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Preparation method of super-molecule metal gel

A metal gel and supramolecular technology, applied in zinc organic compounds, cadmium organic compounds, lead organic compounds, etc., can solve problems such as insufficient coordination bonds

Inactive Publication Date: 2012-07-04
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the supramolecular gels currently studied use hydrogen bonding or molecular packing, while coordination bonds, which are equally important in supramolecular chemistry, are far from being used in gel synthesis.

Method used

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  • Preparation method of super-molecule metal gel
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  • Preparation method of super-molecule metal gel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1. Preparation of Gel G1

[0023] (1) Preparation of compound L1 (N,N'-dicarboxymethyl-2-ethylbenzimidazole):

[0024] Take 4.00g (42mmol) of chloroacetic acid in a three-necked round bottom flask equipped with a reflux condenser, and adjust the pH to 8~10 with NaOH solution, then add 3.49g (14mmol) of 2-ethylbenzimidazole and heat to reflux During the period, the pH value was continuously adjusted to maintain the pH value of the system at 8~10, until the pH value was stable, then continue to reflux for 30 minutes, cool, and add concentrated hydrochloric acid to adjust the pH=2~3, and a large amount of white precipitate was formed. Let it stand overnight, filter with suction, wash with distilled water and acetone 3 times, and then recrystallize with water to obtain a white solid.

[0025] Melting point: 279~281°C, yield: 70%. 1 H NMR (400MHz D 2 O, ppm) δ: 7.45~7.56 (m, 4H, ), 4.65~5.01 (d, 4H), 3.03~3.05 (d, 2H), 1.10~1.14 (t, 3H), IR (KBr) v: 1730 (C=O), 1676 (C=O)...

Embodiment 2

[0028] Example 2. Preparation of Gel G2

[0029] (1) Preparation of compound L2 (N,N'-Dicarboxymethyl-2-propylbenzimidazole):

[0030] Take 4.00g (42mmol) of chloroacetic acid in a three-necked round bottom flask equipped with a reflux condenser, and adjust the pH value to 8~10 with NaOH solution, then add 3.86g (14mmol) of 2-propylbenzimidazole and heat to reflux During the period, adjust the pH value continuously to keep the pH value of the system at 8~10 until the pH value is stable, then continue to reflux for 30min, cool, add concentrated hydrochloric acid to adjust the pH=2~3, a large amount of white precipitate is formed. Let it stand overnight, filter with suction, wash with distilled water and acetone 3 times, and then recrystallize with water to obtain a white solid.

[0031] Melting point: 285~286 o C yield: 66%. 1 H NMR (400MHz D 2 O, ppm) δ: 7.46~7.57 (m, 4H), 4.56~4.75 (d, 4H), 1.57~1.63 (m 2H), 2.99~3.03 (m, 2H), 0.85~0.90 (m, 3H), IR(KBr); IR (KBr) v: 1749 (C=O), 1...

Embodiment 3

[0034] Example 3. Preparation of Gel G1

[0035] (1) Preparation of compound L1 (N,N'-Dicarboxymethyl-2-propylbenzimidazole): same as in Example 1.

[0036] (2) Preparation of gel G1

[0037] Mix compound L1 and copper sulfate in a ratio of 1:1 and add to H 2 O / DMSO mixed solution (H 2 The volume ratio of O to DMSO is 2:1). The white fibrous gel G1 is formed by ultrasonic treatment at 40 kHz for 6 seconds and placed at room temperature. The formed gel is heated to return to the solution state.

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Abstract

The invention provides a preparation method of super-molecule metal gel and belongs to the field of functional materials. The super-molecule metal gel is obtained by a complex formed by complexing a benzimidazole carboxylic acid derivative as well as metallic lead, cadmium, copper and zinc in H2O / CH3OH, H2O / DMSO, H2O / CH3CN, H2O / CHC13 or H2O / DMF systems under the ultrasonic condition. FT-IR spectrum and X-ray diffraction results show that the gel prepared according to the invention is formed by constraining solvent micromolecules through the coordination complex formed by the benzimidazole carboxylic acid derivative and the metallic ions; and as the gel shows the conversion nature of reversible gel-sol under the acid-base control, the gel can be used for making a controllable molecular switch.

Description

Technical field [0001] The invention belongs to the field of functional materials, and relates to a supramolecular metal gel, in particular to a supramolecular metal gel formed by a benzimidazole carboxylic acid derivative and metal lead, cadmium, copper, and zinc under the action of ultrasound. Used to make controllable molecular switches. Background technique [0002] In recent years, supramolecular gels have gradually developed into a class of smart / functional nanomaterials with broad application prospects. Most of the supramolecular gels currently studied use hydrogen bonds or molecular stacking. However, coordination bonds, which are equally important in supramolecular chemistry, are far from being used in gel synthesis. Since the introduction of metal ions can bring new properties such as photoelectricity, catalysis, and redox to the gel, the research on supramolecular metal gels has also been heating up in recent years. Summary of the invention [0003] The purpose of the...

Claims

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Application Information

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IPC IPC(8): C07F7/24C07F3/08C07F1/08C07F3/06C07D235/08
Inventor 张有明张万强林奇魏太保
Owner NORTHWEST NORMAL UNIVERSITY
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