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Fluorescence probe for recognizing molybdate and production method and recognition method thereof

A technology of molybdate ion and fluorescent probe, which is applied in the direction of fluorescence/phosphorescence, chemical instruments and methods, luminescent materials, etc., can solve problems such as low cost, and achieve the effects of high selectivity, low recognition concentration, and strong anti-interference ability

Active Publication Date: 2019-08-16
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Fluorescent probes are reagents that identify certain ions through fluorescence changes. They have the characteristics of high selectivity, high sensitivity, low cost, and visible results. However, no fluorescent probes for the identification of molybdate ions have been reported so far.

Method used

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  • Fluorescence probe for recognizing molybdate and production method and recognition method thereof
  • Fluorescence probe for recognizing molybdate and production method and recognition method thereof
  • Fluorescence probe for recognizing molybdate and production method and recognition method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1: a kind of preparation method of the fluorescent probe of recognition molybdate ion, the steps are as follows:

[0042] (1) Add 286mg of 1,4-dibromonaphthalene, 263mg of 4-vinylpyridine, 30mg of palladium dichloride, 100mg of triphenylphosphine and 400mg of potassium carbonate into 4ml of triethylamine and mix, and seal the mixture in N 2 In a high-pressure reaction flask under atmosphere, react at 115°C for 30 hours, extract the product 3 times with dichloromethane, then extract 3 times with saturated brine, then dry with anhydrous magnesium sulfate for 1.5 hours and then spin dry. 95% ethanol was recrystallized, and then filtered and dried to obtain product A;

[0043] (2) Product A is dissolved in N,N-dimethylformamide, then 1-bromo-n-octane is added in a ratio of 1:20 according to the amount of product A and 1-bromo-n-octane, heated to 85°C, react for 22 hours, then add diethyl ether until it completely precipitates, filter with suction, wash the preci...

Embodiment 2

[0044] Embodiment 2: a kind of preparation method of the fluorescent probe of recognition molybdate ion, the steps are as follows:

[0045] (1) Add 286mg of 1,4-dibromonaphthalene, 263mg of 4-vinylpyridine, 30mg of palladium dichloride, 100mg of triphenylphosphine and 400mg of potassium carbonate into 3ml of triethylamine and mix, and seal the mixture in N 2In a high-pressure reaction flask under atmosphere, react at 110°C for 24 hours, extract the product 3 times with dichloromethane, and then extract 3 times with saturated brine, then dry it with anhydrous magnesium sulfate for 1 hour and then spin it dry with a concentration of 96 % of ethanol for recrystallization, and then filter and dry to obtain product A;

[0046] (2) Product A is dissolved in N,N-dimethylformamide, then 1-bromo-n-octane is added in a ratio of 1:20 according to the amount of product A and 1-bromo-n-octane, heated to 80°C, react for 20 h, then add diethyl ether until it completely precipitates, filter ...

Embodiment 3

[0047] Embodiment 3: a kind of preparation method of the fluorescent probe of recognition molybdate ion, the steps are as follows:

[0048] (1) Add 286mg of 1,4-dibromonaphthalene, 263mg of 4-vinylpyridine, 30mg of palladium dichloride, 100mg of triphenylphosphine and 400mg of potassium carbonate into 5ml of triethylamine and mix, and seal the mixture in N 2 In a high-pressure reaction flask under atmosphere, react at 120°C for 36 hours, extract the product 3 times with dichloromethane, and then extract 3 times with saturated brine, then dry it with anhydrous magnesium sulfate for 2 hours and spin it dry with a concentration of 96 % of ethanol for recrystallization, and then filter and dry to obtain product A;

[0049] (2) Product A is dissolved in N,N-dimethylformamide, then 1-bromo-n-octane is added in a ratio of 1:20 according to the amount of product A and 1-bromo-n-octane, heated to 90°C, react for 24 hours, then add diethyl ether until it completely precipitates, filter...

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Abstract

The invention discloses a fluorescence probe for recognizing molybdate and a production method and a recognition method thereof. The production method of the fluorescence probe comprises the steps of(1) adding 1,4-dibromonaphthalene, 4-vinyl pyridine, palladium dichloride, triphenylphosphine and potassium carbonate into triethylamine for mixing, sealing a mixture in a high-pressure reaction bottle in a N2 atmosphere, carrying out reaction at 110-120 DEG C for 24-36 h, extracting a product by using dichloromethane and a saturated salt solution, then conducting spin dry, conducting recrystallization by means of ethyl alcohol, and then conducting filtering and drying to obtain a product A; and (2) dissolving the product A in N,N-dimethylformamide, then adding 1-bromooctane, heating a mixtureto 80-90 DEG C, carrying out reaction for 20-24 h, then adding diethyl ether until a mixture completely participates, conducting suction filtering, washing a participate twice with diethyl ether, andconducting drying to obtain the probe. By means of the fluorescence probe for recognizing the molybdate and the production method and the recognition method thereof, the molybdate can be recognized,and the fluorescence probe for recognizing the molybdate and the production method and the recognition method thereof have the characters that the recognition cost is low, operation is simple, a result is visible, the sensibility is high, and the selectivity is good.

Description

technical field [0001] The invention relates to a fluorescent probe and its preparation method and identification method, in particular to a fluorescent probe for identifying molybdate ions and its preparation method and identification method. Background technique [0002] Ammonium molybdate is mainly used to smelt ferromolybdenum and produce molybdenum trioxide and metal molybdenum powder as the raw material of tungsten-molybdenum alloy and molybdenum wire, and secondly, it is used as a chemical catalyst and a small amount is used as agricultural molybdenum fertilizer. Ammonium paramolybdate is a A kind of trace element fertilizer, which can promote nitrogen fixation, and can increase the nitrogen fixation capacity to dozens to hundreds of times for legumes such as peanuts and soybeans. It is used in medicine in a very small amount. It is a component of various enzymes. The lack of molybdenum can cause dental caries, kidney stones, Keshan disease, Kashin-Beck disease, esoph...

Claims

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Application Information

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IPC IPC(8): C07D213/20C09K11/06G01N21/64
CPCC07D213/20C09K11/06G01N21/643C09K2211/1029G01N2021/6432
Inventor 王攀张晓东周桂林倪新龙
Owner GUIZHOU UNIV
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