A kind of coordination polymer microsphere and its preparation method and hydrogen storage application
A technology of coordination polymers and microspheres, applied in the production of hydrogen, etc., can solve the problems of low thermal stability and achieve the effects of easy control of reaction conditions, low energy consumption, and controllable particle shape
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[0032] The preparation method of the coordination polymer microspheres of the present invention is: using 1,1'-ferrocenedicarboxylic acid and 4,4'-bipyridine as ligands, mixing and dissolving them in N,N '-Dimethylformamide (DMF), add metal salt and mix well, the molar ratio of metal salt and 1,1'-ferrocenedicarboxylic acid is 1:1, heat in a blast drying oven at 120-180 ℃ reaction 12h. After the reaction is finished, cool the reactor to room temperature, and then obtain the reaction solution in the upper layer by centrifugation. The reaction solution obtained is obtained by rotary evaporation to obtain a solid product, which is dried in a vacuum oven to obtain coordination polymer microspheres. .
[0033] The coordination polymer microsphere prepared by the present invention has a structural formula of:
[0034] ;
[0035] Wherein, M is Mn, Co or Zn. The molecular weight range is 200-800.
[0036] The coordination polymer microspheres constructed based on two kinds of l...
Embodiment 1
[0063] Taking Mn-CPM as an example, its specific preparation method is as follows: 0.3981 g (2 mmol) MnCl 2 4H 2 O,, 0.5480 g (2 mmol) 1,1’-ferrocenedicarboxylic acid (Fc(COOH) 2 ) and 0.3120 g (2 mmol) of 4,4'-bipyridine were dissolved in a mixed solvent of 8 mL N,N'-dimethylformamide (DMF) and 8 mL deionized water, and then the solution was added to the 23 mL polytetrafluoroethylene-lined stainless steel reaction kettle, mix evenly, seal the reaction kettle and put it in the oven. o C / min heat up to 120 o C, after constant temperature reaction for 12 h, it was naturally cooled to room temperature. Centrifuge to obtain a precipitate, and then use DMF and CHCl 3 Repeated washing several times (sonication for 10 min each time, and then centrifugation at 3000 r / min and 2000 r / min respectively), until the supernatant liquid was clear liquid, after removing the clear liquid, the obtained precipitate was separated at 40 o C for 24 h under vacuum.
[0064] from figure 1 From ...
Embodiment 2
[0066] Taking Co-CPM as an example, its specific preparation method is as follows: 0.4278 g (1.8 mmol) CoCl 2 4H 2 O, 0.4938 g (2 mmol) 1,1’-ferrocenedicarboxylic acid (Fc(COOH) 2 ) and 0.2813 g (1.8 mmol) of 4,4'-bipyridine were dissolved in a mixed solvent of 8 mL N,N'-dimethylformamide (DMF) and 8 mL deionized water, and the solution was added to the 23 mL polytetrafluoroethylene-lined stainless steel reaction kettle, mix evenly, seal the reaction kettle and put it in the oven. o C / min heat up to 125 o C, after constant temperature reaction for 12 h, it was naturally cooled to room temperature. Centrifuge to obtain a precipitate, and then use DMF and CHCl 3 Repeated washing several times (sonication for 10 min each time, and then centrifugation at 3000 r / min and 2000 r / min respectively), until the supernatant liquid was clear liquid, after removing the clear liquid, the obtained precipitate was separated at 40 o C for 24 h under vacuum.
[0067] from figure 1 From C-...
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