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Process method for synthesizing liquid ruthenium nitrate

A synthesis process, the technology of ruthenium nitrate, applied in the field of ruthenium nitrosyl nitrate synthesis, can solve the problems of high content of sodium ion and chloride ion and low concentration of liquid products

Pending Publication Date: 2021-11-02
合创无锡环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, ruthenium powder is adopted to adopt chlorine gas as an oxidant, and ruthenium alkali is dissolved in the process of nitration to synthesize ruthenium nitrate, and there are problems such as high sodium ion and chloride ion content in the prepared product system; and oxidation of vanadium pentoxide by ruthenium powder Finally, after adding sodium nitrite to synthesize ruthenium nitrosyl chloride, the solution is extracted and evaporated with ether to obtain solid ruthenium nitrosonitrate. Although the problem of excessive chloride ion content has been avoided, it needs to be dissolved again during use, and the concentration of the obtained liquid product is not high. High, can not directly meet the demand

Method used

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  • Process method for synthesizing liquid ruthenium nitrate
  • Process method for synthesizing liquid ruthenium nitrate
  • Process method for synthesizing liquid ruthenium nitrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1) 500 g of ruthenium powder was added to 15 l 15% sodium hydroxide solution, and excess of chlorine gas was introduced to ensure sufficient oxidation, and the reaction temperature was controlled at 85-90 ° C. The liquid level is boiling, there is golden water mist, surrounded with golden yellow bubbles, stopping accession to chlorine;

[0034] 2), adding ethanol reducing agent according to the ratio of the rhodium to 1: 0.6, the color of the solution is black, filtered to obtain Ru 4+ Black precipitate.

[0035] 3), using 0.5% nitric acid and 0.3% ammonia, alternately washed with water, and filtered the filter cake after washing.

[0036] Note: 0.5% nitric acid formulation, nitric acid volume = (filter cake mass × 3 × 0.5%) ÷ (0.65 × 1.41)

[0037] 0.3% ammonia water formulation, ammonia water volume = (filter cake mass × 3 × 0.3% × 4) ÷ 0.9;

[0038] The present formula indicates how to utilize 65% mass concentrations of commercially available nitroths, density of 141 g / ...

Embodiment 2

[0042] 1) 500 g of ruthenium powder was added to 15 l 15% sodium hydroxide solution, and chlorine gas was introduced, and the reaction temperature was controlled at 85-90 ° C. The liquid level is boiling, there is golden water mist, surrounded with golden yellow bubbles, stopping accession to chlorine;

[0043] The ethanol reducing agent is added to 1: 0.7 with the ruthenium ratio, the solution color is black, filtered to obtain Ru 4+ Black precipitate.

[0044] It was washed with 0.5% nitric acid and 0.3% ammonia, and the filter cake was collected after washing.

[0045] Note: 0.5% nitric acid formulation, nitric acid volume = (filter cake mass × 3 × 0.5%) ÷ (0.65 × 1.41)

[0046] 0.3% ammonia water formulation, ammonia volume = (filter cake mass × 3 × 0.3% × 4) ÷ 0.9

[0047] According to the water washing filter, the amount of 5.5 times the mass of the mass of 5.5% is reacted with the filter cake. The reaction temperature was controlled at 85-90 ° C, and the reaction was added ...

Embodiment 3

[0050] 1) 500 g of ruthenium powder was added to 15 l 15% sodium hydroxide solution, and chlorine gas was introduced, and the reaction temperature was controlled at 85-90 ° C. The liquid level is boiling, there is golden water mist, surrounded with golden yellow bubbles, stopping accession to chlorine;

[0051] The ethanol reducing agent is added to 1: 0.8 with the rhodium ratio, and the solution color is black, filtered to obtain Ru. 4+ Black precipitate.

[0052] It was washed with 0.5% nitric acid and 0.3% ammonia, and the filter cake was collected after washing.

[0053] Note: 0.5% nitric acid formulation, nitric acid volume = (filter cake mass × 3 × 0.5%) ÷ (0.65 × 1.41)

[0054] 0.3% ammonia water formulation, ammonia volume = (filter cake mass × 3 × 0.3% × 4) ÷ 0.9

[0055] The 65% nitric acid containing 6 times mass of the ruthenium was carried out in water washing cake. The reaction temperature was controlled at 85-90 ° C, and the reaction was added for about 9 hours, and 1...

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Abstract

The invention provides a process method for synthesizing liquid ruthenium nitrate, and belongs to the field of synthesis of ruthenium nitrosyl nitrate. The specific synthesis process comprises the following steps: heating and stirring a sodium hydroxide solution, then adding ruthenium powder, introducing chlorine, and maintaining the temperature at 85-90 DEG C; adding a reducing agent into the obtained reaction liquid, filtering to obtain filtrate and a filter cake, analyzing the ruthenium content in the filtrate, and recording the mass of the filter cake so as to analyze the ruthenium content; washing the obtained filter cake with water, then alternately washing the filter cake with 0.5% nitric acid and 0.3% ammonia water, and recording the mass of the filter cake after washing each time; mixing nitric acid with the cleaned filter cake for reaction, then adding sodium nitrite for reaction, and filtering to obtain filtrate and filter residues; and heating and concentrating the obtained filtrate to obtain the liquid ruthenium nitrate. The method for preparing ruthenium nitrate is high in conversion rate, and the obtained ruthenium nitrate is high in purity.

Description

Technical field [0001] The present invention belongs to the field of nitrogen nitrate, and is relate to a liquid nitrate synthesis process, and more particularly to a specifically by synthesizing a high-pure nitrate solution by ruthenium powder. Background technique [0002] Regarding the preparation technique of nitroxyl nitric nitric nitrid, patent CN102167405A reported that tetrachloride is a raw material, and sodium nitrate is added to nitride, and then the nitrogenated ruthenium and nitrate is reacted. The nitrate solution, the solution is evaporated to evaporate the solid nitrogen nitrogen nitrate; patent CN104556250A reports that the new nitric acid and trichloride return to nitrrylachidium oxide, and the nitrrylalogenic acid is also reacted with nitrate. The nitric nitrate solution was produced, and the solution was evaporated to evaporate the solid nitrositropylate. Patent CN201710165689.7 Reports After oxidizing osteadium dioxide, the sodium nitrite is added to the nitr...

Claims

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Application Information

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IPC IPC(8): C01G55/00
CPCC01G55/00Y02P10/20
Inventor 戴明飞
Owner 合创无锡环保科技有限公司
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