Method for preparing high-purity acetylacetonatodicarbonyl rhodium through using rhodium trichloride

A technology of rhodium acetone dicarbonyl and rhodium trichloride, which is applied in the field of catalysis and can solve problems such as difficult removal of impurities

Active Publication Date: 2014-12-03
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, if you want to react with impurities by adding reagents, it is difficult to achieve the purpose of removing impurities

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020]1.00 g of rhodium chloride hydrate containing sodium, iron, nickel, and calcium metal impurities (the mass contents of rhodium, sodium, iron, nickel, and calcium are respectively: 35.21%, 0.97%, 0.0143%, 0.0014%, and 0.0256%) and Put 15 ml of N, N-dimethylformamide and 4 ml of acetylacetone in a 50 ml round-bottomed flask, heat to 80°C, keep for 0.5 hour, continue to raise the temperature to 136°C and keep for 1 hour, after the reaction is completed, the reaction solution is naturally Cool to room temperature, add 100 milliliters of deionized water, filter out acetylacetonate rhodium dicarbonyl precipitation after mixing evenly, wash filter cake with deionized water, after the acetylacetonate dicarbonyl rhodium crude product that obtains is dissolved with 40 milliliters of toluene solvent, then with 40 milliliters Wash the toluene phase twice (40×2) with a disodium edetate aqueous solution (mass concentration 0.1%), and then wash the toluene phase once with 40 ml of deion...

Embodiment 2

[0022] 1.00 g of rhodium chloride hydrate containing sodium, iron, nickel, and calcium metal impurities (the mass contents of rhodium, sodium, iron, nickel, and calcium are respectively: 34.87%, 0.69%, 0.0118%, 0.8920%, and 0.0235%) and Put 15 ml of N, N-dimethylformamide and 4 ml of acetylacetone in a 50 ml round-bottomed flask, heat to 80°C, keep for 0.5 hour, continue to raise the temperature to 136°C and keep for 1 hour, after the reaction is completed, the reaction solution is naturally Cool to room temperature, add 100 milliliters of deionized water, filter out the rhodium acetylacetonate precipitate after mixing evenly, wash the filter cake with deionized water, after the crude product of rhodium acetylacetonate dicarbonyl is dissolved with 40 milliliters of toluene solvent, then use 2 milliliters Wash the toluene phase twice (2×2) with an aqueous solution of disodium edetate (mass concentration 2.0%), and then wash the toluene phase once (2×1) with 2 ml of deionized wat...

Embodiment 3

[0024] 1.00 g of rhodium chloride hydrate containing sodium, iron, nickel, and calcium metal impurities (the mass contents of rhodium, sodium, iron, nickel, and calcium are respectively: 34.30%, 0.54%, 0.0124%, 0.0018%, and 0.8630%) and Put 15 ml of N, N-dimethylformamide and 4 ml of acetylacetone in a 50 ml round-bottomed flask, heat to 80°C, keep for 0.5 hour, continue to raise the temperature to 136°C and keep for 1 hour, after the reaction is completed, the reaction solution is naturally Cool to room temperature, add 100 milliliters of deionized water, filter out the rhodium acetylacetonate precipitate after mixing evenly, wash the filter cake with deionized water, after the crude product of rhodium acetylacetonate dicarbonyl is dissolved with 4 milliliters of toluene solvent, then use 8 milliliters Wash the toluene phase twice (8×2) with a disodium edetate aqueous solution (mass concentration 0.6%), and then wash the toluene phase once with 8 ml of deionized water (8×1), t...

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Abstract

The invention relates to a method for preparing high-purity acetylacetonatodicarbonyl rhodium through using rhodium trichloride. The method comprises the following steps: mixing rhodium trichloride containing metal impurities with N,N-dimethyl formamide and acetylacetone, heating to reaction completeness, cooling the obtained reaction solution to room temperature, adding deionized water, filtering the obtained precipitate, washing the precipitate to obtain crude acetylacetonatodicarbonyl rhodium, dissolving the crude acetylacetonatodicarbonyl rhodium in a sufficient amount of an organic solvent, washing the obtained organic phase by an aqueous solution of disodium ethylene diamine tetraacetate twice, and washing the organic phase by water once to obtain an acetylacetonatodicarbonyl rhodium solution. The method which adopts the acetylacetonatodicarbonyl rhodium containing the metal impurities as a reaction raw material enables the rhodium recovery process to be substantially shortened, so the production cost is reduced, and the economic benefit of the method is large.

Description

Technical field: [0001] The invention relates to the technical field of catalysis, and is a method for preparing high-purity rhodium acetylacetonate carbonyl with rhodium trichloride, in particular to using rhodium trichloride containing metal impurities to prepare a high-purity homogeneous reaction catalyst or catalyst precursor acetyl Acetone carbonyl rhodium method. Background of the invention: [0002] Rhodium homogeneous organic complex catalysts have the advantages of high catalytic activity and good selectivity, and have important applications in catalytic reactions such as catalytic hydrogenation, olefin hydroformylation, and oxo synthesis, and many of them have been used in industrial production. For example: Tris(triphenylphosphine)rhodium chloride is used in industry as an efficient olefin hydrogenation catalyst, rhodium acetylacetonate dicarbonyl, triphenylphosphine acetylacetonate carbonyl rhodium, tris(triphenylphosphine)carbonyl hydrogen rhodium, triphenylphos...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/92C07C49/14C07C45/77C07F15/00
Inventor 李晨于海斌蒋凌云李继霞郑书忠刘红光李俊郝婷婷
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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