Preparation method of polymer fluorescence sensing film containing cholesterol

A fluorescence sensing, cholesterol technology, applied in fluorescence/phosphorescence, chemical instruments and methods, luminescent materials, etc., can solve the problems of being susceptible to interference from other substances, harsh sampling conditions, and low signal-to-noise ratio, etc. Long, easy-to-operate, high-sensitivity results

Active Publication Date: 2012-07-25
SHAANXI NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the sensitivity of the above method meets the requirements of the application, it still has many deficiencies.
For example: long response time, low signal-to-noise ratio, susceptible to interference from other substances, complicated equipment, high cost, and harsh sample conditions, etc.

Method used

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  • Preparation method of polymer fluorescence sensing film containing cholesterol
  • Preparation method of polymer fluorescence sensing film containing cholesterol
  • Preparation method of polymer fluorescence sensing film containing cholesterol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1. Preparation of cholesterol-containing polymers

[0037] (1) Synthesis of 2,5-diiodo-1,4-bis(methoxy)-benzene

[0038]Under the condition of argon gas with a flow rate of 0.6-0.8mL / s, add 2g of p-xylylene dimethyl ether, 1.2g of potassium iodate, and 4g of iodine into the mixed solution of 150mL of anhydrous acetic acid and 15mL of 10% sulfuric acid aqueous solution , the molar ratio of p-xylylene dimethyl ether to potassium iodate, iodine, anhydrous acetic acid and sulfuric acid is 1:0.4:1:170:2, reflux reaction at 70°C for 12 hours, filter, and dry at 25°C for 12 hours to prepare 2 , 5-diiodo-1,4-two (methoxy)-benzene, its reaction equation is as follows:

[0039]

[0040] (2) Synthesis of 2,5-diiodo-1,4-bis(hydroxyl)-benzene

[0041] Dissolve 3g of 2,5-diiodo-1,4-di(methoxy)-benzene in 30mL of dichloromethane, add 19mL of boron tribromide dropwise at -80°C, 2,5-diiodo- The molar ratio of 1,4-bis(methoxy)-benzene to boron tribromide and dichloromethane was 1:3...

Embodiment 2

[0062] In the synthesis of 2,5-diiodo-1,4-bis(methoxy)-benzene step (1) in the preparation of cholesterol-containing polymer step 1 in Example 1, at a flow rate of 0.6 to 0.8 mL / s Under argon atmosphere, add 2 g of p-xylylene dimethyl ether, 0.6 g of potassium iodate, and 3.2 g of iodine into a mixed solution of 130 mL of anhydrous acetic acid and 8 mL of 10% sulfuric acid aqueous solution. The molar ratio of potassium, iodine, anhydrous acetic acid and sulfuric acid is 1:0.2:0.8:150:1, reflux at 70°C for 14 hours, filter and dry to prepare 2,5-diiodo-1,4-bis(methyl Oxy)-Benzene. In the synthesis of 2,5-diiodo-1,4-bis(hydroxy)-benzene step (2), 3 g of 2,5-diiodo-1,4-bis(methoxy)-benzene was dissolved in 20 mL di In methyl chloride, add 12.6 mL of boron tribromide dropwise at -80°C, the molar ratio of 2,5-diiodo-1,4-bis(methoxy)-benzene to boron tribromide and dichloromethane 1:2:40, stirred for 14 hours, filtered and dried to prepare 2,5-diiodo-1,4-bis(hydroxyl)-benzene. In...

Embodiment 3

[0064]In the synthesis of 2,5-diiodo-1,4-bis(methoxy)-benzene step (1) in the preparation of cholesterol-containing polymer step 1 in Example 1, at a flow rate of 0.6 to 0.8 mL / s Under argon atmosphere, add 2 g of p-xylylene dimethyl ether, 1.8 g of potassium iodate, and 4.8 g of iodine into a mixed solution of 170 mL of anhydrous acetic acid and 22.5 mL of 10% sulfuric acid aqueous solution with a mass fraction of p-xylylene dimethyl ether and iodine. Potassium chloride, iodine, anhydrous acetic acid, and sulfuric acid in a molar ratio of 1:0.6:1.2:190:3 were refluxed at 70°C for 8 hours, filtered, and dried to prepare 2,5-diiodo-1,4-bis( Methoxy)-Benzene. In the synthesis of 2,5-diiodo-1,4-bis(hydroxy)-benzene step (2), 3 g of 2,5-diiodo-1,4-bis(methoxy)-benzene was dissolved in 40 mL di In methyl chloride, add 25.3 mL of boron tribromide dropwise at -80°C, the molar ratio of 2,5-diiodo-1,4-bis(methoxy)-benzene to boron tribromide and dichloromethane 1:4:80, stirred for 10...

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Abstract

The invention relates to a preparation method of a polymer fluorescence sensing film containing cholesterol. According to the invention, the cholesterol is introduced into the side chain of a conjugated fluorescence molecule through utilizing the characteristics of supermolecule self-assembly, rigid construction and good film-forming properties of the cholesterol, and the molecule and diamine are polymerized, so that the polymer which contains the cholesterol and has a fluorescence property is obtained; and the novel polymer is utilized as a sensing element so as to prepare the fluorescence sensing film, thereby realizing hypersensitization of a thin film sensor and solving the stability and the permeability of a solid fluorescence sensor. The preparation method provided by the invention has the advantages that the operation is simple, and the reaction conditions are mild; and the prepared fluorescence sensing film is good in stability, long in service life, and high in hydrogen chloride gas detection sensitivity, can be applied to a sensor for detecting the hydrogen chloride gas, and can also be used in a detection instrument for detecting the hydrogen chloride gas by utilizing a fluorescence principle; and the fluorescence sensing film senses the hydrogen chloride gas so as to carry out detection directly through a fluorescence instrument.

Description

technical field [0001] The invention belongs to the technical field of using cholesterol-containing polymers to prepare fluorescent sensing film materials, and in particular relates to a method for preparing a fluorescent sensing film sensitive to hydrogen chloride. Background technique [0002] With the development of social economy and the wide application of various chemical products, the problem of environmental pollution is becoming more and more serious. Among them, hydrogen chloride gas is an important component of commonly used chemical raw materials. It is used in the production of polymers and plastic products, rubber, fertilizers, dyes and pigments. It is also used in cleaning, soaking, electroplating metals, ore smelting, oil well extraction, tanning, and soap. And edible oil refining and other industries. Hydrogen chloride gas is volatile, not easy to be adsorbed by particles, has strong diffusivity, and can be freely mixed with air. Therefore, in the chemical...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08L61/22C08G12/06C09K11/06G01N21/64
Inventor 房喻王红月刘幸蕾崔红刘太宏曹源赵珂如
Owner SHAANXI NORMAL UNIV
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