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Preparation method of hexaammineruthenium(III) chloride

A technology of trichlorohexammonium and chlororuthenic acid, applied in chemical instruments and methods, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, inorganic chemistry, etc., can solve the problem of complex preparation methods and difficulty in obtaining electronic grade purity products and other problems, to achieve the effect of simple operation, low cost and short time

Active Publication Date: 2019-04-05
JIANGSU SINOCOMPOUND CATALYST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current preparation method adopts ruthenium trichloride as starting raw material, first reacts with concentrated hydrochloric acid and zinc powder to prepare ruthenium hexaamine dichloride, and then oxidizes it with oxygen to prepare ruthenium hexaamine trichloride. The route preparation method is complicated, It involves multiple material transfers and precise control of electronic equipment, so it is difficult to obtain products with electronic grade purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Step 1, dissolving ruthenium chloride in concentrated ammonia water to obtain a solution with a ruthenium concentration of 15%;

[0027] Step 2, adding Mg to the solution, heating to 50°C under the protection of an inert gas, and stirring to make the catalyst evenly dispersed;

[0028] Step 3. Slowly add hydrogen peroxide dropwise at 40°C until the solution is colorless;

[0029] Step 4: remove the catalyst by filtration, cool and crystallize at room temperature or low temperature, wash and dry the crystal to obtain white or light yellow solid ruthenium trichlorohexammine.

[0030] The yield of ruthenium trichlorohexammine obtained in this embodiment is 75%, the mass purity is greater than 99%, and the elemental analysis shows H5.80%, N 27.20%, and ruthenium 32.60%.

Embodiment 2

[0032] Step 1, dissolving ruthenium chloride in concentrated ammonia water to obtain a solution with a ruthenium concentration of 15%;

[0033] Step 2, adding Mg to the solution, heating to 50°C under the protection of an inert gas, and stirring to make the catalyst evenly dispersed;

[0034] Step 3. Slowly add chlorine gas at 40°C until the solution is colorless;

[0035] Step 4: remove the catalyst by filtration, cool and crystallize at room temperature or low temperature, wash and dry the crystal to obtain white or light yellow solid ruthenium trichlorohexammine.

[0036] The yield of ruthenium trichlorohexammine obtained in this embodiment is 77%, the mass purity is greater than 99%, and the elemental analysis shows H5.81%, N 27.22%, and ruthenium 32.62%.

Embodiment 3

[0038] Step 1, dissolving ruthenium chloride in concentrated ammonia water to obtain a solution with a ruthenium concentration of 15%;

[0039] Step 2, adding Zn to the solution, heating to 50°C under the protection of an inert gas, and stirring to disperse the catalyst evenly;

[0040] Step 3. Slowly add hydrogen peroxide dropwise at 40°C until the solution is colorless;

[0041] Step 4: remove the catalyst by filtration, cool and crystallize at room temperature or low temperature, wash and dry the crystal to obtain white or light yellow solid ruthenium trichlorohexammine.

[0042] The yield of ruthenium trichlorohexammine obtained in this embodiment is 79%, the mass purity is greater than 99%, and the elemental analysis shows H5.79%, N 27.18%, and ruthenium 32.57%.

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Abstract

The invention discloses a preparation method of hexaammineruthenium(III) chloride. The preparation method includes the following steps: 1, dissolving ruthenium hydrochloride in concentrated ammonia water; 2, adding a catalyst into the solution, and heating the solution to 50-100 DEG C under inert gas protection to uniformly disperse the catalyst; 3, slowly dropwise adding an oxidant at the temperature of 30-50 DEG C until the solution is colorless; 4, removing the catalyst through filtration, performing cooling crystallization at the room temperature or a low temperature, and washing and drying crystals to obtain the white or light-yellow solid hexaammineruthenium(III) chloride. The preparation method has the advantages that the method is simple to operate and low in cost and consumes lesstime; the product is precipitated out in the form of the crystals, and no other salt is added in the preparation process, so that the purity is high; the ruthenium complex obtained by the preparationmethod is widely used in the fields requiring high-purity products, including electrochemical biosensors and precursors serving as high-purity metallocene compounds.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, and relates to a preparation method of a ruthenium complex. Background technique [0002] Among the platinum group metals, metal ruthenium is more and more widely used in the fields of organic synthesis and electrochemical biosensors due to its low price, special electrochemical properties and excellent catalytic performance. Ruthenium can accept many different kinds of complexes to form special spatial structures, which can be applied in the fields of chemistry and electronics. More and more such complexes have been used in the fields of catalysis, biological enzymes and electronics. [0003] Hexaammine ruthenium trichloride is used as an electron mediator in electrochemical biosensors, which transfers electrons generated by biochemical reactions from the active center to the electrode surface, and causes a corresponding current on the electrode surface, and is widely used in blood gl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G55/00
CPCC01G55/002C01P2006/80
Inventor 陈虎邓生财祁义军李娟
Owner JIANGSU SINOCOMPOUND CATALYST
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