A kind of crystalline porous framework material and its preparation method and application
A porous skeleton and crystallization technology, applied in chemical instruments and methods, other chemical processes, alkali metal compounds, etc., can solve the problems of low adsorption capacity and low selectivity
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[0033] The invention provides a method for preparing a crystalline porous framework material, comprising the following steps:
[0034] Using scandium ions and 4-aminophenylacetic acid to conduct a coordination reaction in N,N-dimethylformamide solution to obtain scandium ligand blocks;
[0035] Using the scandium ligand block, 2,4,6-triformaldehyde phloroglucinol and p-phenylenediamine to perform Schiff base reaction in an organic solvent to obtain a scandium-containing crystalline porous framework material;
[0036] The scandium-containing crystalline porous framework material is washed and dried in sequence to obtain a crystalline porous framework material.
[0037] The invention utilizes scandium ions and 4-aminophenylacetic acid to carry out coordination reaction in N,N-dimethylformamide solution to obtain scandium ligand block.
[0038] In the present invention, unless otherwise specified, the raw materials used are conventional commercially available products in this fi...
Embodiment 1
[0051] Weigh 259.3mg of scandium chloride hexahydrate and 453.5mg of 4-aminophenylacetic acid and dissolve in 2mL of N,N-dimethylformamide solution (volume concentration is 80%), after stirring at room temperature for three hours, under vacuum condition, 60 °C, drain the organic solvent to obtain a triangular scandium ligand block.
[0052] Add 25.2 mg 2,4,6-triformaldehyde phloroglucinol, 15 mg p-phenylenediamine and 5.9 mg triangular scandium ligand block (molar ratio: 2:27:20) into the saddle bottle, and then add 0.6 mL Mesitylene and 0.6mL dioxane, ultrasonic the mixed system for 10min to ensure uniform dispersion, then add 0.6mL 3mol / L acetic acid solution. Freeze the mixed system under the condition of 77K liquid nitrogen for 5 minutes, vacuumize it with an oil pump for 2 minutes, then pour nitrogen into the saddle bottle to thaw the system, then freeze the system under the condition of 77K liquid nitrogen for 5 minutes, and seal the tube under the condition of vacuumizi...
Embodiment 2
[0055] In the saddle bottle, add 25.2mg 2,4,6-triformaldehyde phloroglucinol, 15.6mg p-phenylenediamine, the triangular scandium ligand block that 11.8mg embodiment 1 prepares (molar ratio is: 4:24: 20), then add 0.6mL of mesitylene and 0.6mL of dioxane, and then sonicate the mixed system for 10min to ensure uniform dispersion, then add 0.6mL of 3mol / L acetic acid solution, and freeze the mixed system for 5min under the condition of 77K liquid nitrogen , use an oil pump to evacuate for 2 minutes, then pour nitrogen into the saddle bottle and thaw the system, then freeze the system for 5 minutes under the condition of 77K liquid nitrogen, seal the tube under the condition of oil pump vacuum, and put the sealed tube at 120°C Oven, take it out after three days, open the tube, filter with suction, and wash the obtained solid with N,N-dimethylformamide, 1mol / L sodium hydroxide solution, 1mol / L hydrochloric acid, water, and acetone. The washing time is 2 hours, washed twice, and the...
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