A kind of thienothiophene electrochromic polymer and preparation method thereof
An electrochromic and polymer technology, applied in the field of polymer materials, can solve the problems of poor cycle stability, long response time, slow ion diffusion rate of electrochromic materials, etc., to improve ionic conductivity, response rate, contrast ratio improved effect
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Embodiment 1
[0052] A molecular structure is The electrochromic polymer of the thienothiophene class, its synthetic reaction formula is as follows:
[0053]
[0054] Its preparation steps are as follows:
[0055] 1), add thieno[3,2-b]thiophene (1.340g, 10mmol) into a 250ml reaction vessel, add a mixed solvent of glacial acetic acid (20ml) and chloroform (100ml), drop Br2 (4.735 g, 30mmol), stirred for another 5 hours, and heated to reflux overnight; after cooling to room temperature, a large amount of water was added, filtered and washed, and vacuum-dried to obtain tetrabromothieno[3,2-b]thiophene compound 3-1 (4.065g, 90 %);
[0056] 2), add elemental zinc (1.151g, 18mmol) and tetrabromothieno[3,2-b]thiophene compound 3-1 (4.065g, 9mmol) in the reaction flask, then add glacial acetic acid (20ml), stir at room temperature Overnight; add a large amount of water, filter and wash, and vacuum dry to obtain 3,6-dibromothieno[3,2-b]thiophene compound 3-2 (2.514g, 94.4%);
[0057] 3), und...
Embodiment 2
[0065] A molecular structure is The electrochromic polymer of the thienothiophene class, its synthetic reaction formula is as follows:
[0066] Its preparation method comprises steps:
[0067] According to the preparation method in Example 1, 3,6-dimethoxythieno[3,2-b]thiophene compound was obtained;
[0068] Under nitrogen protection environment, 3,6-dimethoxythieno[3,2-b]thiophene compound (1.6g, 8mmol), sodium p-toluenesulfonate (0.275g, 1.6mmol), triethylene glycol Add monoethyl ether (5.70g, 32mmol) into toluene solvent (80ml), heat and reflux for 20 hours; add water after cooling to room temperature, extract with dichloromethane solvent (300ml) and wash several times, add silica gel after drying the organic phase and spin dry , column chromatography separation to obtain compound 15-M1;
[0069] Under nitrogen protection environment, compound 15-M1 (158.04mg, 0.5mmol), Potassium carbonate (138.21, mg, 1 mmol) and palladium acetate (4.49 mg, 0.02 mmol) were added t...
Embodiment 3
[0071] A molecular structure is The electrochromic polymer of the thienothiophene class, its synthetic reaction formula is as follows:
[0072]
[0073] , its preparation method comprises steps:
[0074] According to the preparation method in Example 1, 3,6-dimethoxythieno[3,2-b]thiophene compound was obtained;
[0075] Under nitrogen protection environment, 3,6-dimethoxythieno[3,2-b]thiophene compound (1.6g, 8mmol), sodium p-toluenesulfonate (0.275g, 1.6mmol), triethylene glycol Add monoethyl ether (5.70g, 32mmol) into toluene solvent (80ml), heat and reflux for 20 hours; add water after cooling to room temperature, extract with dichloromethane solvent (300ml) and wash several times, add silica gel after drying the organic phase and spin dry , column chromatography separation to obtain compound 34-M1;
[0076] Under nitrogen protection environment, compound 34-M1 (158.04mg, 0.5mmol), Potassium carbonate (138.21, mg, 1 mmol) and palladium acetate (4.49 mg, 0.02 mmol) ...
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