Double-state luminous porphyrin fluorescent material and preparation method thereof
A technology of fluorescent materials and porphyrins, which can be used in luminescent materials, chemical instruments and methods, photovoltaic power generation, etc.
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Embodiment 1
[0093] Embodiment 1 A kind of preparation method of the porphyrin fluorescent material of double state light emission
[0094] This embodiment includes the following steps carried out in sequence:
[0095] S1. get 16mmol of 5-(4-hydroxyphenyl)-10,15,20-triphenylporphyrin and 24mmol of hexamethylenetetramine, dissolve in 100mL of trifluoroacetic acid under the protection of nitrogen, Reflux reaction at 70°C for 20h, add 100mL of hydrochloric acid with a concentration of 1mol / L after the reaction, stir at 25°C for 2h, adjust the reaction solution to neutral with NaOH solution, extract with dichloromethane and take the organic layer, The organic layer was washed 3 times with saturated brine, then washed with anhydrous Na 2 SO 4 Dry, filter, remove the solvent by rotary evaporation under reduced pressure, then use a solution of petroleum ether and dichloromethane mixed at a volume ratio of 3:1 as the eluent for elution, then use a silica gel column to purify the product, and fin...
Embodiment 2
[0104] Embodiment 2 A kind of preparation method of the porphyrin fluorescent material of double state light emission
[0105] This embodiment includes the following steps carried out in sequence:
[0106] S1. get 16mmol of 5-(4-hydroxyphenyl)-10,15,20-triphenylporphyrin and 16mmol of hexamethylenetetramine, dissolve in 100mL of trifluoroacetic acid under the protection of nitrogen, Reflux reaction at 90°C for 10h, add 100mL hydrochloric acid with a concentration of 0.8mol / L after the reaction, stir at 30°C for 3h, adjust the reaction solution to neutral with KOH solution, extract with dichloromethane and take the organic layer , the organic layer was washed 5 times with saturated brine, and washed with anhydrous Na 2 SO 4 Dry, filter to remove the desiccant, remove the solvent by rotary evaporation under reduced pressure, then use a solution of petroleum ether and dichloromethane mixed in a volume ratio of 3:1 as the eluent for elution, and then use a silica gel column to p...
Embodiment 3
[0109] Embodiment 3 A kind of preparation method of the porphyrin fluorescent material of double state light emission
[0110] This embodiment includes the following steps carried out in sequence:
[0111] S1. get 16mmol of 5-(4-hydroxyphenyl)-10,15,20-triphenylporphyrin and 32mmol of hexamethylenetetramine, dissolve in 100mL of trifluoroacetic acid under the protection of nitrogen, Reflux reaction at 80°C for 12 hours, add 100mL of hydrochloric acid with a concentration of 1.5mol / L after the reaction, stir at 20°C for 3h, adjust the reaction solution to neutral with NaOH solution, extract with dichloromethane and take the organic layer , the organic layer was washed 4 times with saturated brine, and washed with anhydrous Na 2 SO 4 Dry, filter to remove the desiccant, remove the solvent by rotary evaporation under reduced pressure, then use a solution of petroleum ether and dichloromethane mixed in a volume ratio of 3:1 as the eluent for elution, and then use a silica gel co...
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