A "one-pot" method for the preparation of metal-coordination polymer gels
A technology of metal coordination and polymer, which is applied in the field of preparing metal coordination polymer gel by "one pot method", which can solve the problems of limiting the potential application of intelligent polymer materials, and achieves a novel and simple method line effect
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Embodiment 1
[0026] a) Synthesis of azido compounds: polyethylene glycol (M n =2000, 10g) into a dry 250mL high-vacuum bottle, 150mL of dry anhydrous tetrahydrofuran was added into the bottle, and polyethylene glycol was dissolved at 40°C. After the system was cooled to room temperature, sodium hydride (NaH, 0.44 g, 60%) powder was added, and the reaction was stirred at room temperature overnight. 4 mL of epichlorohydrin (ECH) solution was added to the reaction system the next day. After reacting for 24 hours, the unreacted sodium hydride and by-product salts in the reaction system were removed through a neutral alumina column, and the obtained solution was rotovapped to remove tetrahydrofuran. The residual solution was precipitated in diethyl ether several times, filtered and dried in vacuo to obtain a white powder.
[0027] Put the 5g white solid powder prepared above, 3g sodium azide and 0.25g ammonium chloride in 40mL DMF / H 2 In a 100 mL round-bottomed flask of O (V / V=1:3) mixture, r...
Embodiment 2
[0034] The basic process is the same as in Example 1, the difference is that:
[0035] In step 1), the linear polyethylene glycol (M n =2000) is 0.2g (0.1mmol), 0.653g (0.18mmol) Add the solvent 1.5mL toluene to dissolve, and the components to be added are dissolved and dispersed evenly. After bubbling the reactor with nitrogen for 5 minutes, quickly add the cuprous chloride catalyst (0.014g, 0.14mmol) and the ligand N,N,N ',N",N"-Pentamethyldiethylenetriamine (0.00015mmol) was ultrasonically dispersed. Under the protection of nitrogen, the reaction temperature was 50°C, and the reaction time was 4h to form a coordination polymer gel network compound.
[0036] The rest are completely consistent with Example 1.
Embodiment 3
[0038] The basic process is the same as in Example 1, the difference is that:
[0039] In step 1), the linear polyethylene glycol (M n =2000) is 0.2g (0.1mmol), 0.726g (0.2mmol) Add the solvent 1mL tetrahydrofuran to dissolve. After the components added are dissolved and dispersed evenly, after bubbling the reactor with nitrogen for 5 minutes, quickly add the cuprous iodide catalyst (0.0304g, 0.16mmol) and the ligand N,N,N' , N”, N”-pentamethyldiethylenetriamine (0.0002mmol) was ultrasonically dispersed. Under the protection of nitrogen, the reaction temperature was 60°C, and the reaction time was 3h to form a coordination polymer gel network compound.
[0040] In step 2), the above-mentioned polymer network is taken out, put into an ethylene glycol solvent to remove unreacted reactants and metal catalysts remaining in the polymer network, and a regular coordination polymer network is obtained after drying.
[0041] The rest are completely consistent with Example 1.
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