Simple preparation method of ruthenium polypyridine complex

A technology of ruthenium chloride hydrate and bipyridyl, which is applied in the field of electrochemistry, can solve the problems of unfavorable industrialized expansion of production, high requirements for reaction vessels, and difficulty in large-scale procurement, etc., and achieves good purification effect, increased overall yield, and improved product purity. Effect

Inactive Publication Date: 2014-07-30
WUHAN UNIV OF TECH
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Problems solved by technology

This method uses ethylene glycol as a solvent. If a part of the ethylene glycol is not spun off first, a large amount of ether needs to be added in the post-treatment to precipitate the solid. However, ethylene glycol has a boiling point of 198°C and is not easy to remove, so the post-processing of this method is troublesome. Add a large amount of ether, and ether has anesthetic effect, controlled, not easy to purchase in large quantities
The reaction temperature is high, and the requirements for the reaction vessel are high, so it is not conducive to industrial expansion of production

Method used

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  • Simple preparation method of ruthenium polypyridine complex
  • Simple preparation method of ruthenium polypyridine complex
  • Simple preparation method of ruthenium polypyridine complex

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preparation example Construction

[0030] The preparation method of ruthenium (II) complex tris (2,2'-bipyridyl) ruthenium (II) chloride hexahydrate of the present invention, the steps are as follows:

[0031] Ruthenium chloride hydrate and 2,2'-bipyridine are dissolved in ethanol and ethylene glycol mixed solvent;

[0032] The reaction was heated, cooled to room temperature, and the ethanol was rotary evaporated;

[0033] Add saturated sodium chloride solution to precipitate a solid, filter, add water to recrystallize, and dry to obtain tris(2,2'-bipyridyl)ruthenium(II) chloride hexahydrate.

[0034] The reaction of the invention is simple and easy to operate, and the overall yield and product purity are greatly improved compared with the existing method. After recovering ethanol in post-treatment, directly add saturated sodium chloride solution, precipitate solid, and obtain crude product by suction filtration, without using any organic solvent, which is greatly simplified compared with the prior art, and is...

Embodiment 1

[0040]A total of 13g (50mmol) of ruthenium chloride hydrate and 39g (250mmol) of 2,2'-bipyridine were added to 2L ethylene glycol and ethanol mixed solution (ethylene glycol 400ml), and the reaction solution was heated to After about 20 minutes at 100°C, the ruthenium chloride hydrate was completely dissolved, reacted for about 7 hours, stopped heating and cooled to room temperature. Distill the reaction liquid under reduced pressure, recover about 1200ml of ethanol, add 1000ml of saturated sodium chloride solution, precipitate a large amount of red solid, filter with suction to obtain 37g of solid, recrystallize with 93ml of water, dry to obtain tris(2,2'-bipyridine) Ruthenium(II) chloride hexahydrate was 35g, and the yield was 94.6%.

[0041] The infrared absorption spectrum of the product obtained in this embodiment and the purchased J&K brand three (2,2'-bipyridyl) ruthenium (II) chloride hexahydrate (IR spectrum testing instrument: Bruker VECTOR-22, testing condition: KBr...

Embodiment 2

[0048] A total of 26g (100mmol) of ruthenium chloride hydrate and 78g (500mmol) of 2,2'-bipyridine were added to 4L ethylene glycol and ethanol mixed solution (ethylene glycol 1600ml), and the reaction solution was heated to After about 30 minutes at 90°C, the ruthenium chloride hydrate was completely dissolved, reacted for about 9 hours, stopped heating and cooled to room temperature. Distill the reaction liquid under reduced pressure, recover about 2000ml of ethanol, add 2000ml of saturated sodium chloride solution, precipitate a large amount of red solid, and obtain 79g of solid by suction filtration, recrystallize with 158ml of water, dry to obtain tris(2,2'-bipyridine) Ruthenium(II) chloride hexahydrate was 71g, and the yield was 95.9%.

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Abstract

The invention discloses a simple preparation method of an electrochemiluminescent reagent ruthenium polypyridine complex. The preparation method comprises the following steps: dissolving a ruthenium chloride hydrate and 2, 2'-dipyridyl in a mixed solvent of ethanol and ethylene glycol, wherein the ratio of ruthenium trichloride in the ruthenium chloride hydrate to 2, 2'-dipyridylis 1:4-1:5, and the concentration of ruthenium trichloride in the mixed solvent is 0.02-0.025mol / L; heating to react, wherein the reaction temperature is 70-100 DEG C and the reaction time is 6-10 hours; cooling to room temperature and carrying out rotary evaporation to remove ethanol; adding a saturated sodium chloride solution to separate out solids, filtering, adding water to recrystallize and drying to obtain tri(2, 2'-dipyridyl) ruthenium chloride (II) hexahydrate. The synthetic method is simple and convenient, short in reaction step, easy to operate, less in consumption of organic solvents, simple in post-treatment and high in product purity. The conversation ratio of noble metal ruthenium reaches up to 95%, so that the preparation method is less in environmental protection pressure and convenient for industrialized production.

Description

technical field [0001] The invention relates to the technical field of electrochemistry, in particular to a simple preparation method of an electrochemiluminescent reagent ruthenium polypyridine complex. Background technique [0002] Ruthenium is a rare metal element in the platinum group metals, which plays a vital role in catalysis and industrial production. In the field of coordination chemistry, ruthenium complexes have been widely used in nonlinear optical materials, Research in the fields of chemiluminescence, molecular recognition, molecular photoswitching electron transfer, and photocatalytic degradation of water and organic matter. In addition, some ruthenium complexes are used as efficient dye sensitizers for dyes due to their obvious absorption in the visible light region. In sensitized solar cells, some ruthenium complexes also have excellent electrochemical properties, and have important applications in electroluminescent materials, biosensors, etc. In order t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/22C07D213/127
CPCC07D213/127C07D213/22
Inventor 秦华利陈小清韩家斌郝建宏张方林
Owner WUHAN UNIV OF TECH
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