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Preparation method of mono-molecule layer polysilane fluorescent sensing film sensitive to nitro-aromatic compounds

A monolayer, fluorescence sensing technology, applied in fluorescence/phosphorescence, material excitation analysis, etc., to achieve the effects of high sensitivity, mild reaction conditions, and feasible process

Inactive Publication Date: 2007-10-17
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the research of fluorescent sensing thin film materials that covalently bind conjugated fluorescent polymers to the surface of glass substrates to realize the detection of vapors containing trace amounts of nitroaromatic compounds.

Method used

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  • Preparation method of mono-molecule layer polysilane fluorescent sensing film sensitive to nitro-aromatic compounds
  • Preparation method of mono-molecule layer polysilane fluorescent sensing film sensitive to nitro-aromatic compounds
  • Preparation method of mono-molecule layer polysilane fluorescent sensing film sensitive to nitro-aromatic compounds

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Experimental program
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Effect test

Embodiment 1

[0042] Taking the sodium metal raw material 3g used for the preparation of the monomolecular layer polydiphenylsilane fluorescent sensing film of the present invention as an example, the preparation method is as follows:

[0043] 1. Tailoring the substrate

[0044] Cut the glass plate into 0.9×2.5cm 2 sized rectangular piece of glass.

[0045] 2. Prepare lotion

[0046] Mix 30% hydrogen peroxide and 98% sulfuric acid at a volume ratio of 7:3 to make a washing solution.

[0047] 3. Preparation of activated substrate

[0048] First wash the glass piece with water and ethanol, dry it, put it into the lotion, heat it at 80-100°C for 1-2 hours, cool it naturally, wash the glass piece with twice distilled water, wash off the lotion remaining on the surface, and blow it with a hair dryer. Dry to make an activated substrate.

[0049] 4. Preparation of silanized substrate

[0050] Put the activated substrate into a solution with a volume ratio of 3-chloropropyltrimethoxysilane an...

Embodiment 2

[0058] Taking the sodium metal raw material 3g used for the preparation of the monomolecular layer polydiphenylsilane fluorescent sensing film of the present invention as an example, the preparation method is as follows:

[0059] In this embodiment, in the preparation of silylated substrate 4, the activated substrate is put into a solution whose volume ratio of 3-chloropropyltrimethoxysilane and toluene solution is 1:100, and refluxed for 3 hours. Others in this step Process is identical with embodiment 1. In step 5 of preparing polysiladiphenylane, in a 500mL three-necked flask equipped with an electromagnetic stirrer, a reflux condenser and a constant pressure dropping funnel, 3g of sodium was added under the condition of 0.6-0.8mL / s argon gas, Heat 60g of toluene to 110°C, reflux, and stir for 1 hour with an electromagnetic stirrer at a speed of 1800 rpm; mix 16.51g of diphenyldichlorosilane with 60g of toluene, that is, the molar ratio of diphenyldichlorosilane to sodium i...

Embodiment 3

[0061] Taking the sodium metal raw material 3g used for the preparation of the monomolecular layer polydiphenylsilane fluorescent sensing film of the present invention as an example, the preparation method is as follows:

[0062] In this embodiment, in the preparation of silylated substrate 4, the activated substrate is put into a solution whose volume ratio of 3-chloropropyltrimethoxysilane and toluene solution is 1:120, and refluxed for 6 hours. Others in this step Process is identical with embodiment 1. In step 5 of preparing polysiladiphenylane, in a 500mL three-necked flask equipped with an electromagnetic stirrer, a reflux condenser and a constant pressure dropping funnel, 3g of sodium was added under the condition of 0.6-0.8mL / s argon gas, Heat 90g of toluene to 110°C, reflux, and stir for 1 hour with an electromagnetic stirrer at a speed of 1800 rpm; mix 16.51g of diphenyldichlorosilane with 90g of toluene, that is, the molar ratio of diphenyldichlorosilane to sodium i...

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Abstract

A method of preparing monomolecular layer polysilane fluorescence sensing thin film sensitized to nitroarene includes steps of: cutting substrate, preparing lotion, preparing active substrate, preparing silanized substrate, preparing polysilane, and preparing monomolecular layer polysilane fluorescence sensing thin film. The invention assembles a monolayer of silanization agent with chlorine functional group at terminal to a glass substrate surface, polysilane with lithium at terminal reacts with the alkyl chloride to be chemically combined on the surface of the substrate, conjugated fluorescence macromolecule is introduced into the sensing thin film, hypersensitization of the thin film sensor is realized, and problem of stability and permeability for solid fluorescence sensor is solved. Advantages of the invention are: stability is good, life time is long, sensitivity is high, the fluorescence sensing thin film can be used on sensor and detection instrument for detecting nitroarene-containing compound, and the fluorescence sensing thin film sensed nitroarene compound can be directly detected by fluorescence instrument.

Description

technical field [0001] The invention belongs to the technical field of conjugated fluorescent polymer fluorescent sensing thin film materials, and in particular relates to a preparation method of a monomolecular layer polysilane fluorescent sensing thin film sensitive to nitroaromatics. Background technique [0002] In recent years, with the increasing demand for anti-terrorism, anti-chemical and biological weapons, non-metal mine detection, and environmental quality monitoring, countries around the world have paid more and more attention to the research of various high-performance thin-film sensors. Compared with homogeneous (solution) sensors, thin-film sensors have the advantages of being reusable, basically not polluting the system to be measured, and being easy to device, so they have attracted much attention. Most of the existing optical sensing films are semiconductor films, fluorescent polymer films, and dye-doped (or dye-modified) polymer or oxide films. Among them...

Claims

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Application Information

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IPC IPC(8): G01N21/64C08G77/60C08J5/18
Inventor 房喻何刚张国防吕凤亭
Owner SHAANXI NORMAL UNIV
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