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Ruthenium acetate and preparation method thereof

A technology of ruthenium acetate and acetic acid solution, applied in the field of ruthenium acetate and its preparation, can solve problems such as pollution, and achieve the effects of high yield, short synthesis time and low halogen content

Pending Publication Date: 2018-12-28
CHENZHOU GAOXIN PLATINUM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese Patent Publication No. CN1279012C, named as the method for preparing ruthenium (Ⅲ) acetate solution, this application discloses ruthenium oxide (Ⅳ) as raw material, selects hydrazine as reducing agent, and in the aqueous solution of acetic acid, ruthenium oxide (Ⅳ) is reduced to Ruthenium(Ⅲ) acetate, this method needs to add hydrazine, which may introduce nitrogen pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 270g of ruthenium trichloride (containing 100g of ruthenium), add 2000mL of deionized water, stir to dissolve, add sodium hydroxide to adjust the pH value to 8, and continue to stir for 0.5 hours, the solution is filtered and washed to obtain ruthenium hydroxide precipitate. Add ruthenium hydroxide precipitate to 2000mL 20% nitric acid solution and heat to 70°C, add sodium carbonate solution to adjust the pH value to 7 after complete dissolution, keep stirring for 1 hour, filter and wash until the filtrate is free of chloride ions, and the obtained ruthenium hydroxide precipitates Add 2000mL of 60% acetic acid solution, heat to reflux for 1 hour under stirring, cool to room temperature after stopping the reaction, filter and concentrate to obtain ruthenium acetate solid. 492ppm.

Embodiment 2

[0022] Take 540g of ruthenium trichloride (containing 200g of ruthenium), add 4000mL of deionized water, stir and dissolve, add potassium hydroxide to adjust the pH value to 10, and continue to stir for 0.5 hours. After the solution is filtered and washed, ruthenium hydroxide precipitate is obtained. Add ruthenium hydroxide precipitate to 4500mL 30% nitric acid solution and heat to 60°C, add potassium carbonate solution to adjust the pH value to 8 after complete dissolution, keep stirring for 1 hour, filter and wash until the filtrate is free of chloride ions, and the obtained ruthenium hydroxide precipitates Add 4000mL of 60% acetic acid solution, stir and heat to reflux for 3h, stop the reaction, cool to room temperature, filter and concentrate to obtain ruthenium acetate solid, the yield is 96.1% based on the weight of ruthenium, detected by ion chromatography, the chlorine in the solid The ion content is 370ppm.

Embodiment 3

[0024] Take 1000g of ruthenium trichloride (containing 370g of ruthenium), add 7000mL of deionized water, stir and dissolve, add sodium hydroxide to adjust the pH value to 10, and continue stirring for 0.5 hours, the solution is filtered and washed to obtain ruthenium hydroxide precipitate. Add ruthenium hydroxide precipitate to 8000mL 45% nitric acid solution and heat to 50°C, add sodium carbonate solution to adjust the pH value to 7 after complete dissolution, keep stirring for 1 hour, filter and wash until the filtrate is free of chloride ions, and the obtained ruthenium hydroxide precipitates Added to 7000mL 60% acetic acid solution, heated to reflux for 4 hours under stirring, cooled to room temperature after stopping the reaction, filtered and concentrated to obtain ruthenium acetate solid with a yield of 97.5%. The chloride ion content in the solid was 413ppm as detected by ion chromatography.

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PUM

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Abstract

The invention discloses a preparation method of ruthenium acetate. Ruthenium trichloride is taken as an initial material, ruthenium hydroxide is obtained after alkali is added and dissolved by nitricacid, ruthenium hydroxide is precipitated after alkali is added, an acetic acid solution is added after filtration and washing, heating reflux is performed for 1-4 h, and concentration is performed after cooling to obtain a liquid or solid ruthenium acetate product. By means of the method, the high-yield and high-purity ruthenium acetate product is obtained under the condition that no additive isadded, the synthesis time is short, and for solid ruthenium acetate, the halogen impurity content is lower than 500 ppm.

Description

technical field [0001] The invention belongs to the field of chemical product preparation, and in particular relates to ruthenium acetate and a preparation method thereof. Background technique [0002] Ruthenium acetate, also known as ruthenium acetate, has the molecular formula [Ru 3 O(OAc) 6 (H 2 O) n (AcOH) 3-n ]OAc, dark blue or black solid, solution product is dark blue. The main use of ruthenium acetate is as a catalyst or co-catalyst for various chemical reactions, such as hydrogenation, isomerization, carbonylation, etc., and can also be used as a precursor of supported ruthenium catalysts. [0003] In the "Handbook of Noble Metal Compound-Based Complex Synthesis", it is described that its synthesis method is to mix carbon tetrachloride mixed with ruthenium tetroxide with 50% glacial acetic acid, add acetaldehyde to produce dark blue precipitate, and filter tetrachloride Carbonization washing, drying under reduced pressure in a desiccator, this method will inev...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C53/10C07F15/00
CPCC07C51/412C07F15/0053C07C53/10
Inventor 雷婧杨拥军欧阳文兵雷海波叶咏祥雷涤尘杨静
Owner CHENZHOU GAOXIN PLATINUM
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