A kind of fluorescent sensing material based on rare earth hybrid layer, its preparation method and application

A fluorescent sensing and layered technology, applied in the field of fluorescent sensing material preparation, can solve the problems of low sensitivity and inability to detect on-site in real time, and achieve the effects of high chemical stability, convenient industrial application, and simple preparation method

Active Publication Date: 2022-08-02
HEBEI NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the problems of low sensitivity and inability to detect on-site in real time in the method for detecting copper ions in the prior art, the present invention provides a fluorescent sensing material based on a rare earth hybrid layer and its preparation method and application

Method used

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  • A kind of fluorescent sensing material based on rare earth hybrid layer, its preparation method and application
  • A kind of fluorescent sensing material based on rare earth hybrid layer, its preparation method and application
  • A kind of fluorescent sensing material based on rare earth hybrid layer, its preparation method and application

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Embodiment 1

[0045] An embodiment of the present invention provides a method for preparing a fluorescent sensing material based on a rare earth hybrid layer, which at least includes the following steps:

[0046] Step 1. NO 3 –Synthesis of LGdH:Eu solid powder:

[0047] According to the molar ratio of Gd to Eu of 1.9:0.1, take 4.75mL of 0.2mol / L Gd(NO 3 ) 3 , 0.25mL of 0.2mol / L Eu(NO 3 ) 3 , 1.1049g of NaNO 3 and 0.1402g of hexamethylenetetramine, reacted in a polytetrafluoroethylene autoclave at 90°C for 12h, centrifuged, washed and dried after the reaction to obtain NO 3 -LGdH:Eu solid powder;

[0048] The chemical reaction occurs gradually according to the following equation:

[0049] C 6 N 4 H 12 +6H 2 O→6H 2 CO+4NH 3 ………………………………… (1)

[0050] 2RE(NO 3 ) 3 +5NH 3 +(n+5)H 2 O→RE 2 (OH) 5 NO 3 ·nH 2 O↓+5NH 4 NO 3 (2)

[0051] RE=Gd,Eu

[0052] Step 2. DS 0.6 CC 0.4 –Synthesis of LGdH:Eu solid powder:

[0053] According to the molar ratio of coumarin-3-carbox...

Embodiment 2

[0057] An embodiment of the present invention provides a method for preparing a fluorescent sensing material based on a rare earth hybrid layer, which at least includes the following steps:

[0058] Step 1. NO 3 –Synthesis of LGdH:Eu solid powder:

[0059] According to the molar ratio of Gd to Eu as 1.9:0.08, take 4.75mL of 0.2mol / L Gd(NO 3 ) 3 , 0.20mL of 0.2mol / L Eu(NO 3 ) 3 , 1.0098g of NaNO 3 and 0.1402g of hexamethylenetetramine, reacted in a polytetrafluoroethylene autoclave at 95°C for 11h, centrifuged, washed and dried after the reaction to obtain NO 3 -LGdH:Eu solid powder;

[0060] Step 2. DS 0.65 CC 0.35 –Synthesis of LGdH:Eu solid powder:

[0061] According to the molar ratio of coumarin-3-carboxylic acid (CCA) and NaOH being 1:1, 0.1997g of CCA (1.05mmol) and 0.042g of NaOH were weighed, added to 70mL of deionized water, stirred and dissolved to obtain coumarin Sodium pyruvate-3-carboxylate solution;

[0062] According to the CCA:SDS molar ratio of 0.35...

Embodiment 3

[0065] An embodiment of the present invention provides a method for preparing a fluorescent sensing material based on a rare earth hybrid layer, which at least includes the following steps:

[0066] Step 1. NO 3 –Synthesis of LGdH:Eu solid powder:

[0067] According to the molar ratio of Gd to Eu as 1.7:0.11, take 4.64mL of 0.2mol / L Gd(NO 3 ) 3 , 0.30mL of 0.2mol / L Eu(NO 3 ) 3 , 1.1825g of NaNO 3 and 0.1402g of hexamethylenetetramine, reacted in a polytetrafluoroethylene autoclave at 85°C for 13h, centrifuged, washed and dried after the reaction to obtain NO 3 -LGdH:Eu solid powder;

[0068] Step 2. DS 0.55 CC 0.45 –Synthesis of LGdH:Eu solid powder:

[0069] According to the molar ratio of coumarin-3-carboxylic acid (CCA) and NaOH being 1:1, 0.2568g of CCA (1.35mmol) and 0.054g of NaOH were weighed, added to 70mL of deionized water, stirred and dissolved to obtain coumarin Sodium pyruvate-3-carboxylate solution;

[0070] According to the CCA:SDS molar ratio of 0.45...

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Abstract

The invention relates to the technical field of preparation of fluorescent sensing materials, and specifically discloses a fluorescent sensing material based on a rare earth hybrid layered substance, a preparation method and application thereof. In the present invention, sodium dodecyl sulfonate and coumarin-3-carboxylic acid are respectively used as proppant and light absorber, and are co-inserted into layered rare earth hydroxide through ion exchange and intercalation chemistry to prepare a kind of A new type of rare earth hybrid layered material, and then the prepared rare earth hybrid composite is exfoliated with formamide, and a colloidal solution of two-dimensional sheet rare earth hybrid can be obtained. The colloidal solution prepared by the present invention can exhibit Eu 3+ of 5 D 0 → 7 F 2 The red emission of the characteristic transition and the co-intercalation of organic anions significantly enhance the Eu 3+ The fluorescence intensity of the prepared colloidal solution for Cu 2+ It has high sensitivity, the detection limit can reach 0.35μM, and it is expected to be applied in the fields of biomedicine and environment.

Description

technical field [0001] The invention relates to the technical field of preparation of fluorescent sensing materials, in particular to a fluorescent sensing material based on a rare earth hybrid layer, and a preparation method and application thereof. Background technique [0002] Cu 2+ It is one of the most widely distributed metal pollutants with strong physiological toxicity in nature. It is easy to bioaccumulate through the food chain and finally enter the human body. Once it enters the human body, it will cause serious damage to the nervous system, cause cognitive impairment and emotional disturbance, and even lead to death. Therefore, the analytical detection of copper ions in environmental and biological samples has become increasingly important. At present, the commonly used methods for detecting copper ions mainly include atomic absorption spectrometry, inductively coupled plasma mass spectrometry (ICP-MS), ion exchange chromatography and other techniques, and elec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/77G01N21/64
CPCC09K11/7783G01N21/6428G01N21/643G01N2021/6432
Inventor 石士考刘璐余静洁
Owner HEBEI NORMAL UNIV
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