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Preparation method of bis-schiff base fluorescent polymer and application

A fluorescent polymer, double Schiff base technology, applied in fluorescence/phosphorescence, chemical instruments and methods, luminescent materials, etc., to achieve the effects of short sensing time, simple methods and equipment, and high sensitivity

Inactive Publication Date: 2017-06-20
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, until now, fluorescence detection of Schiff base

Method used

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  • Preparation method of bis-schiff base fluorescent polymer and application
  • Preparation method of bis-schiff base fluorescent polymer and application
  • Preparation method of bis-schiff base fluorescent polymer and application

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0032] Example 1: Synthesis of bi-Schiff base fluorescent polymer with fluorescent properties.

[0033] 1. After installing the reaction device, add 0.5366g of terephthalaldehyde, 30mL of methanol or DMF or DMSO to a three-necked flask or other reaction flask in sequence, then stir until the terephthalaldehyde is completely dissolved, then add 1.6mL of ammonia water to the bottle .

[0034] 2. Use a water bath to heat a three-neck flask or other reaction flask to 75°C, and then maintain a constant temperature under reflux for 12 hours.

[0035] 3. After the reaction is over, cool the three-neck flask or other reaction flasks to room temperature, filter the reaction mixture with suction, wash with methanol or ethanol several times, and dry it in a vacuum oven at 60°C. After 24 hours, the products P-meth, P -dmf or P-dmso.

example 2

[0036] Example 2: Test the ultraviolet absorption spectrum and fluorescence spectrum of the product obtained.

[0037] Depend on figure 1 The fluorescence excitation spectrum and figure 2 It can be known that the emission wavelengths of the samples are: P-meth 486nm (λex=412nm), P-dmf 526nm (λex=443nm), P-dmso 548nm (λex=447nm).

example 3

[0038]Example 3: Test the infrared spectrum and carbon nuclear magnetic resonance spectrum of the obtained sample.

[0039] The product is compared with terephthalaldehyde in infrared spectrum, and it is found that 1698cm -1 C=O stretching vibration absorption peak disappears, 1604cm -1 The appearance of C=N stretching vibration absorption peak indicates that the polycondensation reaction has occurred. From the carbon nuclear magnetic resonance spectrum, it can be seen that the peaks at 68 and 81ppm are the carbons of -CH-N, 131-150ppm are the carbons on the benzene ring, 166 and 181ppm are the carbons of -C=N, and 195ppm are the carbons on the terminal aldehyde group carbon.

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Abstract

The invention discloses a preparation method of a bis-schiff base fluorescent polymer and an application in fluorescence detection of small molecular pollutants and an explosive nitrobenzene. The preparation method comprises the following steps of: (1) constructing an organic reflux reaction device, successively adding aldehyde and an organic solvent into a dried reaction container, stirring the mixture till the aldehyde is fully dissolved, and then adding ammonia water; (2) heating the mixture to 60-90 DEG C and keeping a constant temperature reflux reaction for 8-20h; and (3) after reaction, cooling the reaction container to room temperature, and filtering, washing and drying the mixture obtained by the reaction to obtain a product.

Description

technical field [0001] The invention belongs to the technical field of polymer fluorescent material preparation, and relates to a synthesis method of a double Schiff base fluorescent polymer and an application of the polymer. Background technique [0002] Schiff base, also called imine, is obtained by Mannich reaction. This reaction requires acid or base as a catalyst, so it has strict requirements on pH. The polymerization methods of imines currently include suspension polymerization, emulsion polymerization, dispersion polymerization, reprecipitation polymerization, etc. All the above polymerization methods need to add appropriate additives or initiators and the polymerization temperature is relatively high. The invention adopts aldehyde and ammonia water as raw materials, generates Schiff base under the action of a certain solvent, and directly undergoes polymerization reaction to generate Schiff base polymer. Compared with the existing methods, the method adopted in the...

Claims

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Application Information

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IPC IPC(8): C08G12/02C09K11/06G01N21/33G01N21/35G01N21/64G01N24/08
CPCC08G12/02C09K11/06C09K2211/14G01N21/33G01N21/35G01N21/64G01N21/6428G01N21/643G01N24/08G01N2021/6432
Inventor 朱蕙林黄金萍胡岗
Owner SHANGHAI NORMAL UNIVERSITY
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