Fluorescent reagent for detecting trace carbon dioxide and preparation method thereof

A fluorescent reagent and carbon dioxide technology, applied in the field of fluorescent sensors, can solve the problems of high energy consumption, limited use, and high cost, and achieve the effects of reduced fluorescence intensity, simple preparation method, and convenient operation

Inactive Publication Date: 2014-09-24
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have been maturely used by people more than 50 years ago. However, with the passage of time, people have higher and higher requirements for the detection of carbon dioxide. Operating in a complex and harsh environment, the above-mentioned traditional detection ...

Method used

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  • Fluorescent reagent for detecting trace carbon dioxide and preparation method thereof
  • Fluorescent reagent for detecting trace carbon dioxide and preparation method thereof
  • Fluorescent reagent for detecting trace carbon dioxide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Preparation of TPP-DMAE

[0036] Dissolve 100 mg of methyl 4,4',4"-(1H-pyrrole-1,2,5-tri)tribenzoate in 10 mL of N,N-dimethylethanolamine (8.9 g), add 3 mg of hydrogen Sodium oxide solid was heated to 70°C for 24 hours to prepare a white solid powder; the NMR and mass spectrometry data of the solid powder obtained by NMR spectrometer and mass spectrometer were as follows:

[0037] 1 H-NMR (400MHz, CDCl 3 )δ(ppm):7.98-7.96(d,2H),7.87-7.85(d,4H),7.09-7.07(d,6H),6.60(s,2H),4.50(d,6H),2.87(d ,6H),2.47(d,18H).MS(MALDI-TOF):calcd.for C 37 h 44 4O 6 ,640.3;found,641.3;

[0038] The solid powder is TPP-DMAE described in the present invention.

[0039] (2) Preparation of TPP-DMAE fluorescent reagent

[0040] Dissolve 16 mg of TPP-DMAE in 20 mL of THF to make a concentration of 1.25 × 10 -3Mother liquor of M. Take 16mL of the mother liquor and add it to the sample bottle, then add 4mL of deionized water to the sample bottle, and shake evenly to obtain the TPP-DMAE f...

Embodiment 2

[0044] (1) Preparation of TPP-DMAE

[0045] Dissolve 100 mg of methyl 4,4',4"-(1H-pyrrole-1,2,5-tri)tribenzoate in 4.5 mL of N,N-dimethylethanolamine (4.0 g), add 1 mg Sodium hydroxide solid was heated to 130°C for 10 hours to prepare a white solid powder; the NMR and mass spectrometry data of the solid powder were obtained through nuclear magnetic resonance spectrometer and mass spectrometer as follows:

[0046] 1 H-NMR (400MHz, CDCl 3 )δ(ppm):7.98-7.96(d,2H),7.87-7.85(d,4H),7.09-7.07(d,6H),6.60(s,2H),4.50(d,6H),2.87(d ,6H),2.47(d,18H).MS(MALDI-TOF):calcd.for C 37 h 44 4O 6 ,640.3;found,641.3;

[0047] The solid powder is TPP-DMAE described in the present invention.

[0048] (2) Preparation of TPP-DMAE fluorescent reagent

[0049] Dissolve 6.4 mg of TPP-DMAE in 10 mL of THF to make a concentration of 10 -3 Mother liquor of M. Take 0.03mL of the mother liquor and add it to the sample bottle, then add 2.97mL of deionized water to the sample bottle, and shake evenly to...

Embodiment 3

[0053] (1) Preparation of TPP-DMAE

[0054] Dissolve 100 mg of methyl 4,4',4"-(1H-pyrrole-1,2,5-tri)tribenzoate in 15 mL of N,N-dimethylethanolamine (13.4 g) and add 6 mg of hydrogen Sodium oxide solid was heated to 40°C for 48 hours to prepare a white solid powder; the NMR spectrum and mass spectrum data of the solid powder were obtained through nuclear magnetic resonance spectrometer and mass spectrometer as follows:

[0055] 1 H-NMR (400MHz, CDCl 3 )δ(ppm):7.98-7.96(d,2H),7.87-7.85(d,4H),7.09-7.07(d,6H),6.60(s,2H),4.50(d,6H),2.87(d ,6H),2.47(d,18H).MS(MALDI-TOF):calcd.for C 37 h 44 4O 6 ,640.3;found,641.3;

[0056] The solid powder is TPP-DMAE described in the present invention.

[0057] (2) Preparation of TPP-DMAE fluorescent reagent

[0058] Dissolve 6.4 mg of TPP-DMAE in 10 mL of THF to make a concentration of 10 -3 Mother liquor of M. Take 0.3mL of the mother liquor and add it to the sample bottle, then add 2.7mL of deionized water to the sample bottle, oscill...

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Abstract

The invention discloses a fluorescent reagent for fluorescent detection of trace carbon dioxide and a preparation method thereof, belonging to the field of fluorescent sensors. The fluorescent reagent is composed of ethyl 4,4',4''-(1H-pyrryl-1,2,5-triyl)tri(2-dimethylamino)benzoate (TPP-DMAE for short), deionized water and a good solvent. The preparation method comprises the following steps: dissolving the TPP-DMAE in N,N-dimethylethanolamine, adding a catalyst, and reacting to obtain the TPP-DMAE; and dissolving the TPP-DMAE in a mixed solvent composed of the deionized water and good solvent to obtain the fluorescent reagent. The fluorescent reagent can quantitatively detect carbon dioxide, has the advantages of high response speed, high sensitivity and high selectivity, has favorable visual detection signals, can be completely independent from high-precision instruments according to actual demands, and can satisfy the requirements of current people for carbon dioxide detection to great extent. The preparation method is simple and convenient to operate.

Description

technical field [0001] The invention relates to a fluorescent reagent for detecting trace amounts of carbon dioxide and a preparation method thereof, in particular to a fluorescent reagent for solution fluorescent detection of trace amounts of carbon dioxide, which belongs to the field of fluorescent sensors. Background technique [0002] As a component of the atmosphere, carbon dioxide participates in the carbon cycle process in nature and the human body, and has a great impact on the global environment and human health. On the one hand, carbon dioxide is not only the main carbon source for plant photosynthesis, but also widely used in human industrial production and daily life; on the other hand, if it is not properly handled and used, carbon dioxide will cause great damage to the environment and human body. In recent years, due to the increasing production and consumption activities of human beings, the concentration of carbon dioxide in the atmosphere has gradually incre...

Claims

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Application Information

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IPC IPC(8): C09K11/06C07D207/337G01N21/64
Inventor 董宇平王焕韩天宇张亚会石建兵佟斌
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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