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Preparation of light-emitting crystal material {[Cd2(tpphz)(bdc)([mu]2-OAc)2].tpphz.2H2O}n for rapid and high-sensitivity detection of permanganate ions

A technology of permanganate and luminescent crystal, applied in luminescent materials, material analysis by optical means, analysis of materials, etc., can solve the problems of cumbersome analyte pretreatment, low sensitivity, detection range, limitation, etc., and achieve a simple synthesis route , Highly sensitive detection, easy to control effect

Active Publication Date: 2020-01-07
JIANGNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The detection of MnO by using electrochemical, spectrophotometric, optical fiber has been reported in the literature 4 - , but these methods are greatly limited by cumbersome analyte pretreatment, low sensitivity and limited detection range

Method used

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  • Preparation of light-emitting crystal material {[Cd2(tpphz)(bdc)([mu]2-OAc)2].tpphz.2H2O}n for rapid and high-sensitivity detection of permanganate ions
  • Preparation of light-emitting crystal material {[Cd2(tpphz)(bdc)([mu]2-OAc)2].tpphz.2H2O}n for rapid and high-sensitivity detection of permanganate ions
  • Preparation of light-emitting crystal material {[Cd2(tpphz)(bdc)([mu]2-OAc)2].tpphz.2H2O}n for rapid and high-sensitivity detection of permanganate ions

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1: A kind of luminescent crystal material {[Cd 2(tpphz)(bdc)(μ 2 -OAc) 2 ]·tpphz·2H 2 O} n The preparation comprises the following steps:

[0028] In the first step, 0.025mmol tetrapyrido[3,2-a:2′,3′-c:3″,2″-h:2″′,3″′-j]phenazine, 0.05mmol cadmium nitrate Add 0.1mmol terephthalic acid to a mixed solvent of 3mL N,N-dimethylacetamide and 2mL water and stir to obtain a stable suspension;

[0029] In the second step, the suspension prepared in the first step is placed in a closed reaction kettle and heated to 170°C for 84 hours, and then slowly cooled to room temperature at a rate of 2°C / h, then filtered, washed, and dried to obtain crystals Material.

[0030] Permanganate ion detection performance test: Disperse the prepared crystal material (2mg) into 20mL of deionized water, take 2mL of suspension, add different volumes of permanganate ion aqueous solution (2mmol / L) to it, and separate them at 383nm The fluorescence intensity was tested under excitation...

Embodiment 2

[0032] Embodiment 2: A luminescent crystal material {[Cd 2 (tpphz)(bdc)(μ 2 -OAc) 2 ]·tpphz·2H 2 O} n The preparation comprises the following steps:

[0033] In the first step, 0.02mmol tetrapyrido[3,2-a:2′,3′-c:3″,2″-h:2″′,3″′-j]phenazine, 0.05mmol cadmium nitrate Add 0.15mmol terephthalic acid to a mixed solvent of 4mL N,N-dimethylacetamide and 2mL water and stir to obtain a stable suspension;

[0034] In the second step, the suspension prepared in the first step is placed in a closed reaction kettle and heated to 170°C for 84 hours, and then slowly cooled to room temperature at a rate of 2°C / h, then filtered, washed, and dried to obtain crystals Material.

[0035] Permanganate ion detection performance test: Disperse the prepared crystal material (2mg) into 20mL of deionized water, take 2mL of suspension, add different volumes of permanganate ion aqueous solution (2mmol / L) to it, and separate them at 383nm The fluorescence intensity was tested under excitation light....

Embodiment 3

[0037] Embodiment 3: A luminescent crystal material {[Cd 2 (tpphz)(bdc)(μ 2 -OAc) 2 ] The preparation comprises the following steps:

[0038] In the first step, 0.02mmol tetrapyrido[3,2-a:2′,3′-c:3″,2″-h:2″′,3″′-j]phenazine, 0.05mmol cadmium nitrate Add 0.15mmol terephthalic acid to a mixed solvent of 4mL N,N-dimethylacetamide and 2mL water and stir to obtain a stable suspension;

[0039] In the second step, the suspension prepared in the first step is placed in a closed reaction kettle and heated to 190°C for 80 hours. After slowly cooling down to room temperature at a rate of 5°C / h, the crystal is obtained by filtering, washing and drying. Material.

[0040] Permanganate ion detection performance test: Disperse the prepared crystal material (2mg) into 20mL of deionized water, take 2mL of suspension, add different volumes of permanganate ion aqueous solution (2mmol / L) to it, and separate them at 383nm The fluorescence intensity was tested under excitation light.

[0041...

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Abstract

The invention discloses preparation of a light-emitting crystal material {[Cd2(tpphz)(bdc)([mu]2-OAc)2].tpphz.2H2O}n for rapid and high-sensitivity detection of permanganate ions. The preparation method comprises: adding tetrapyrido[3,2-a:2',3'-c:3'',2''-h:2''',3'''-j]phenazine, cadmium nitrate and terephthalic acid into water,stirring in N,N-dimethylacetamideto obtain a stable suspension, puttingthe suspension into a closed reaction kettle, carrying out a heating reaction, slowly cooling to a room temperature, filtering, washing, and drying to obtain the light-emitting crystal material. According to the invention, with the preparation method, the light-emitting crystal material {[Cd2(tpphz)(bdc)([mu]2-OAc)2].tpphz.2H2O}n for rapid and high-sensitivity detection of permanganate ions is obtained.

Description

[0001] a technical field [0002] The invention relates to the preparation of strong oxidative compound detection materials, in particular to a luminescent crystal material {[Cd 2 (tpphz)(bdc)(μ 2 -OAc) 2 ]·tpphz·2H 2 O} n [H 2 bdc=terephthalic acid; tpphz=tetrapyrido[3,2-a:2′,3′-c:3″,2″-h:2″′,3″′-j]phenazine; HOAc= Acetic acid] preparation. [0003] Two background technology [0004] Due to the rapid development of industry, anionic pollutants have also become a pressing environmental problem. The strong oxidizing permanganate ion (MnO 4 - ) has been included in the US Environmental Protection Agency (EPA) list. MnO 4 - Commonly used as a laboratory chemical, it is also widely used as a disinfectant for water treatment, skin infections, and aquaculture. However, excess MnO 4 - It can cause ecological risks and human health problems, including respiratory infections, cardiovascular failure and gastrointestinal discomfort. Therefore, the rapid and sensitive detect...

Claims

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Application Information

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IPC IPC(8): C07F3/08C09K11/06G01N21/64
CPCC07F3/08C09K11/06C09K2211/188G01N21/643G01N2021/6432
Inventor 张金方贾雯任思猛
Owner JIANGNAN UNIV
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