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Reagent for detecting mercury ion in water and its preparation method

A technology for chemical reagents and water detection, applied in the field of chemical reagents, can solve problems such as the inability of optical chemical sensors of mercury ions to be practical, and achieve the effect of expanding the scope of use, high selectivity, and rapid detection

Inactive Publication Date: 2008-01-09
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a class of highly selective, qualitative, semi-quantitative and Chemical reagent for quantitative detection of mercury ions in water and preparation method thereof

Method used

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  • Reagent for detecting mercury ion in water and its preparation method
  • Reagent for detecting mercury ion in water and its preparation method
  • Reagent for detecting mercury ion in water and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1: Preparation of rhodamine B lactam-based phenylthiourea. The structure of rhodamine B lactam phenylthiourea is as follows:

[0041]

[0042] First, rhodamine B hydrazide was synthesized by adding 1 part of rhodamine B to a round bottom flask, dissolving it with 40 parts of methanol (the first organic solvent), and then adding 15 parts of 80% hydrazine hydrate. Heat to reflux until the purple color of rhodamine B disappears; filter and wash the obtained solid with water to obtain white rhodamine hydrazide, yield: 75%.

[0043] 1 H NMR (CDCl3): δ7.93 (m, 1H, ArH), 7.45 (m, 2H, ArH), 7.11 (m, 1H, ArH), 6.46 (d, 2H, xanthene-H), 6.42 (d, 2H, xanthene-H), 6.29(dd, 2H, xanthene-H), 3.61(s, 2H, NH2), 3.34(q, 8H, NCH 2 CH 3 ), 1.17(t, 12H, NCH 2 CH 3 ).

[0044] ESI MS, C 28 h 32 N 4 o 2 , m / z: 457.3 ([M+H] + ).

[0045] Synthesis of rhodamine B-lactamyl phenylthiourea: In a round bottom flask, add 1 part of rhodamine B hydrazide compound to 40 parts o...

Embodiment 2

[0049] Example 2: Preparation of rhodamine B lactam p-methoxyphenylthiourea. The structure of rhodamine B lactam p-methoxyphenylthiourea is as follows:

[0050]

[0051] First, rhodamine B hydrazide was synthesized by adding 1 part of rhodamine B to a round bottom flask, dissolving it with 40 parts of methanol (the first organic solvent), and then adding 15 parts of 80% hydrazine hydrate. Heat to reflux until the purple color of rhodamine B disappears; filter and wash the obtained solid with water to obtain white rhodamine hydrazide, yield: 65%.

[0052] Synthesis of rhodamine B lactam-based p-methoxyphenylthiourea: In a round-bottomed flask, add 1 part of rhodamine B hydrazide compound to 45 parts of CH 3 CN (the second organic solvent) is dissolved; then add 3 parts of p-methoxyphenyl isothiocyanate. After the mixture was heated to reflux for 5 hours, the CH 3 CN, separated by column chromatography, the target product was obtained, yield: 25%.

[0053] ESI MS, C 36 h...

Embodiment 3

[0054] Example 3: Preparation of rhodamine B lactam p-nitrophenylthiourea. The structure of rhodamine B lactam p-nitrophenylthiourea is as follows:

[0055]

[0056]First, rhodamine B hydrazide was synthesized: 1 part of rhodamine B was added to a round bottom flask, dissolved with 40 parts of ethanol (the first organic solvent), and then 15 parts of 80% hydrazine hydrate was added. Heat to reflux until the purple color of rhodamine B disappears; filter and wash the obtained solid with water to obtain white rhodamine hydrazide, yield: 65%.

[0057] Synthesis of rhodamine B lactam-based p-nitrophenylthiourea: In a round-bottomed flask, add 1 part of rhodamine B hydrazide compound to 50 parts of CH 3 CN (the second organic solvent) dissolved; then add 3 parts of p-nitrophenyl isothiocyanate. After the mixture was heated to reflux for 6 hours, CH was removed 3 CN, separated by column chromatography to obtain the target product, yield: 30%.

[0058] ESI MS, C 35 h 36 N 6...

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Abstract

The present invention relates to a chemical reagent for detecting mercury ion in water and its preparation method. Said invention provides the structural formula of said reagent, and its preparation method includes the following steps: firstly, synthesizing rhodamine hydrazide, adding rhodamine dye in container, dissolving by using organic solvent, adding hydrazine hydrate, heating to make reflux reaction until the rhodamine dye colour is eliminated, filtering, washing the obtained solid by using water to obtain rhodamine hydrazide compound, adding organic solvent to dissolve said compound, adding aryl isothiocyanate, heating mixture and making reflux reaction, removing organic solvent, using column chromatography to make separation so as to obtain target product.

Description

technical field [0001] The invention relates to a chemical reagent, in particular to a highly selective chemical reagent capable of qualitatively, semiquantitatively and quantitatively detecting mercury ions in water and a preparation method thereof. Background technique [0002] Mercury is a chemical substance with severe physiological toxicity. Due to its persistence, easy migration and high bioaccumulation, it has become one of the most concerned environmental pollutants in the world. On February 3, 2003, the United Nations Environment Program (UNEP) published a report on "Global Mercury Status Assessment" in Nairobi. The report pointed out that since the industrial revolution, the content of mercury in the global atmosphere, water and soil has increased by about 3 times, and the content of mercury near industrial areas is even higher. [0003] Mercury is widely used in various industrial production processes based on its unique chemical and physical properties, such as ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02C08G12/12
Inventor 郑洪钱振华许金钩
Owner XIAMEN UNIV
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