Preparation method of high-selectivity Hg<2+> color indicator based on Rhodamine B thiohydrazine derivative

A technology of thiohydrazide and color indication, which is applied in the direction of material analysis by observing the influence on chemical indicators, measurement of color/spectral characteristics, analysis by making materials undergo chemical reactions, etc., which can solve the problem of detection sensitivity and applicability Range limitations, poor solubility, unsatisfactory combination of mercury ions and color indicators, etc., to achieve strong anti-interference ability, low detection limit, and high sensitivity

Inactive Publication Date: 2015-05-13
TONGJI UNIV
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Problems solved by technology

[0011] However, most of the currently studied mercury ion color indicators use the principle of complexing metal ions with organic groups, so most of the color indicators are molecules containing organic heterocycles, and their solubility in aqueous solution is not ideal.
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  • Preparation method of high-selectivity Hg&lt;2+&gt; color indicator based on Rhodamine B thiohydrazine derivative
  • Preparation method of high-selectivity Hg&lt;2+&gt; color indicator based on Rhodamine B thiohydrazine derivative
  • Preparation method of high-selectivity Hg&lt;2+&gt; color indicator based on Rhodamine B thiohydrazine derivative

Examples

Experimental program
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Embodiment 1

[0036] Add 5 g of rhodamine B and 15 mL of absolute ethanol into a 100 mL reaction flask, stir well to completely dissolve rhodamine B, add 3 g of hydrazine monohydrate dropwise while maintaining stirring, and store at 80 °C under nitrogen protection React for 12 h. After the reaction, the reaction bottle was cooled to room temperature, filtered to obtain a light-colored solid powder, and finally the light-colored powder was repeatedly washed with absolute ethanol until it was colorless, and then dried with anhydrous sodium sulfate for 24 h to obtain a Hydrazinated rhodamine B derivatives with a yield of 79%.

[0037] Weigh 3 g of rhodamine B hydrazine and 7.5 mL of absolute ethanol into a 100 mL reaction flask, stir well to completely dissolve rhodamine B, add 2.6 g of Lowe’s reagent dropwise while maintaining stirring, and place under nitrogen protection React at 80°C for 6 h. After the reaction, cool the reaction bottle to room temperature, filter to obtain a light-colored ...

Embodiment 2

[0040] Embodiment 2: same as embodiment 1, but the volume ratio of water and ethanol becomes 3: 1 in the step (2).

Embodiment 3

[0041] Embodiment 3: same as embodiment 1, but the volume ratio of water and ethanol becomes 5: 1 in the step (2).

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Abstract

The invention relates to a preparation method for a high-selectivity Hg<2+> color indicator based on a Rhodamine B thiohydrazine derivative. The preparation method comprises the following steps: performing condensation reaction on Rhodamine B and hydrazine monohydrate to generate Rhodamine B hydrazine; performing reaction on the Rhodamine B hydrazine and a Lawesson reagent; after replacing a carbonyl oxygen atom in the Rhodamine B hydrazine with a sulphur atom capable of selectively identifying heavy metal Hg<2+>, obtaining the Rhodamine B thiohydrazine derivative, wherein a water-ethanol mixed solution based on the Rhodamine B thiohydrazine derivative can be taken as an Hg<2+> color indicator. The high-selectivity Hg<2+> color indicator based on the Rhodamine B thiohydrazine derivative can be used for quickly analyzing the content of appointed Hg<2+> in a water sample; the high-selectivity color indicator has high anti-interference capability to other metal ions, a suitable pH range is from weak acidity to neutrality; the high-selectivity Hg<2+> color indicator has the advantages of simple synthesis process, low cost, simpleness and convenience in operation, good selectivity, high sensitivity, high response speed, low limit of detection, wide application prospect and the like, and can be applied to real-time and quick measurement of complex samples.

Description

technical field [0001] The present invention relates to a mercury ion (Hg 2+ ) detection agent, specifically a highly selective Hg based on rhodamine B thiohydrazide derivatives 2+ Preparation method of color indicator. Background technique [0002] Mercury is a very harmful environmental pollutant. In recent years, my country's "Heavy Metal Pollution Comprehensive Prevention and Control Plan" and "Twelfth Five-Year Plan for Joint Prevention and Control of Air Pollution in Key Areas" have included mercury pollution and its comprehensive prevention and control as priorities. field. It is clearly pointed out in the plan: During the "Twelfth Five-Year Plan" period, it is necessary to establish a calculation model for the emission inventory of typical coal-fired units, and carry out online monitoring and testing of atmospheric mercury emissions from coal-fired power plants; At the same time, control mercury pollution, achieve joint control of multiple pollutants, and conduct...

Claims

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Application Information

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IPC IPC(8): G01N21/78G01N21/33
Inventor 杨正龙
Owner TONGJI UNIV
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