Preparation of thiophene monomer and its polymerizing method
A polymerization method and polymer technology, applied in the preparation and application of thiophene polymer monomers, and the application field of preparation of thiophene polymers, can solve the problems of not meeting the electronic level requirements, small resistivity, film transparency and conductivity Insufficient performance and other problems, to achieve the effect of saving solvent consumption and improving economic benefits
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Embodiment 1
[0038] Embodiment one catalytic decarboxylation reaction
[0039] Add 240ml of sulfolane into the reactor, stir to make it uniform, add 50g of ethylenedioxydicarboxylic acid (water content, the content is measured by liquid chromatography), and 2.5g of copper carbonate+1.0g of chromium oxide. Heat to 80°C under a vacuum of 2000Pa, and keep the temperature for 40 minutes to remove the contained moisture. Fill it with nitrogen, and continue to heat up to 110-130°C. The mixture was reacted at this temperature for 8 h until CO was no longer formed 2 The reaction is over. The temperature of the mixture is slightly lowered, and the mixture is evacuated at a vacuum degree of 2000 Pa and 130-150° C. to distill out the mixed solution of ethylenedioxythiophene / sulfolane.
[0040] Add the same amount of ethylene dioxydicarboxylic acid and a small amount of copper carbonate to the remainder of the reactor, and the sulfolane that evaporates is replenished with new sulfolane, and the sub...
Embodiment 2
[0044] Embodiment two catalyst-free, pure heat decarboxylation reaction
[0045] 350ml of dibutyl phthalate was added to the reaction flask, and 24g of 3,4-ethylenedioxythiophene dicarboxylic acid was added with stirring (the content was given by liquid chromatography). Under the condition of vacuum degree of 3KPa, heat the internal temperature of the mixed material to 140-150°C, and keep the temperature constant for 40 minutes. During this process, the moisture inside the material evaporates.
[0046] Fill the reactor with nitrogen, continue heating to 240-250°C, keep the temperature for 24 hours until there is no more CO 2 Until the generation, the reaction is over, keep vacuum cooling, and distill off the reaction product colorless liquid 3,4-alkylenedioxythiophene (EDT or EDOT) at 180 ° C and 100 Pa to obtain 12 g of the product (theoretical yield is 80%). EDT boiling point 225°C (1000Kpa), HPLC: 97.5%.
[0047] experimental method
Embodiment 3
[0048] Embodiment three 3, the catalytic decarboxylation reaction of 4-dimethoxythiophene
[0049] 175ml of sulfolane and 50g of 70% 3,4-dimethoxythiophene dicarboxylic acid containing water (35g, dry basis) were added into the reactor and stirred evenly. 4.5 g of copper hydroxide was added, the temperature of the mixture was raised to 85° C., and the temperature was kept constant for 1.0 h under a vacuum of 5000 Pa. Fill with nitrogen, raise the temperature to 120°C, and keep the temperature constant for 9.0 hours until there is no more CO 2 generated. Then 1.5g of chromium hydroxide was added, and the mixture was stirred and reacted for 3.0h. The temperature at the bottom of the rectification column was 140-150° C., and the temperature at the top was 110-140° C. to distill the product 3,4-dimethoxythiophene to obtain 19.5 g of the product with a yield of 85%. Product IR (KBr, discs) Ar-H, 3115cm -1 ; 1 HNMR (400MHz, CDCl 3 , 25°C) δ=3.78 (OCH 3 ), δ=6.37 (Ar-H).
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