Preparation method of acetylacetone triphenylphosphine carbonyl rhodium (I)

Abstract

The invention discloses a synthetic method of acetylacetone triphenylphosphine carbonyl rhodium (I). The method comprises the following steps: (1) mixing rhodium trichloride hydrate and N,N-dimethylfomamide (DMF), heating to 130-150 DEG C under the protection of nitrogen, adding acetylacetone after rhodium trichloride is completely dissolved, heating until reflux reaction is performed for 0.5-1.5 hours, then putting the reaction solution in a power ultrasound area in a room temperature state, adding a precipitation enhancer in a low temperature state, and performing precipitation after-treatment, thereby preparing acetylacetone dicarbonyl rhodium (I); and (2) dissolving the acetylacetone dicarbonyl rhodium (I) prepared in the step (1) by using an organic solvent, adding triphenylphosphine which causes generation of bubbles, performing reflux reaction for 0.5-1 hour until no bubble is generated, putting the reaction solution in the power ultrasound area in the room temperature state to perform crystallization and precipitation, and treating to obtain acetylacetone triphenylphosphine carbonyl rhodium (I). By adopting the method disclosed by the invention, the total yield of acetylacetone triphenylphosphine carbonyl rhodium (I) is obviously improved, and the production cost is reduced; and a relatively environment-friendly solvent is adopted, so that benzene and toluene which are harmful to human bodies are avoided, environmental pollution is reduced, and safety is improved.

Description

technical field [0001] The invention relates to a preparation method of triphenylphosphine carbonyl rhodium (I) acetylacetonate. Background technique [0002] Triphenylphosphinecarbonyl rhodium(I) acetylacetonate is an alpha-olefin and syngas (CO and H 2 A good catalyst for the hydroformylation reaction to generate normal and isomeric aldehydes. For example, propylene and synthesis gas generate n-butyraldehyde and isobutyraldehyde in the presence of triphenylphosphinecarbonyl rhodium(I) acetylacetonate homogeneous catalyst. [0003] Because rhodium is a kind of extremely expensive rare metal, the key technology of mass production of acetylacetonate triphenylphosphine carbonyl rhodium (I) is exactly to improve its synthesis yield, thereby reducing the synthesis cost of catalyst. In addition, when triphenylphosphinecarbonyl rhodium (I) acetylacetonate is used as a homogeneous complexation catalyst for olefin hydroformylation, it is also required that the content of harmful i...

AI Technical Summary

Problems solved by technology

But because the price of rhodium is extremely expensive, and there is almost no natural resource of rhodium in the country, increasing the yield by 1 percentage point is enough to offset other costs of preparing acetylacetonate triphenylphosphinecarbonyl rhodium (I), and can also reduce the recovery in the waste liquid after synthesis The cost of rhodium, so in acetylacetonate triphenylphosphine carbonyl rhodium (I) catalyst industrial production, synthesis yield is extremely important, and all adopt non-environmentally friendly solvents such as toluene or benzene in the past report technology, and will pass through distillation process, The steps are long, which is not good for industrial production