Synthetic method and application of MOFs (metal-organic frameworks) with fluorescence property

A technology with organic framework and fluorescent properties, which is applied in the direction of luminescent materials, material analysis through optical means, and analysis of materials, etc. It can solve the problems of complex extraction and purification procedures, and achieve simple and fast detection steps, stable performance, and fast response. Effect

Inactive Publication Date: 2017-06-30
ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims at the disadvantages of complex extraction and purification procedures in the existing detection methods, and the analytical instruments required for the determination are expensive, etc., and provides a method for synthesizing metal-organic frameworks (MOFs) with fluorescence properties and using the metal-organic Application of Framework Materials (MOFs) for Fast and Easy Pesticide Residue Detection

Method used

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  • Synthetic method and application of MOFs (metal-organic frameworks) with fluorescence property
  • Synthetic method and application of MOFs (metal-organic frameworks) with fluorescence property
  • Synthetic method and application of MOFs (metal-organic frameworks) with fluorescence property

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Experimental program
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Effect test

Embodiment 1

[0036] Step 1, take middle-tetrakis (4-carboxyphenyl) porphine 160mg or 0.201mmol, 1,2,4,5-tetrakis (4-carboxyphenyl) benzene 223mg or 0.399mmol and Zn(NO 3 ) 2 ·6H 2 O 131mg or 0.440mmol in a beaker, then add N,N-dimethylformamide 34mL, ultrasonic 15min to make it mix into a uniform dispersion;

[0037] Step 2. Pour the dispersion described in step 1 into the reaction kettle, and react at a temperature of 110° C. for 36 hours;

[0038] Step 3, centrifuging the product reacted in step 2 to remove the upper layer liquid, adding ethanol and repeating centrifugal washing for more than 3 times; the rotating speed is 8000r / min, and the rotating speed time is 5min;

[0039] Step 4. Dry the product after the reaction in step 3 at a temperature of 80° C. for 18 hours to obtain a reddish-brown MOFs solid powder.

Embodiment 2

[0041] Step 1, take middle-tetrakis (4-carboxyphenyl) porphine 160mg or 0.201mmol, 1,2,4,5-tetrakis (4-carboxyphenyl) benzene 223mg or 0.399mmol and Zn(NO 3 ) 2 ·6H 2 O 131mg or 0.440mmol in a beaker, then add N,N-dimethylformamide 34mL, ultrasonic 15min to make it mix into a uniform dispersion;

[0042] Step 2. Pour the dispersion described in step 1 into the reaction kettle, and react at a temperature of 100° C. for 24 hours;

[0043] Step 3, centrifuging the product after the reaction in step 2 to remove the upper layer liquid, adding ethanol and repeating the centrifugal washing for more than 3 times; the rotation speed is 6000r / min, and the rotation speed time is 4min;

[0044] Step 4. Dry the product after the reaction in step 3 at a temperature of 60° C. for 12 hours to obtain a reddish-brown MOFs solid powder.

Embodiment 3

[0046] Step 1, take middle-tetrakis (4-carboxyphenyl) porphine 160mg or 0.201mmol, 1,2,4,5-tetrakis (4-carboxyphenyl) benzene 223mg or 0.399mmol and Zn(NO 3) 2 ·6H 2 O 131mg or 0.440mmol in a beaker, then add N,N-dimethylformamide 34mL, ultrasonic 15min to make it mix into a uniform dispersion;

[0047] Step 2. Pour the dispersion described in step 1 into the reaction kettle, and react at a temperature of 120° C. for 48 hours;

[0048] Step 3, centrifuging the product reacted in step 2 to remove the upper layer liquid, adding ethanol and repeating centrifugal washing for more than 3 times; the rotating speed is 10000r / min, and the rotating speed time is 6min;

[0049] Step 4. Dry the reaction product of step 3 at a temperature of 100° C. for 24 hours to obtain a reddish-brown MOFs solid powder.

[0050] An application of a metal-organic framework material (MOFs) with fluorescent properties in the rapid detection of parathion in pesticide residues, the detection method steps...

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Abstract

The invention discloses a synthetic method of MOFs (metal-organic frameworks) with good fluorescence property and an application of the MOFs to detection of parathion in pesticide residues. The synthetic method comprises the following steps: porphyrin with a large conjugated structure, 1,2,4,5-tetrakis(4-carboxyphenyl)benzene and Zn(NO3)2.6H2O are fed to a beaker, then N,N-dimethylformamide is added, and the substances are mixed ultrasonically; the uniformly mixed solution is poured into a reactor for a reaction; a reaction product is centrifuged, an upper liquid is removed, and ethyl alcohol is added, and the reaction product is subjected to repeated centrifugal washing three times or more; solid powder of the MOFs is obtained after high-temperature drying. Parathion has a specific quenching effect on fluorescence signals of the MOFs, and fluorescence quenching is more obvious when more parathion is added; when the concentration of parathion is in the range of 5-1,000 ppb, the fluorescence intensity in inverse proportion to the logarithm of the parathion concentration, and high-sensitivity and high-specificity detection of parathion is realized.

Description

technical field [0001] The invention belongs to the field of pesticide residue detection, in particular to a method for synthesizing metal-organic framework materials (MOFs) with fluorescent properties, and also relates to an application of the metal-organic framework materials (MOFs) in detecting pesticide residues . Background technique [0002] Parathion (O, O-diethyl-O-(4-nitrophenyl) phosphorothioate), is a broad-spectrum highly toxic organophosphate insecticide and acaricide, parathion It is highly toxic to humans and animals, and the residues in food and vegetables often exceed the standard seasonally, so poisoning incidents often occur. The widespread use of parathion will cause harm to humans and the environment. Therefore, many countries and regions have banned parathion and listed it as an important detection object for crop pesticide residues. [0003] Traditional analysis methods for parathion in the prior art include gas chromatography, high pressure liquid c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C09K11/06G01N21/64
CPCC08G83/008C09K11/06C09K2211/188G01N21/6428
Inventor 徐霞红王新全王祥云王强杨华郭玉娜齐沛沛汪志威何开雨
Owner ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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