a zn based 5 Copolymerized monolithic column of metal clusters and its preparation method and application
A monolithic column and metal cluster technology, which is applied in the fields of analytical chemistry and environmental analysis, can solve the problem of undiscovered coordination clusters for adsorption and removal of environmental pollutants, and achieve the effect of simple method, high sensitivity and simple synthesis steps
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Embodiment 1
[0029] Example 1 Based on Zn 5 Preparation of Coopolytic Cumulative Columns of Metal Clusters
[0030] First, such as figure 1 As shown, Zn based on this embodiment 5 The method of preparing the metal cluster of the column is:
[0031] First step, Zn 5 Preparation of a coordination cluster. The specific method is as follows:
[0032] Contain Zn (NO 3 ) 2 · 6h 2 O (150mg, 0.5mmol), h 4 L (294 mg, 1.0 mmol), a 25 mL of the 25 ml of the polytetrafluoroethylene liner of Triethylamine (0.15 mL) 1: 1 of MeOH and water (16 mL) mixture. The reactor was heated at 140 ° C for 24 hours. Then the autoclave is 10 ° C · h -1 The rate is cooled to room temperature. Collect Zn 5 Yellow block crystals, h 2 O wash and dried in air (based on Zn based on the yield of about 80%).
[0033] The second step, Zn 5 -COC 2 Hide 5 Preparation. The specific method is as follows:
[0034] Weigh 0.5g Zn 5 The coordination cluster is sued in DMF, adding equimolar triethylamine, and adding a benzene phenol-added a...
Embodiment 2
[0037] First step, Zn 5 Preparation of a ligating cluster is in Example 1.
[0038] The second step, Zn 5 -COC 2 Hide 5 Preparation: Weigh 0.5g Zn 5 Composition cluster is in DMF, triethylamine is added (Zn 5 The molar ratio ratio of the tissue cluster and triethylamine is 1: 3), and an osne phenol-polymerized agent was added, and an excess (105% -110%) acryloyl chloride was added dropwise at room temperature / frozen. After the reaction is complete, excess ultrapure water is added to recrystallize, and the obtained yellow crystal is dried.
[0039] The third step, Zn 5 -COC 2 Hide 5 -CO-EGDMA copolymer column preparation: 8mg Zn 5 -COC 2 Hide 5 And 80 mg EGDMA (crosslinking agent) was dissolved in 800 μl of PEG 200 or methanol solvent, 2 mg of AIBN initiator, ultrasonic dissolution, to obtain an organic prepolymer solution. A 100 μl of the organic prepolymer solution was taken, and the reaction container was reacted at 70 ° C for 10 h, and finally Zn was obtained. 5 -COC 2 Hide 5...
Embodiment 3
[0041] First step, Zn 5 Preparation of a ligating cluster is in Example 1.
[0042] The second step, Zn 5 -COC 2 Hide 5 Preparation: Weigh 0.5g Zn 5 Composition cluster is in DMF, triethylamine is added (Zn 5 The molar ratio of the ligand cluster and triethylamine is 1: 3), and the phenol-added agent to prevent self-polymerization, add excess (105% -110%) acryloyl chloride, reaction 3 under room temperature / frozen. -4h. After the reaction is complete, excess ultrapure water is added to recrystallize, and the obtained yellow crystal is dried.
[0043] The third step, Zn 5 -COC 2 Hide 5 Preparation of the - CO-EGDMA Copolymer Column. The specific method is as follows: 10 mg of Zn5-COC2H5 and 40 mg EGDMA is dissolved in 400 μl of methanol, and a 3 mg Aibn initiator is added, and an ultrasonic dissolved organic prepolymer solution is dissolved. A 100 μl of the organic prepolymer was taken to react at 90 ° C for 16 h at 90 ° C, and finally the Zn5-COC2H5-Co-EGDMA copolymerization int...
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