A kind of synthetic method of triphenylphosphine carbonyl rhodium acetylacetonate

Abstract

The invention discloses a synthesis method of rhodium(triphenylphosphine)carbonylacetylacetonate.The method includes the steps of conducting backflow reaction on rhodium chloride trihydrate and a triphenylphosphine solution to prepare triphenylphosphine rhodium chloride, mixing prepared triphenylphosphine rhodium chloride with N,N-dimethylformamide under the protection of nitrogen, then adding acetylacetone, conducting backflow heating reaction, cooling to the room temperature, concentrating a solution, adding icy water, standing, separating out crystals, conducting filtering, washing filter cakes with water, and conducting vacuum drying to obtain rhodium(triphenylphosphine)carbonylacetylacetonate.By means of the new synthesis method, intermediates are replaced with triphenylphosphine rhodium chloride capable of being stably stored in air, the step-by-step yield and once through yield of the product are increased, and benzene and alkane type toxic solvent are not used; by means of environment-friendly type solvent ethyl alcohol, production cost is reduced, and remarkable economic and environment advantages are achieved.

Description

technical field [0001] The invention relates to a synthesis method of a catalyst, in particular to a synthesis method of triphenylphosphinecarbonyl rhodium acetylacetonate. Background technique [0002] Triphenylphosphinecarbonyl rhodium acetylacetonate is the core catalyst in the low-pressure propylene hydroformylation carbonylation process to synthesize butanol and octanol. Because rhodium natural resources are scarce, the price is very expensive, and there are almost no natural resources of rhodium in China; improving the synthesis yield of acetylacetonate triphenylphosphinecarbonyl rhodium catalyst and reducing the catalyst synthesis cost become the key. [0003] Triphenylphosphine carbonyl rhodium acetylacetonate was first synthesized by British chemist G.Wilkinson [Bonati F, Wilkinson G. Preparation of carbonyl (triphenylphosphine) rhodium [J]. J.Chem. Soc., 1964,3156-3159. ], M.J.Lawrenson[Lawerenson M J. Some Rh-complexes in synthesis of oxo alcohols[P]. British Pat...

AI Technical Summary

Problems solved by technology

But because the price of rhodium is extremely expensive, and there are almost no natural resources of rhodium in the country, increasing the yield by 1 percentage point is enough to offset other costs of preparing triphenylphosphine acetylacetonate rhodium, and can also reduce the cost of reclaiming rhodium in the waste liquid after synthesis. Therefore, in the industrial production of triphenylphosphine-rhodium acetylacetonate catalyst, the synthesis yield is extremely important, and non-environmentally friendly solvents such as toluene or benzene have been used in previous reports, and the distillation process will take longer steps and the loss of precious metal rhodium Relatively large, not good for industrial production