated at 120°C for 48 hours; after the reaction, the white solid was collected and used Washing with dimethylformamide and methanol, and ...
Embodiment 2
[0037] Example 2 Zirconium-based metal-organic framework material DUT-67 is used for adsorption and separation of niacin in a mixed solution of niacinamide and niacin
[0038] The zirconium-based metal-organic framework material DUT-67 prepared in Example 1 is used to adsorb nicotinamide and nicotinic acid at a pH value of 4.26 and 303K. The specific method is as follows:
[0039] Weigh 5 mg of sample DUT-67 and add it to 10 mL of a mixed solution of nicotinamide and nicotinic acid with an initial concentration of 5-500 mg / g. After ultrasonication for 10 seconds, transfer the mixed system to a constant temperature shaker for adsorption at 303K for 12 hours , the shaker speed is set to 155rpm. After the adsorption separation, filter with a microporous membrane with a pore size of 0.22 μm, collect the clear filtrate and use ultra-high performance liquid chromatography to determine the content of nicotinic acid and nicotinamide. The adsorption capacity is calculated using the eq...
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