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Water-soluble phenazine derivative as well as preparation method and application thereof

A derivative and water-soluble technology, applied in the fields of chemical synthesis and anion detection, can solve problems such as thermal equipment scaling, unfavorable power plant safe operation, corrosion, etc., and achieve a wide range of practical effects

Active Publication Date: 2020-09-25
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Excessive concentration of silicate ions will cause scaling and corrosion of thermal equipment
These hazards are not only detrimental to the safe operation of the power plant, but also greatly reduce the energy efficiency of the power plant.
The detection of silicate is also very important in daily life. The silicate detector is expensive and not suitable for qualitative experiments.
At present, in qualitative experiments, the detection method of silicate ions in water is relatively simple. We use ultraviolet detection technology to realize the detection of silicate ions

Method used

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  • Water-soluble phenazine derivative as well as preparation method and application thereof
  • Water-soluble phenazine derivative as well as preparation method and application thereof
  • Water-soluble phenazine derivative as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1, the synthesis of phenazine derivatives S1

[0038] (1) Synthesis of 2,3-diaminophenazine: According to the literature [Li.G., Wu.Y.C., Gao.J.K., Wang.C.Y., Li.J.B., Zhang.H.C.J Am Chem Soc.2012,134,20298 .】synthesis. 1 H-NMR(400MHz,DMSO)δ:7.89(s,2H,ph-H),7.54(s,2H,ph-H),6.91(s,2H,ph-H),6.25(s,4H,NH 2 ). figure 1 It is the H NMR spectrum of 2,3-diaminophenazine.

[0039] (2) Synthesis of phenazine derivatives S1: 2mmol 2,3-diaminophenazine, 2mmol 3,4-dihydroxybenzaldehyde, 10ml glacial acetic acid were dissolved in 20ml anhydrous DMF, refluxed, and the temperature of the reaction system was Rising to 165°C, monitored by TLC. The raw materials were reacted for 12 hours, and the reaction was stopped. After the reaction system dropped to room temperature, the reaction solution was poured into 200ml of water (solids were formed), centrifuged, the solids were washed with distilled water, dried, and the crude product was washed with DMF / H 2 O recrystallized,...

Embodiment 2

[0040] Embodiment 2, the synthesis of water-soluble phenazine derivatives S1-Na

[0041] Add 0.25 mmol of S1 to 20 ml of ethanol solution, stir for 10 min, then add 0.5 mmol of NaOH (0.02 g), the solution changes from brown-black to wine red instantly, and continue stirring for 30 min. After the reaction is completed, rotary evaporation is performed to obtain a brown-red or brown-black solid, which is dried in a vacuum oven to obtain the product water-soluble phenazine derivative S1-Na. Figure 4 It is the H NMR spectrum of S1-Na. It can be clearly seen from the figure that compared with the H NMR spectrum of S1, the absorption peaks of the two hydroxyl groups at 9.4-9.9pm disappear, which proves that S1-Na was successfully synthesized.

Embodiment 3

[0042] Example 3, Water-soluble phenazine derivatives S1-Na UV recognition of SiO in aqueous solution 3 2-

[0043] 2.0 x 10 in 3ml -3 mol L -1 Add 60 μL of 4.0×10 -2 mol L -1 different anions (CH 3 COO - , HCOO - , CO 3 2- , SiO 3 2- , SO 4 2- , NO 2 - , HSO 3 - , HCO 3 - , H 2 PO 4 - , F - , Cl - , B r - ). It was found that when the above-mentioned anion solutions were added to the aqueous solution of S1-Na, only SiO 3 2- The addition of ions makes its ultraviolet absorption spectrum red shift to 468nm at 424nm and the absorption peak at 260nm increases, and the addition of other ions hardly changes its ultraviolet absorption spectrum significantly ( Figure 5 ). It is obtained by measuring the ultraviolet absorption spectrum. If the ultraviolet absorption spectrum is red-shifted to 468nm at 424nm and accompanied by an increase in the absorption peak at 260nm, it means that SiO is added. 3 2- , otherwise other ions are added.

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Abstract

The invention relates to a water-soluble phenazine derivative as well as a preparation method and an application thereof. The structural formula of the derivative is shown in the specification. The preparation method of the water-soluble phenazine derivative comprises the following steps: adding N, N-dimethylformamide, 2, 3-diaminophenazine, glacial acetic acid and 3, 4-dihydroxy benzaldehyde intoa reactor to obtain the phenazine derivative; in absolute ethyl alcohol, adding phenazine derivatives and sodium hydroxide into the absolute ethyl alcohol, and carrying out a stirring reaction at room temperature to obtain the water-soluble phenazine derivatives. The water-soluble phenazine derivative is used for anion recognition of a silicate ion sensor.

Description

technical field [0001] The present invention designs a silicate ion sensor molecule, especially relates to a sensor molecule capable of ultraviolet recognition of silicate ion: water-soluble phenazine derivative S1-Na; the present invention also relates to the silicate ion sensor molecule in pure water The research on the performance of ultraviolet recognition of silicate ions in the system belongs to the field of chemical synthesis and the field of anion detection technology. Background technique [0002] The detection of silicate in the daily operation of power plants is one of the important items, and the content of silicate in boiler water and cooling circulating water is an important parameter for supervision. Excessive concentration of silicate ions will cause scaling and corrosion of thermal equipment. These hazards are not only detrimental to the safe operation of the power plant, but also greatly reduce the energy efficiency of the power plant. The detection of si...

Claims

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Application Information

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IPC IPC(8): C07D487/04G01N21/33G01N21/35G01N24/08
CPCC07D487/04G01N21/33G01N21/35G01N24/08
Inventor 段中余温雨晴许云鹏史大鹏刘宾元
Owner HEBEI UNIV OF TECH
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