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Preparation method and application of 9,9'-(4,4'-biphenyl)bisfluorone bromination reagent

A technology of bifluorone and biphenyl, which is applied in the direction of fluorescence/phosphorescence, chemical instruments and methods, and luminescent materials, can solve the problems of unsatisfactory sensitivity and selectivity, and achieve improved sensitivity, fast response, and simple preparation methods Effect

Inactive Publication Date: 2015-09-16
SHANXI DATONG UNIV
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Problems solved by technology

[0004] The present invention provides a 9,9'-(4,4'-biphenyl)bisfluorone brominated reagent and its Preparation method and application

Method used

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  • Preparation method and application of 9,9'-(4,4'-biphenyl)bisfluorone bromination reagent
  • Preparation method and application of 9,9'-(4,4'-biphenyl)bisfluorone bromination reagent
  • Preparation method and application of 9,9'-(4,4'-biphenyl)bisfluorone bromination reagent

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Experimental program
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Embodiment

[0030] Such as figure 2 As shown, a 9,9'-(4,4'-biphenyl)bisfluorone brominated reagent, referred to as 9,9'-QBBPBF, has a molecular structure of

[0031] .

[0032] Such as image 3 Shown, the preparation method of 9,9'-QBBPBF comprises the following steps:

[0033] (1) Synthesis of p-benzoquinone: Dissolve 60g of hydroquinone in 1000mL of water at 50°C, cool to a temperature of 20°C, and slowly add 32mL of concentrated H 2 SO 4 , stir vigorously, control the reaction temperature ≤ 30°C, add 400mL of K with a concentration of 0.2g / ml dropwise at a rate of 0.5~1.0mL / min 2 Cr 2 o 4 The solution was cooled to room temperature after the dropwise addition, filtered with suction, and the precipitate was washed with deionized water until the filtrate was light yellow, and the precipitate was dried at 80°C to obtain 32.3 g of yellow p-benzoquinone with a yield of 54%;

[0034] (2) Synthesis of trimerol triacetate: In a 100mL beaker, add 28.0mL acetic anhydride and 1.0mL conc...

experiment example 1

[0037] Experimental example 1: Photometric analysis and detection of Mo(VI) in alkaline medium.

[0038] In a 25mL volumetric flask, add 5μg Mo(VI) standard solution, 2.0% Triton X-100 aqueous solution 2.0mL, 0.3g / L 9,9'-QBBPBF ethanol solution 3.0mL, pH8.0 borax- Sodium hydroxide buffer solution 1.5mL, dilute to the mark with water, shake well, take the blank reagent as a reference, measure the absorbance of the complex at 670nm with a 1cm cuvette, the apparent molar absorptivity is 1.9×10 5 L·mol -1 cm -1 . The comparison results of the sensitivity of Mo(VI) measured by the photometric analysis method of the present invention and the sensitivity of molybdenum measured by existing similar reagents are shown in Table 1, and the results show that the photometric method of the present invention for molybdenum ions has high sensitivity.

[0039] Table 1: Sensitivity of several reagents for determination of molybdenum

[0040]

[0041] The comparison results of the sensitiv...

experiment example 2

[0047] Experimental Example 2: Fluorescent detection of Mn(II) by 9,9'-QBBPBF.

[0048] Sample processing: According to the method in the literature [Du Rongshan, Huang Liping, Journal of Analytical Science, 2010, 26(5), 535-538], take two different urine samples of 100 mL each, and place them in Erlenmeyer flasks respectively. Add 25.0mL concentrated nitric acid, 4.0mL perchloric acid, heat and digest until colorless, and concentrate to 1.0-2.0mL. Take it off to cool, add a small amount of water, transfer to a 10mL centrifuge tube, and wash the Erlenmeyer flask twice with a small amount of twice distilled water, and pour the washing solution into the centrifuge tube. Centrifuge at 8000r / min for 10min, then transfer all the supernatant into a beaker, and use 0.2mol / L NH 3 ·H 2 O to neutralize to PH=7.0, finally dilute to 100mL volumetric flask, shake well. Take 5.00mL of the test solution, add 1.00mL167μg / mL ascorbic acid solution, the Fe in the sample 3+ reduced to Fe 2+...

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Abstract

The invention belongs to the technical field of phenylfluorone compounds, and provides a 9,9'-(4,4'-biphenyl)bisfluorone bromination reagent, and a preparation method and an application thereof in order to solve the problem of unsatisfactory sensitivity and selectivity of reagents for detection of heavy metal ions in the prior art. 4,4'-Biphenyldicarboxaldehyde with a large conjugated system reacts with 1,2,4-trihydroxybenzene triacetate to synthesize the novel bisfluorone reagent with a larger conjugated system, so the sensitivity and the fluorescence characteristic of the reagent are enhanced. The 9,9'-(4,4'-biphenyl)bisfluorone bromination reagent can be used in detection of Mo (VI) ions under alkaline conditions and fluorescence detection of Mn (II). The reagent is a highly-selective and highly-selective fluorescence analysis reagent for detecting Mo (VI) and Mn (II), and is a luminosity analysis developer with a good analysis performance.

Description

technical field [0001] The invention belongs to the technical field of phenylfluorone compounds, and in particular relates to a preparation method and application of a 9,9'-(4,4'-biphenyl)bisfluorone bromide derivative. Background technique [0002] The fluorone reagent refers to a class of triphenylmethane derivatives containing a 2,3,7-trihydroxy-6-keto-pyran ring structure in the molecule. The compound formed when the 9-position hydrogen atom is replaced by phenyl, also known as phenylfluorone (structure such as figure 1 ). Phenylfluorone is mostly orange or red crystals, hardly soluble in water and cold ethanol, but easily soluble in acidified ethanol. The compound has strong fluorescence due to its large conjugated system. Since there are 3 hydroxyl groups at the 2, 3 and 7 positions, and the oxygen atom in the hydroxyl group has 2 lone pairs of electrons, it is easy to form a coordination bond with the empty orbital of the metal ion, so it can form a complex with a ...

Claims

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Application Information

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IPC IPC(8): C07D311/82C09K11/06G01N21/64
CPCC07D311/82C09K11/06C09K2211/1088G01N21/6428
Inventor 解海樊月琴
Owner SHANXI DATONG UNIV
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