A kind of porphyrin phthalocyanine bilayer metal complex and its preparation method and application

A double-layer metal and porphyrin phthalocyanine technology, which is applied in the field of porphyrin phthalocyanine double-layer metal complexes and its preparation, can solve the problems of poor stability and high working temperature, achieve good practical value, low response concentration, The preparation method is simple and effective

Inactive Publication Date: 2018-05-01
UNIV OF JINAN
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although metal-oxide-semiconductor gas sensors are widely used in the fields of household, industry, and environmental monitoring due to their advantages of low cost, simple preparation method, and high sensitivity, they have high operating temperature (generally 250-450°C) and high stability. Poor and other shortcomings

Method used

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  • A kind of porphyrin phthalocyanine bilayer metal complex and its preparation method and application
  • A kind of porphyrin phthalocyanine bilayer metal complex and its preparation method and application
  • A kind of porphyrin phthalocyanine bilayer metal complex and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Embodiment 1 (preparation of Eu(TPyP){Pc-(OC 8 h 17 ) 8})

[0051] 1.1

[0052] 65 mg (0.1 mmol) of 5, 10, 15, 20-pyridylporphyrin 5,10,15,20-tetrakis(4-pyridyl)porphyrin (CAS No.: 16834-13-2;) and 45 mg Europium acetylacetonate (0.1 mmol) was dissolved in 6 mL of trichlorobenzene, nitrogen was used as a protective gas, and reacted at 190 °C for 6 hours. After the reaction was completed, trichlorobenzene was evaporated to dryness under reduced pressure and cooled. Add 238 mg (0.6 mmol) of 4,5-dioctyloxy-1,2-dicyanylbenzene (CAS No.: 118132-11-9) and 0.1 mL of 1,8-diazabicyclo[5.4.0] Undec-7-ene (CAS number: 6674-22-2) was reacted with n-octanol (8 mL) as the medium and nitrogen as the protective gas with stirring for 12 hours at a reaction temperature of 190 °C. After the reaction was completed, n-octanol was evaporated to dryness under reduced pressure and cooled. Using chloroform / methanol (volume ratio 100:6) as the eluent, the silica gel column was used for pu...

Embodiment 2

[0056] 2.1

[0057] ①Put the anodized aluminum film with a pore size of 200nm into a beaker, then place it in an ultrasonic cleaner, and use solvents of different polarities including water, ethanol, acetone, and chloroform to ultrasonically clean it for ten minutes in sequence, and then vacuum dry it for later use.

[0058] ② Dissolve 0.003mmol Eu(TPyP){Pc-(OC8H17)8} in 1 mL THF to obtain a THF solution of Eu(TPyP){Pc-(OC8H17)8}; (AAO) soaked in the tetrahydrofuran solution of Eu(TPyP){Pc-(OC8H17)8}, after standing for 8 hours, the tetrahydrofuran solution was sucked out, and dried in vacuum; Eu(TPyP){Pc-(OC8H17)8} containing AAO was obtained nanotube.

[0059] ③The Eu(TPyP){Pc-(OC8H17)8} nanotubes containing AAO were dissolved with 6 mol / L sodium hydroxide aqueous solution to remove the anodized aluminum oxide film, remove the liquid, and collect the solid product.

[0060] ④ The obtained Eu(TPyP){Pc-(OC8H17)8} nanotubes were washed with distilled water, and then diffused ...

Embodiment 3

[0086] Example 3 Preparation of Eu(TPyP){Pc-(OC8H17)8}Nanotube Nitrogen Dioxide Gas Sensor

[0087] (1) The substrate of the ITO conductive glass interdigitated electrode was ultrasonically treated three times with toluene, acetone, ethanol, and deionized water, respectively, for five minutes each time, and vacuum-dried for later use.

[0088] (2) Use a dropper to drop-coat 1 mg of Eu(TPyP){Pc-(OC8H17)8} nanotubes prepared in Example 2 onto the interdigitated electrodes of the above-mentioned treated ITO conductive glass substrate, and let it dry naturally , that is, the gas sensor of the gas sensor (such as figure 1 shown).

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Abstract

The invention relates to a porphyrin-phthalocyanine double-layer metal complex, and a preparation method and application thereof, belonging to the technical field of organic semiconductor material chemistry. Eu(TPyP){Pc-(OC8H17)8} and Eu(TPyP){Pc-(OC8H17)8} nanotubes are synthesized for the first time. The preparation process of the Eu(TPyP){Pc-(OC8H17)8} nanotubes comprises the following steps: (1) dissolving Eu(TPyP){Pc-(OC8H17)8} in a specific solvent to prepare a solution; (2) immersing AAO in the solution prepared in the step (1), and standing in a sealed state for 8-12 hours; removing the solution, and carrying out vacuum drying; and (3) dissolving out the AAO by using a sodium hydroxide water solution. The preparation method is simple and effective, is controllable in the experimentation process, and can be carried out at room temperature. The Eu(TPyP){Pc-(OC8H17)8} nanotubes are pure and ordered, and can be used for detecting nitrogen dioxide at room temperature. The Eu(TPyP){Pc-(OC8H17)8} nanotubes have the advantages of low response concentration for NO2, low gas-sensitive detection limit for NO2, high response speed and short restoration time. The Eu(TPyP){Pc-(OC8H17)8} nanotubes can resist interference of ammonia gas and CO.

Description

technical field [0001] The invention relates to a porphyrin phthalocyanine double-layer metal complex and its preparation method and application, belonging to the technical field of organic semiconductor material chemistry. Background technique [0002] The main ways of causing air pollution at present: ①Industrial production produces a large number of flammable, explosive, toxic gases and their mixtures (such as CH 4 、H 2 , NO 2 , ammonia, etc.); ②In household and office situations, quite a lot of man-made materials volatilize a variety of trace gases (such as aromatic hydrocarbons (benzene, toluene, etc.), ketones and aldehydes, ammonia and amines, etc.); ③ Exhaust gas emitted by vehicles. These gases not only pollute the atmospheric environment, but most of them have acute or chronic harmful effects on the human body, and even cause the loss of human life. Therefore, the development and research of gas sensors to detect toxic and harmful gases is of great value to the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/00C07D487/22B82Y40/00G01N27/00
CPCB82Y40/00C07D487/22C07F5/003G01N27/00
Inventor 朱沛华王榆成方明亮荆路
Owner UNIV OF JINAN
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