Method of utilizing one-pot reaction to prepare metal coordination polymer gel
A metal coordination and polymer technology, which is applied in the field of preparing metal coordination polymer gel by "one-pot method", can solve the problems of limiting the potential application of intelligent polymer materials, and achieves a novel and simple method. row 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 that in Example 1, except that:
[0035] In step 1), the azide-terminated linear polyethylene glycol (M n =2000) is 0.2g (0.1mmol), 0.653g (0.18mmol) Add solvent 1.5mL toluene to dissolve, the components to be added are dissolved and dispersed uniformly, the reactor is bubbled with nitrogen gas for 5 minutes, then cuprous chloride catalyst (0.014g, 0.14mmol) and ligand N,N,N are added quickly. ',N",N"-pentamethyldiethylenetriamine (0.00015 mmol) was sonicated for uniform dispersion. Under the protection of nitrogen, the reaction temperature was 50 °C, and the reaction time was 4 h to form a coordination polymer gel network compound.
[0036] The rest are exactly the same as in Example 1.
Embodiment 3
[0038] The basic process is the same as that in Example 1, except that:
[0039] In step 1), the azide-terminated linear polyethylene glycol (M n =2000) is 0.2g (0.1mmol), 0.726g (0.2mmol) Add solvent 1mL of tetrahydrofuran to dissolve, and the components to be added are dissolved and dispersed uniformly. After bubbling the reactor with nitrogen for 5 minutes, cuprous iodide catalyst (0.0304g, 0.16mmol) and ligand N,N,N' are quickly added. ,N",N"-pentamethyldiethylenetriamine (0.0002mmol) was sonicated to make it uniformly dispersed. Under the protection of nitrogen, the reaction temperature was 60℃, 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 exactly the sam...
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