A kind of rare earth ionic liquid and its preparation method and its application in detecting ferric ion

A technology of rare earth ions and ferric iron, applied in chemical instruments and methods, measuring devices, instruments, etc., can solve the problems of endangering inspectors' health, inconvenient production and use, harmful environment, etc., and achieves convenient and fast detection process and high detection effect Good, short synthetic cycle effect

Active Publication Date: 2017-05-24
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, fluorescein is an organic substance and is slightly soluble in water, so it needs to be used with organic solvents during use. Most organic solvents are volatile and toxic, and will cause secondary pollution to the environment during detection; Rhodamine B was found by mouse experiments It can cause sarcoma in the subcutaneous tissue and is suspected to be a carcinogen. It will endanger the health of inspectors during the test, so there are many inconveniences in production and use.
[0004] Because traditional organic solvents are highly volatile, difficult to preserve and harmful to the environment, scientists gradually classify traditional organic solvents as hazardous chemical substances

Method used

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  • A kind of rare earth ionic liquid and its preparation method and its application in detecting ferric ion
  • A kind of rare earth ionic liquid and its preparation method and its application in detecting ferric ion
  • A kind of rare earth ionic liquid and its preparation method and its application in detecting ferric ion

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Experimental program
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Effect test

Embodiment 1

[0036] The synthesis of embodiment 1 rare earth ionic liquid

[0037] 1) Synthesis of intermediate 1-butyl-3-methylimidazolium bromide

[0038] N-methylimidazole and butane bromide were distilled under reduced pressure separately for use.

[0039] Heating with a silicone oil bath to raise the temperature of N-methylimidazole to 50°C, and then adding bromobutane dropwise into the three-necked flask containing N-methylimidazole with a constant pressure dropping funnel, the molar ratio of the two is 1:1.1, after the dropwise addition, react at 50°C-60°C under reflux for about 48h. Filter and recrystallize with a mixture of acetonitrile and ethyl acetate (the volume ratio of acetonitrile and ethyl acetate is 1:2) with a total volume of 30 mL to obtain the intermediate 1-butyl-3-methylimidazolium bromide, the reaction formula is as follows :

[0040]

[0041] Intermediate 1-Butyl-3-methylimidazolium Bromide

[0042] 2) Synthesis of intermediate 1-butyl-3-methylimidazole nitr...

Embodiment 2

[0049] Example 2 Application of Rare Earth Ionic Liquids as Fluorescent Probes in Detection of Ferric Ions

[0050] Accurately add 2.5mL standard detection solution (aqueous solution of 1mol / L rare earth ionic liquid) to several cuvettes, and then add 10μL aqueous solution of 1mol / L metal cation (Zn 2+ , Pb 2+ 、Cd 2+ , Hg 2+ 、Co 2+ 、Ni 3+ 、Cr 3+ , Ca 2+ , Fe 2+ , Fe 3+ 、Cu 2+ ), so that the final concentration of metal cations is 4×10 -3 mol / L, respectively measure its fluorescence spectrum at 325nm excitation wavelength, the results are as follows figure 1 shown. Draw a histogram of the fluorescence intensity of different metal cations at 480nm, such as figure 2 shown.

[0051] From figure 1 and figure 2 It can be seen from the figure that at the excitation wavelength of 325nm, the addition of other heavy metal cations does not cause a significant change in the fluorescence intensity, only the addition of Fe 3+ After that, the fluorescence intensity of the f...

Embodiment 3

[0052] Example 3 Rare earth ionic liquid is used as a fluorescent probe to determine the detection limit of ferric ions

[0053] Accurately add 2.5mL of standard detection solution (aqueous solution of 1mol / L rare earth ionic liquid) to several cuvettes, and then add 10μL of different concentrations of Fe with a pipette gun 3+ Aqueous solutions (concentrations from low to high are 4×10 -4 , 4.5×10 -4 , 5×10 -4 , 5.5×10 -4 , 6×10 -4 , 6.5×10 -4 , 7×10 -4 , 7.5×10 -4 , 8×10 -4 , 8.5×10 -4 , 9×10 -4 、10 -3 , 2×10 -3 , 3×10 -3 , 4×10 -3 mol / L), respectively measure its fluorescence spectrum at 325nm excitation wavelength, such as image 3 shown. Draw a histogram of the fluorescence intensity at 480nm of different concentrations of ferric ions, such as Figure 4 shown.

[0054] From image 3 and Figure 4 It can be seen that as the concentration of iron ions increases, the fluorescence intensity of the fluorescent probe decreases gradually until it is quenched. ...

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Abstract

The invention relates to rare earth ion liquid as well as a preparation method and application thereof in o detection of ferric ions. According to the invention, the rare earth ion liquid [C4mim] [Dy(NO3)4] is used as a fluorescence probe, a rare earth ion liquid aqueous solution with fixed concentration is prepared to be used as standard detection liquid, and whether water contains ferric ions or not can be judged by observing whether the ionic liquid fluorescence light cancels or not under 325nm excitation wavelength. By adopting the rare earth ion liquid, the ferric ions can be exclusively recognized, interference of other heavy metal ions is avoided, the detection method is simple and fast, a detection reagent is short in synthesis period and high in yield, and when being applied to actual production, the ion liquid is an environment-friendly solvent and has a wide application prospect.

Description

technical field [0001] The invention relates to a new technology for detecting ferric ions in water, and specifically belongs to a method for qualitatively and quantitatively detecting ferric ions in water by using a rare earth ionic liquid as a fluorescent probe. Background technique [0002] Iron is an essential trace element for the human body. The water contains an appropriate amount of iron, which is beneficial and harmless to the human body; however, if the human body takes in excessive iron for a long time, it will be harmful to the human body. Excess ferric iron will combine with iron ions in the human body, reducing the iron ion content in the blood, causing anemia and dizziness in the human body. When the iron content in water is greater than 0.3mg / L, the water will become turbid, and when it exceeds 1mg / L, the water will have an iron smell. Therefore, it is of great significance to detect the concentration of iron ions in the environment in real time. [0003] ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/58C09K11/06G01N21/64
CPCC07D233/58C09K11/06C09K2211/1044G01N21/6428
Inventor 关伟樊本汉魏杰邢楠楠郑玲
Owner LIAONING UNIVERSITY
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