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3,5-dinitro-2,6-bis(4,4'-sulfoazophenylazoamino)pyridine and its preparation method and application

A technology of sulfoazobenzene azoamino and sulfoazobenzene, which is applied in the field of bistriazene compounds, can solve the problems of low sensitivity and unsatisfactory selectivity of heavy metal ions, and achieve low cost and convenient The effect of mild storage and preparation conditions

Inactive Publication Date: 2018-07-27
SHANXI DATONG UNIV
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Problems solved by technology

[0003] The present invention provides a 3,5-dinitro-2,6-bis(4,4 ， -Sulfonic acid azoanilinoazo)pyridine and its preparation method and application

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  • 3,5-dinitro-2,6-bis(4,4'-sulfoazophenylazoamino)pyridine and its preparation method and application

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Embodiment Construction

[0029] A 3,5-dinitro-2,6-di(4,4 ， -Sulphonic acid azophenylazoamino)pyridine (abbreviated as DNDSZBZAB), its molecular structure is:

[0030] .

[0031] 3,5-Dinitro-2,6-di(4,4 ，- the preparation method of sulfonic acid azophenyl (azoamino) pyridine, comprises the following steps, as figure 1 Shown:

[0032] (1) Preparation of 4-amino-4´-sulfoazobenzene

[0033] In a beaker, add 10.4 g (0.1 mol) NaHSO 3 , then add 38 mL of water and 8 mL of 40% (0.1 mol) formaldehyde by volume fraction, stir in a water bath at 60-66°C for 40 minutes, add 7.2 g (0.08 mol) of aniline, and react for 2 hours to obtain light yellow anilinomethylsulfonic acid Sodium clarified solution; another 13.8g (0.08 mol) p-aminobenzenesulfonic acid was dissolved in 140 mL of 3% sodium carbonate solution, and under ice water cooling, 5.6 g of sodium nitrite was dissolved in 30 mL of water. solution; under stirring, add 210 mL of concentrated hydrochloric acid, the dropwise addition process is controlled ...

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Abstract

The invention belongs to the field of bistriazene compounds, and solves the problem in the prior art that detection of heavy metal ions by triazene reagents has a low sensitivity and unideal selectivity. The method comprises the following steps: firstly, NaHSO3, formaldehyde and aniline are used for preparing a settled solution of sodium aniline methyl sulfonate, sulfanilic acid is used for preparing a solution of diazonium salt, the two kinds of solution are mixed, and 4-amino-4'-azobenzene sulfonic acid; secondly, 2,6-diamino pyridine, KNO3 solid and fuming nitric acid are used, in order to produce 3,5-dinitro-2,6-diamino pyridine; thirdly, two kinds of substances prepared by the two steps are produced into a solution, after a reaction, produced products are separated by column chromatography, and 3,5-dinitro-2,6-bis(4,4'-sulfonic azobenzene azo amino)pyridine. Pyridine is a high-sensitivity developer for measuring cadmium by a photometric method, and measurement of cadmium is good selectivity.

Description

technical field [0001] The invention belongs to the field of bistriazene compounds, in particular to a 3,5-dinitro-2,6-bis(4,4 ， -Sulphonic acid azophenyl (azoamino)pyridine and its preparation method and application. Background technique [0002] Triazene reagent is a kind of highly sensitive chromogenic reagent for photometric analysis. Its general formula is Ar-N=N-NH-Ar´, where Ar and Ar´ are aromatic hydrocarbon groups or aromatic heterocyclic groups. In the presence of surfactants, triazene reagents coordinate with IB and IIB group metal ions to form stable complexes. Therefore, this type of reagent is usually used for Cd 2+ , Hg 2+ 、Cu 2+ 、Ni 2+ and Ag + Photometric determination of other metal ions (Feng Yonglan, Liu Zhifang. Metallurgical Analysis, 2008, 26(4): 65-67). This type of reagent has the advantages of high sensitivity, simple synthesis, easy purification, and low cost. Therefore, it has been widely used in the photometric determination of metal ions ...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/76G01N21/78
CPCC07D213/76G01N21/78
Inventor 解海许琳赵强
Owner SHANXI DATONG UNIV
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