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Preparation method of zirconium tetramethoxyphenylporphyrin nanotube-selenium trioxide nanosheet composite thermosensitive sensing material

A technology of tetramethoxyphenylporphyrin and tetramethoxyphenyl, which is applied in the field of thermal sensing materials to achieve the effects of improving transmission efficiency, improving stability and expanding specific surface area

Active Publication Date: 2020-02-28
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, there are still few reports on combining the above materials as sensor materials. Therefore, research in this direction has certain significance for the field of sensor materials.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention relates to the field of thermosensitive sensing materials, and discloses a preparation method of a zirconium tetramethoxyphenylporphyrin nanotube-selenium trioxide nanosheet composite thermosensitive sensing material. The method comprises the following steps: preparing tetramethoxybenzaldehyde, and reacting with trichloromethane in a hydrogen chloride atmosphere to prepare tetramethoxyphenyl porphyrin; adding tetramethoxyphenyl porphyrin and anhydrous zirconium chloride into a mixed solution of benzoic acid and polyethylene glycol for reaction to obtain zirconium tetramethoxyphenyl porphyrin; preparing selenium trioxide, and generating selenium trioxide nanosheets on the stem of the porphyrin tetramethoxyphenyl zirconium nanotube by utilizing a hydrothermal method; and spin-coating the surfaces of the zirconium tetramethoxyphenyl porphyrin nanotube-selenium trioxide nanosheet with a polymethylphenyl siloxane film. Thus, the structure of the zirconium tetramethoxyphenyl porphyrin nanotube-selenium trioxide nanosheet composite material is kept regular, and the material is protected to certain extent.

Description

technical field [0001] The invention relates to the field of heat-sensitive sensing materials, in particular to a preparation method of a tetramethoxyphenyl zirconium porphyrin nanotube-selenium trioxide nanosheet composite heat-sensitive sensing material. Background technique [0002] Porphyrin is a class of biomimetic compounds with a large π structure that has many important enzyme active sites. It is also the active center of many proteins and enzymes in nature. Because of its unique structure and superior properties, it has been widely studied in various fields. Many porphyrins exist in nature in the form of coordination with metal ions. Porphyrins or modified porphyrins can coordinate with metals such as iron, cobalt, and aluminum, and catalyze the copolymerization of carbon dioxide and epoxy compounds under the joint action of co-catalysts. Porphyrin nanotubes have a large specific surface area, which can enhance the electrical signal and improve the catalytic ability...

Claims

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Application Information

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IPC IPC(8): G01K13/00
CPCG01K13/00
Inventor 万军民王倩易彭志勤王秉
Owner ZHEJIANG SCI-TECH UNIV
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