A preparation method of tetramethoxyphenyl zirconium porphyrin nanotube-selenium trioxide nanosheet composite thermal sensing material
A technology of tetramethoxyphenylporphyrin and tetramethoxyphenyl, which is applied in the field of heat-sensitive sensing materials, to increase the transmission path, facilitate the transmission of electrons, and improve the transmission efficiency
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Embodiment 1
[0030] 1) preparation of tetramethoxybenzaldehyde
[0031] Get 30g p-Hydroxybenzaldehyde and 160mL distilled water, add in the 250mL there-necked bottle that 25wt% NaOH aqueous solution is housed, after treating that p-Hydroxybenzaldehyde dissolves completely, add 5g dimethyl sulfate and 10g tetrabutylammonium bromide (Bu 4NBr), refluxed at 100°C for 7h. When the temperature dropped to 100°C, the reaction solution was quickly transferred to a large beaker, and gradually cooled to room temperature. After the reaction solution cooled, it was washed three times with NaOH aqueous solution until the pH value was 8. Dry in a vacuum oven at 60° C. for 5 hours to obtain a crude product; dry the resultant, then vacuum distill to collect the product and store it for future use.
[0032] 2) Preparation of Tetramethoxyphenylporphyrin
[0033] Dissolve 40g of tetramethoxybenzaldehyde in 180mL of toluene and dichloromethane, react with dichloromethane dissolved in fuming sulfuric acid und...
Embodiment 2
[0049] 1) preparation of tetramethoxybenzaldehyde
[0050] Get 15g p-Hydroxybenzaldehyde and 100mL distilled water, add in the 250mL there-necked flask that the aqueous solution of 20wt%NaOH is housed, after treating that p-Hydroxybenzaldehyde dissolves completely, add 7g dimethyl sulfate and 9g tetrabutylammonium bromide (Bu 4 NBr), refluxed at 120°C for 7h. When the temperature dropped to 100°C, the reaction solution was quickly transferred to a large beaker, and gradually cooled to room temperature. After the reaction solution cooled, it was washed three times with NaOH aqueous solution until the pH value was 8. Dry in a vacuum oven at 60° C. for 5 hours to obtain a crude product; dry the resultant, then vacuum distill to collect the product and store it for future use.
[0051] 2) Preparation of Tetramethoxyphenylporphyrin
[0052] Dissolve 60g of tetramethoxybenzaldehyde in 180mL of toluene and chloroform, react with chloroform with oleum dissolved in hydrogen chloride ...
Embodiment 3
[0068] 1) preparation of tetramethoxybenzaldehyde
[0069] Get 20g p-Hydroxybenzaldehyde and 130mL distilled water, add in the 250mL there-necked flask that the aqueous solution of 30wt%NaOH is housed, after treating that p-Hydroxybenzaldehyde dissolves completely, add dimethyl sulfate and tetrabutylammonium bromide (Bu 4 NBr), reflux at 150° C. for 5 h. When the temperature dropped to 100°C, the reaction solution was quickly transferred to a large beaker, and gradually cooled to room temperature. After the reaction solution cooled, it was washed four times with NaOH aqueous solution until the pH value was 8. Dry in a vacuum oven at 60° C. for 5 hours to obtain a crude product; dry the resultant, then vacuum distill to collect the product and store it for future use.
[0070] 2) Preparation of Tetramethoxyphenylporphyrin
[0071] Dissolve 80g of tetramethoxybenzaldehyde in 200mL of toluene and chloroform, react with chloroform with oleum dissolved in hydrogen chloride atmosp...
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