Stimulation responsive spiral polyyne infrared radiation material and preparation method
An infrared radiation and responsive technology, which is applied in the field of stimuli-responsive helical polyalkyne infrared radiation materials and preparation, can solve the problems of large thickness, low emission colored pigment molecule design difficulty, high infrared emissivity, etc., and achieve mild reaction conditions , good thermal stability and controllability of infrared radiation performance, and the effect of simple preparation process
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example 1
[0025] a) Under ice bath, add 1.73g (S)-2-(6-hydroxy-2-naphthalene)propionic acid, 1.51g isobutyl chloroformate, and 1.01g N-methylmorpholine to a chamber containing 50mL of tetrahydrofuran. In the reaction kettle, 10 mL of propargylamine tetrahydrofuran solution with a concentration of 0.8 mol / L was added dropwise to the mixed solution after the reaction for 15 min. After the dropwise addition for 15 min, the reaction was continued at 30 ° C for 12 h, filtered, and the tetrahydrofuran was evaporated under reduced pressure at 60 ° C. Then extract with 30 mL of ethyl acetate each time, combine the three extractions to obtain an extraction mixture, and sequentially use 25 mL of aqueous hydrochloric acid with a mass fraction of 2 wt %, 25 mL of saturated NaHCO 3 The extract was washed with an aqueous solution and 25 mL of saturated aqueous NaCl solution, and the obtained extract was washed with 2.2 g of anhydrous MgSO 4Dry for 12h, filter, and evaporate the filtrate under reduced...
example 2
[0032] a) Under ice bath, add 2 g of (S)-2-(6-hydroxy-2-naphthalene) propionic acid, 1.8 g of isobutyl chloroformate, and 1.4 g of N-methylmorpholine to a solution containing 100 mL of tetrahydrofuran. The reaction was carried out in the reaction kettle for 20 min, and then 30 mL of propargylamine tetrahydrofuran solution with a concentration of 1.2 mol / L was added dropwise to the mixed solution. After the dropwise addition for 20 min, the reaction mixture was reacted at 30 °C for 20 h, filtered, and decompressed at 50 °C. The tetrahydrofuran was evaporated, extracted with 30 mL of ethyl acetate each time, and the extracts were combined for three times to obtain an extraction mixture, and 30 mL of aqueous hydrochloric acid with a mass fraction of 3 wt % and 30 mL of saturated NaHCO were successively used. 3 The extract was washed with an aqueous solution and 30 mL of saturated NaCl aqueous solution, and the obtained extraction mixture was washed with 2 g of anhydrous MgSO 4 Dr...
example 3
[0039] a) Under ice bath, 1.50g (S)-2-(6-hydroxy-2-naphthalene)propionic acid, 1.37g isobutyl chloroformate, 0.81g N-methylmorpholine were added to the tetrahydrofuran containing 40mL In the reaction kettle, 10 mL of propargylamine tetrahydrofuran solution with a concentration of 1.00 mol / L was added dropwise to the mixed solution after the reaction for 25 min. After the dropwise addition for 25 min, the reaction was continued at 30 °C for 18 h, filtered, and the tetrahydrofuran was evaporated under reduced pressure at 55 °C. Then extract with 20 mL of ethyl acetate each time, combine the three extractions to obtain an extraction mixture, and sequentially use 20 mL of aqueous hydrochloric acid with a mass fraction of 2 wt %, 20 mL of saturated NaHCO 3 The extract was washed with an aqueous solution and 20 mL of saturated NaCl aqueous solution, and the extracted mixture after washing was washed with 3.6 g of anhydrous MgSO. 4 Dry at 25°C for 12h, filter, and evaporate the filt...
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