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3,3'-dimethylthio-4,4'-bis(2,6-dichloro-4-nitrophenyldiazoamino)biphenyl and preparation method and application

A technology of diaminobiphenyl dithiazole and dimethylthio, which is applied in the field of bistriazene compounds, can solve the problems of difficult heavy metal ion fluorescence detection, large interference of coexisting ions, unsatisfactory sensitivity and selectivity, etc., and achieves selectivity. Good, improve sensitivity, enhance the effect of π electron mobility

Inactive Publication Date: 2017-10-27
SHANXI DATONG UNIV
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Problems solved by technology

[0004] The present invention provides a 3,3'- Dimethylthio-4,4'-bis(2,6-dichloro-4-nitrophenyldiazoamino)biphenyl and its preparation method and application

Method used

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  • 3,3'-dimethylthio-4,4'-bis(2,6-dichloro-4-nitrophenyldiazoamino)biphenyl and preparation method and application

Examples

Experimental program
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preparation example Construction

[0027] The preparation method of the 3,3'-dimethylthio-4,4'-bis(2,6-dichloro-4-nitrophenyldiazoamino)biphenyl comprises the following steps:

[0028] (1) Preparation of 2,2'-diaminobiphenylbithiazole: Add 18.4 g of 4,4'-diaminobiphenyl to a 500 ml three-necked flask equipped with a drying tube, condenser and dropping funnel (0.1 mol), 150 ml of glacial acetic acid and 79.6 g of potassium thiocyanate, stirred at room temperature for 20 min, then measured 9.0 ml of bromine dissolved in 120 ml of glacial acetic acid, slowly added dropwise to the reaction mixture, and kept the reaction temperature at 60°C , continue to stir and react for 22 h, pour the mixture in the three-necked flask into cold water, add ammonia to it under constant stirring, adjust the pH value to 8, let it stand, and filter and dry the solution after cooling; V 乙酸乙酯 : V 乙醇 = 1:1 mixed solution of ethyl acetate and ethanol was recrystallized, dried under vacuum at 60°C to obtain 24 g of off-white solid 2,2'...

experiment example 1

[0034] Experimental example 1: DMSDCNPDP on Hg 2+ photometric analysis.

[0035] Add the standard solution of ≤20 μg Hg (Ⅱ) to the 25 ml volumetric flask in turn, add 3.0 ml of borax-sodium hydroxide buffer solution with pH 10.0, 2.0 ml of 30 g / L TritonX-100 solution, shake well, add 0.2 g / LDMSDCNPDP DMF solution 2.0 ml, diluted with water to the mark, using the reagent blank as a reference, using a 1cm cuvette, at 560nm, measure the absorbance of the complex solution.

[0036] Treat the hair and water samples according to the method in the literature [Analytical Chemistry, Guo Zhongxian, 1996, Volume 24, No. 1, Page 65-68], add 1ml of mixed masking agent, and measure according to the test method. The results are shown in Table 1. The comparison results of the sensitivity of the present invention to mercury and the sensitivity of existing reagents to mercury are shown in Table 2, and the results show that the compound of the present invention has high detection sensitivity fo...

experiment example 2

[0042] Experimental example 2: Determination of lead (II) by DMSDCNPDP fluorescence quenching method: in a 25 ml volumetric flask, add 1.2×10 lead ions in sequence -9 ~1.6×10 -7 mol / L lead (Ⅱ) solution, 3 ml 3% Tween-80 aqueous solution, 2.0 ml pH8.2 borax-sodium hydroxide buffer solution, 2.5 ml 2×10 -5 mol / L DMSDCNPDP solution, then double-distilled water to volume. Using a 1cm cuvette, at the excitation wavelength (λ ex ) 246 nm, emission wavelength (λ em ) at 440 nm to measure its fluorescence intensity, and record ΔF (the fluorescence absorbance of reagent blank is 100).

[0043] Process the sample according to the literature [Physical and Chemical Test-Chemistry Volume, Wei Qin, Shou Chongqi, etc., 2004, Volume 40, No. 1, Page 12-14], and then use the experimental method to determine. The results are shown in Table 4. The results show that the reagent fluorescence quenching method of the invention is better in sensitivity and selectivity than the existing reagents ...

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Abstract

The invention belongs to the technical field of double triazene compounds and provides 3,3'-dimethylthio-4,4'-bis(2,6-dichloro-4-nitrophenyl diazoamino) biphenyl, a preparation method and an application in order to solve the problems that when an existing triazene reagent is used for detecting heavy metal ions through photometric analysis, interference from coexisting ions is strong, sensitivity and selectivity are not ideal enough and the existing triazene reagent cannot be taken as a fluorescent reagent for fluorescence detection of the heavy metal ions. 3,3'-dimethylthio-4,4'-diaminodiphenyl and 2,6-dichloro-4-nitrophenyl are linked together through a triazene functional group -N=N-NH-, and a prepared reagent is not only a photometric analysis reagent with good sensitivity and selectivity, but also is a fluorescence analysis reagent with a high fluorescence characteristic. The sensitivity of the reagent for measuring mercury with a photometric method is improved; the reagent is a fluorescent lead (II) measurement reagent with good sensitivity and selectivity; the allowed coexistence number of common interfering ions is greatly increased; a synthetic method is simple, conditions are mild, and complexes formed by a solid reagent and a reagent solution with mercury are all stable.

Description

technical field [0001] The invention belongs to the technical field of bistriazene compounds, in particular to a 3,3'-dimethylthio-4,4'-bis(2,6-dichloro-4-nitrophenyldiazoamino)bis Benzene and its preparation method and application. Background technique [0002] Triazene reagent refers to the general term of all reagents with R-N=N-NH-R' structure. The -N=N-NH-functional group of the reagent is easy to coordinate with IB and IIB group metal ions in the presence of surfactants to form stable colored complexes. Therefore, this type of reagent can be used for photometric detection of metal ions. [0003] Currently, triazene reagents are mainly used for Ca 2+ 、Ni 2+ , Hg 2+ 、Cu 2+ 、Co 2+ 、Ag + Photometric determination of other metal ions (Teng Sijiang, Jiang Wanquan, Zhu Yurui, etc. Chemical Reagents, 1992, 14 (2): 109). Such reagents have attracted the attention of chemists because of their advantages such as simple operation, high sensitivity, high contrast in color r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/20C07C323/36C07C319/14C07C319/02C07C323/34C07D277/82C07C245/20C09K11/06G01N21/64G01N21/31
CPCC07C245/20C07C319/02C07C319/14C07C319/20C07C323/34C07C323/36C07D277/82C09K11/06C09K2211/1007C09K2211/1014G01N21/31G01N21/643G01N2021/6432
Inventor 刘慧君樊月琴赵强宋金萍樊志会马琦
Owner SHANXI DATONG UNIV
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