Electrolyte comprising 3,4-ethylenedioxythiophene, and electrolytic capacitor and material for electronic material including same
An ethylenedioxythiophene and electrolytic capacitor technology, which is applied in the field of electrolytes, can solve the problems of difficulty in preparing electrolytes with high withstand voltage characteristics and high equivalent series resistance, and achieve excellent long-term reliability, low equivalent series resistance, and high resistance. Excellent voltage characteristics
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preparation example 1
[0057] Preparation Example 1: Preparation of the monomer of chemical formula 4
[0058] As shown in the following reaction formula 5, mix 3,4-dimethoxythiophene (3,4-dimethoxythiphene) 1 (30.00g, 208.06mmol), ethylene glycol (ethyleneglycol) 2 (25.83g, 416.12mmol), Toluenesulfonic acid (p-toluenesulfonic acid) (3.96 g, 20.81 mmol) and 300 mL of toluene were stirred and reacted at 100° C. for 12 hours. Add ethyl acetate to dissolve the reaction solution completely, and use sodium sulfate (Na 2 SO 4 ) to dry the organic layer and concentrate the remaining organic layer. Through silicon dioxide (SiO 2 ) column chromatography and utilize hexane:ethyl acetate=10:1 (volume ratio) mixed solution to develop the concentrated organic layer and carry out column purification, thus obtained as 3,4-ethylenedioxythiophene (3, 4-Ethylenedioxythiophene, EDOT) compound 3 (20.70 g, 70% yield).
[0059] 1 H-NMR (CDCl 3 , Varian 400MHz): δ4.18(4H, s), 6.31(2H, s)
[0060] Reaction 5
[00...
preparation example 2
[0062] Preparation Example 2: Preparation of the monomer of chemical formula 4
[0063] As shown in the following reaction formula 6, mix 3,4-dimethoxythiophene 1 (30.00g, 208.06mmol), 1,2-pentanediol (1,2-pentanediol) 4 (43.34g, 416.12mmol), p-toluenesulfonic acid (3.96 g, 20.81 mmol) and 300 mL of toluene were stirred at 110° C. for 9 hours to react. The reaction solution was completely dissolved by adding ethyl acetate, extracted with water, and the organic layer was dried with sodium sulfate, and the remaining organic layer was concentrated. 2-Propyl-2,3-di Hydrothieno[3,4-b][1,4]di Compound 5 (25.00 g, 70% yield) of Ying (2-Propyl-2,3-dihydrothieno[3,4-b][1,4]dioxine, propyl-EDOT).
[0064] 1 H-NMR (CDCl 3 , Varian 400MHz): δ0.88(3H, t, J=12Hz), 1.31-1.70(4H, m), 3.86(1H, dd, J=8.0, 3.2Hz), 4.10-4.16(2H, m), 6.30 (2H, s).
[0065] Reaction 6
[0066]
preparation example 3
[0067] Preparation Example 3: Preparation of monomers of chemical formula 4
[0068] As shown in the following reaction formula 7, mix 3,4-dimethoxythiophene 1 (50.00g, 346.76mmol), 1,2-decanediol (1,2-octanediol) 6 (120.87g, 693.52mmol), p-toluenesulfonic acid (6.60 g, 34.68 mmol) and 500 mL of toluene were stirred at 110° C. for 9 hours and reacted. Add ethyl acetate to dissolve the reaction solution completely, and use sodium sulfate (Na 2 SO 4 ) to dry the organic layer and concentrate the remaining organic layer. 2-octyl-2,3-di Hydrothieno[3,4-b][1,4]di Compound 7 (57.33 g, 65% yield) of Ying (2-Octyl-2,3-dihydrothieno[3,4-b][1,4]dioxine, octyl-EDOT).
[0069] 1 H-NMR (CDCl 3 , Varian 400MHz): δ0.88(3H, t, J=12Hz), 1.27-1.71(14H, m), 3.86(1H, dd, J=8.0, 3.2Hz), 4.07-4.15(2H, m), 6.29 (2H, s).
[0070] Reaction 7
[0071]
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