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Attapulgite clay-thiocoumarin functional hybrid material and preparation method and application

A technology of thiocoumarin and hybrid materials, which is applied in the field of heavy metal detection, can solve problems such as poor stability, secondary pollution, and difficulty in recycling, and achieve the effects of improved stability, good preservation, and enhanced fluorescence intensity

Active Publication Date: 2019-10-29
HUAIYIN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Coumarin fluorescent probes include monoamine oxidase, β-lactamase genes, hydrogen peroxide, CN ions, etc. At present, there are still many defects in fluorescent probes based on fluorescent dyes, such as: poor stability , Difficult to recycle, mostly detected in the organic phase, which easily leads to secondary pollution, etc.

Method used

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  • Attapulgite clay-thiocoumarin functional hybrid material and preparation method and application
  • Attapulgite clay-thiocoumarin functional hybrid material and preparation method and application
  • Attapulgite clay-thiocoumarin functional hybrid material and preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 1. Synthesis of Thiocoumarin

[0041]

[0042]Coumarin 6 (0.35 g, 1.0 mmol) and Lawson's reagent (0.81 g, 2.0 mmol) were added into two-necked flasks respectively, and then 15 ml of anhydrous toluene was added into the flasks to form a mixture. A rotor was placed in the flask and the flask was placed in a thermostatically heated magnetic stirrer. A cooling water circulation device was set up, and the mixture was heated to 120 °C under nitrogen protection, and the reaction was continued for 1 day. After the reaction was completed, it was cooled to room temperature.

[0043] The reaction product was extracted with dichloromethane and water, and the resulting product was purified by column chromatography (developing agent ratio PE:DCM=1:2~1:3) to obtain the thio derivative of coumarin (0.23 g, 62%). The high resolution mass spectrum is as follows: 1 H NMR (300 MHz, CDCl 3 ) δ 8.96 (br d, J = 0.6 Hz, 1H), 8.01 (d, J = 8.1 Hz, 1H),7.95(d, J = 7.8 Hz, 1H), 7.53 (d,...

Embodiment 2

[0051] Example 2: Preparation of attapulgite-thiocoumarin functional hybrid material

[0052] Attapulgite pretreatment:

[0053] Roll the raw ore, grind the attapulgite after passing through a 200-mesh sieve, grind for 5-10 minutes, add deionized water to the attapulgite for beating, and centrifuge to remove the non-clay impurities in the lower layer. The beating speed is 8000rpm, and the beating time is 40min; the centrifugal speed is 3000rpm, centrifugation time is 40min, repeat the beating and centrifuging operation 3~4 times; put the paste-like attapulgite obtained after the above beating and centrifugation into the refrigerator for 6~7 hours, take it out and thaw, and use the attapulgite sample after thawing Squeeze the roller for 5-6 times in the roller machine, scrape off the sample after the roller and replace it with isopropanol solvent to obtain the pretreated attapulgite;

[0054] The isopropanol solvent replacement step is as follows: disperse the sample after the...

Embodiment 3

[0058] Example 3: Preparation of attapulgite-thiocoumarin functional hybrid material

[0059] Attapulgite pretreatment:

[0060] Roll the raw ore, grind the attapulgite after passing through a 200-mesh sieve, grind for 5-10 minutes, add deionized water to the attapulgite for beating, and centrifuge to remove the non-clay impurities in the lower layer. The beating speed is 12000 rpm, and the beating time is 20 minutes; 4000 rpm, centrifugation time is 20min, repeat the beating and centrifuging operation 3~4 times; put the paste-like attapulgite obtained after the above beating and centrifugation into the refrigerator for 6~7 hours, take it out and thaw it, and put the thawed attapulgite The sample is squeezed 5 to 6 times with the pair of rollers, and the sample after the pair of rollers is scraped off and replaced with isopropanol solvent to obtain the pretreated attapulgite;

[0061] The isopropanol solvent replacement step is as follows: disperse the sample after the roller...

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Abstract

The invention discloses an attapulgite clay-thiocoumarin functional hybrid material, which is characterized in that it is prepared by hybridizing a thiocoumarin fluorescent dye having a molecular sizematching the size of an attapulgite clay pore, and the attapulgite clay under a certain condition; the material can be subjected to a specific selective fluorescence reaction with mercury ions, so that the fluorescence intensity at a certain wavelength is significantly improved; further, the material can produce an eye-recognizable color reaction so as to be used in the detection of mercury ionsto detect mercury contamination in water. The invention also discloses a method for preparing the attapulgite clay-thiocoumarin functional hybrid material, comprising an attapulgite clay preprocessingstep and a wet hybridization step. The processed attapulgite clay has a greatly increased specific area. The isopropyl alcohol wet hybridization can effectively promote the dissociation of the attapulgite clay and further promote the combination with the dye. The high-temperature baking promotes the dehydration of the attapulgite clay and promotes the hybridization of the thiocoumarin and the attapulgite clay.

Description

technical field [0001] The invention belongs to the technical field of heavy metal detection, and relates to a fluorescent material for detecting mercury ions in water or soil, in particular to an attapulgite-thiocoumarin functional hybrid material and a preparation method and application thereof. Background technique [0002] The main source of heavy metal pollution is industrial pollution, followed by traffic pollution and household waste pollution. Industrial heavy metal pollution is mostly discharged into the environment through "three wastes", and accumulates and persists in the environment. There are many types of heavy metal pollution, Cd 2+ , Hg 2+ , Pb 2+ is its main component. At present, these three heavy metal ions that have a great impact on food safety have seriously affected my country's food exports. Among them, the harm of mercury pollution is particularly serious. [0003] Mercury is often called mercury, and mercury and its compounds are highly toxic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64C09K11/06C09B57/02
CPCC09B57/02C09K11/06C09K2211/1037C09K2211/1088G01N21/64G01N21/6428G01N21/643G01N2021/6417G01N2021/6439
Inventor 王志辉陈强张济李万庆杨波陈静丁师杰蔡鹏茆平
Owner HUAIYIN INSTITUTE OF TECHNOLOGY
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