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

Inactive Publication Date: 2015-03-11
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chemically cross-linked polymer gel materials prepared by the traditional click method cannot meet the requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention discloses a method of utilizing a one-pot reaction to prepare metal coordination polymer gel. The method comprises the following step: using the one-pot reaction in the metal coordination chemistry and click chemistry to enable an organic compound and a polydentate ligand organic compound to carry out a click reaction under the action of a metal catalyst, so as to generate the metal coordination polymer gel, wherein the organic compound comprises two or more multiterminal azido groups; the polydentate ligand organic compound at least comprises one terminated alkynyl. The method disclosed by the invention is simple to operate, accessible in reaction materials, moderate in reaction conditions, and high in reaction speed; the metal coordination polymer gel prepared by the method disclosed by the invention has the advantages of regular structure, external stimuli response, self-repairing, unique photoelectromagnetic property and the like.

Description

technical field [0001] The invention belongs to the field of polymer synthesis methods, and relates to a method for preparing a metal coordination polymer gel by using a "one-pot method". Background technique [0002] The metal coordination polymer gel is formed by containing water or organic solvents to form a multidimensional network structure, and the connection of the polymer main chain or polymer functional groups is provided by reversible unstable metal coordination interactions. Compared with traditional chemically cross-linked gels, metal-coordination polymer gels have new chemical and physical properties under different circumstances by introducing ligands into the polymer architecture, such as, Catalytic, luminescent, photoelectric, redox, magnetic and other properties. It can be used to design new sensing and magnetic or emission and catalytic functional materials. [0003] "Click chemistry", especially the cycloaddition reaction (CuAAC) catalyzed by Cu(I) compo...

Claims

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Application Information

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IPC IPC(8): C08G73/06
Inventor 付国东李扬姚芳
Owner SOUTHEAST UNIV
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