A kind of metal organic framework material and its preparation method and application
A metal-organic framework and methanol technology, applied in the field of transition metal complex materials, can solve the problems of harsh reaction conditions, expensive catalyst costs, and low catalytic yields, and achieve easy industrialization, reduced production costs, and simple preparation processes Effect
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Embodiment 1
[0038] Embodiment 1: {Fe(BIm)(OH) CH 4 O·2H 2 Synthesis of O}n
[0039] (1) Preparation of BIm: Weigh 1.001g of hydrazine hydrate (20mmol) and dissolve it in 10mL of methanol, and weigh 3.844g (40mmol) of 4-imidazole formaldehyde in a flask and add 30mL of methanol, and drop the methanol solution of hydrazine hydrate Add it to a flask, stir and reflux at 65°C overnight to form a pale yellow precipitate, filter, wash with methanol, and dry to obtain the BIm;
[0040] (2) BIm and 2mmol ferrous trifluoromethanesulfonate prepared by 2mmol step (1) are added in the 350mL high-pressure bottle, then add the mixed solution (125mL, 1:4, v / v) of DMF and methanol, to Nitrogen gas was introduced into the mixed solution for 20 minutes, sealed and placed in an oven at a constant temperature of 110°C for heating for 72 hours. After cooling, the crystals were collected, washed with acetonitrile, and dried to obtain the {Fe(BIm)(OH)·CH 4 O·2H 2 O}n, the yield was 80%.
[0041] {Fe(BIm)(OH...
Embodiment 2
[0053] Embodiment 2: {Fe(BIm)(OH) CH 4 O·2H 2 Synthesis of O}n
[0054] (1) Preparation of BIm: Weigh 1.001g of hydrazine hydrate (20mmol) and dissolve it in 10mL of methanol, and weigh 3.844g (40mmol) of 4-imidazole formaldehyde in a flask and add 30mL of methanol; drop the above-mentioned methanol solution of hydrazine hydrate Add it to a flask, stir and reflux at 60°C overnight to form a light yellow precipitate, filter, wash with methanol, and dry to obtain the BIm;
[0055] (2) Add 2mmol of BIm prepared in Example 2 and 2mmol of ferrous trifluoromethanesulfonate to a 350mL high-pressure bottle, then add a mixed solution of DMF and methanol (120mL, 1:3, v / v), and mix Nitrogen was introduced into the solution for 20 minutes, sealed and placed in an oven at a constant temperature of 110°C for heating for 72 hours. After cooling, the crystals were collected, washed with acetonitrile, and dried to obtain the {Fe(BIm)(OH)·CH 4 O·2H 2 O}n, the yield was 65%.
[0056] After ...
Embodiment 3
[0058] Embodiment 3: {Fe(BIm)(OH) CH 4 O·2H 2 Synthesis of O}n
[0059] (1) Preparation of BIm: Weigh 1.001g of hydrazine hydrate (20mmol) and dissolve it in 10mL of methanol, and weigh 3.844g (40mmol) of 4-imidazole formaldehyde in a flask and add 30mL of methanol; drop the above-mentioned methanol solution of hydrazine hydrate Add it to a flask, stir and reflux at 70°C overnight to form a light yellow precipitate, filter, wash with methanol, and dry to obtain the BIm;
[0060](2) Add 3mmol of BIm prepared in Example 3 and 2mmol of ferrous trifluoromethanesulfonate to a 350mL high-pressure bottle, then add a mixed solution of DMF and methanol (125mL, 1:4, v / v), and mix Nitrogen was introduced into the solution for 20 minutes, sealed and placed in an oven at a constant temperature of 110°C for heating for 72 hours. After cooling, the crystals were collected, washed with acetonitrile, and dried to obtain the {Fe(BIm)(OH)·CH 4 O·2H 2 O}n, the yield was 75%.
[0061] After N...
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