Anti-humidity mof-5 compound, preparation method and application
A MOF-5 and compound technology, applied in the field of MOFs compounds, can solve the problems of easy moisture absorption and decomposition, restricting the practical application of MOF-5, etc., and achieve the effects of simple preparation method, significant moisture resistance, and high specific surface area.
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Embodiment 1
[0016] a. Mix 10mmol 1-(2-naphthyl)-1,3-butanedione (1-(naphthalen-2-yl) butane-1,3-dione), 10mmol carbon disulfide, 60mmol anhydrous potassium carbonate and 10mL N , N-dimethylformamide (DMF) was placed in a three-necked flask, stirred at room temperature for 30 minutes, added 20 mmol ethyl bromoacetate in an ice bath, and reacted for 6 hours in a water bath at 30°C;
[0017] b. Pour the reaction solution into ice water again, separate the solid, and recrystallize with ethyl acetate to obtain the recrystallized solid;
[0018] c. The obtained recrystallized solid is hydrolyzed in a solution of KOH-dissolved ethanol, the pH value is adjusted to 2, suction filtered and dried to obtain 3-(2-naphthyl)-4-methylthiophene[2 ,3-b]thiophene-2,5-dicarboxylic acid (3-(2-naphthyl)-4-methylthieno[2,3-b]thiophene-2,5-dicarboxylic acid);
[0019] d. Mix 0.1mmol 3-(2-naphthyl)-4-methylthiophene[2,3-b]thiophene-2,5-dicarboxylic acid with 0.6mmol zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O) Dissolve...
Embodiment 2
[0021] a. Mix 10mmol 1-(2-naphthyl)-1,3-butanedione (1-(naphthalen-2-yl) butane-1,3-dione), 10mmol carbon disulfide, 60mmol anhydrous potassium carbonate and 10mL N , N-dimethylformamide (DMF) was placed in a three-necked flask, stirred at room temperature for 30 minutes, added 20 mmol ethyl bromoacetate in an ice bath, and reacted for 4 hours in a water bath at 30°C;
[0022] b. Pour the reaction solution into ice water, separate the solid, and recrystallize with ethanol to obtain the recrystallized solid;
[0023] c. The obtained recrystallized solid is hydrolyzed in a solution of KOH-dissolved ethanol, the pH value is adjusted to 2, suction filtered and dried to obtain 3-(2-naphthyl)-4-methylthiophene[2 ,3-b]thiophene-2,5-dicarboxylic acid (3-(2-naphthyl)-4-methylthieno[2,3-b]thiophene-2,5-dicarboxylic acid);
[0024] d. Mix 0.1mmol 3-(2-naphthyl)-4-methylthiophene[2,3-b]thiophene-2,5-dicarboxylic acid with 0.6mmol zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O) Dissolved in 10mL N,...
Embodiment 3
[0026] a. Mix 10mmol 1-(2-naphthyl)-1,3-butanedione (1-(naphthalen-2-yl) butane-1,3-dione), 10mmol carbon disulfide, 60mmol anhydrous potassium carbonate and 10mL N , N-dimethylformamide (DMF) was placed in a three-necked flask, stirred at room temperature for 30 minutes, added 20 mmol ethyl bromoacetate in an ice bath, and reacted for 10 hours at 30°C in a water bath;
[0027] b. Pour the reaction solution into ice water again, separate the solid, and recrystallize with ethyl acetate to obtain the recrystallized solid;
[0028] c. Hydrolyze the resulting recrystallized solid in an aqueous solution of KOH, adjust the pH to 2, filter with suction and dry to obtain 3-(2-naphthyl)-4-methylthiophene[2,3 -b]thiophene-2,5-dicarboxylic acid (3-(2-naphthyl)-4-methylthieno[2,3-b]thiophene-2,5-dicarboxylic acid);
[0029] d. Mix 0.1mmol 3-(2-naphthyl)-4-methylthiophene[2,3-b]thiophene-2,5-dicarboxylic acid with 0.6mmol zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O) Dissolved in 10mL N,N-dimethy...
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