Preparation method of tris[tri(3-sodium sulfonate-phenyl)phosphine]rhodium carbonylhydride

Abstract

The invention relates to a preparation method of tris[tri(3-sodium sulfonate-phenyl)phosphine]rhodium carbonylhydride, which is characterized by comprising the following steps: mixing a sodium hexachlororhodate hydrate alcoholic solution with a tri(3-sodium sulfonate-phenyl)phosphine water solution, introducing carbon monoxide gas into the mixed solution, heating the reaction solution to 70-90 DEG C, keeping the temperature for 60-90 minutes, adding a potassium hydroxide ethanol solution into the reaction solution, introducing hydrogen gas into the reaction solution, continuing heating the reaction solution to 70-90 DEG C, keeping the temperature for 1-2 hours, cooling, and separating and recycling the product, wherein the alcohol is selected from ethanol, 1-propanol and 2-propanol; the molar concentration of the sodium hexachlororhodate hydrate alcoholic solution is 0.1-1.0 mol / L, the molar concentration of the tri(3-sodium sulfonate-phenyl)phosphine water solution is 1.0-2.0 mol / L, and the mol ratio of tri(3-sodium sulfonate-phenyl)phosphine to sodium hexachlororhodate hydrate is 4-10; and the molar concentration of the potassium hydroxide ethanol solution is 4.0-8.0 mol / L, and the mol ratio of potassium hydroxide to sodium hexachlororhodate hydrate is 6-12.

Description

technical field [0001] The invention relates to the technical field of catalysis, and relates to a method for preparing a tris[tris(3-sulfonate sodium phenyl)phosphine]rhodium carbonyl hydride which is a homogeneous reaction catalyst or a catalyst precursor. 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. Among them, the water-soluble tris[tris(3-sodium phenyl sulfonate)phosphine]rhodium carbonyl hydride [RhH(CO)(TPPTS) 3 ] is often used as a catalyst for the hydroformylation of olefins in an oil-water two-phase system with water as the reaction solvent. According to the method reported in J.Organomet.Chem.389 (1990), 85-101, Rh 2 (CH 3 COO) 4 , Tris (3-sodium phenyl sulfonate) ...

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Problems solved by technology

As can be seen from the description of the above process, although the rhodium powder can be efficiently converted into a water-soluble rhodium salt through the above two methods, it still needs to be neutralized by alkali to produce hydrated rhodium oxide, and the hydrated rhodium oxide is washed to remove impurity ions and dissolved in hydrochloric acid. Rhodium trichloride hydrate can only be obtained after steps such as evaporating and concentrating. The whole process is relatively complicated, and in the process of neutralizing rhodium oxide hydrate with alkali, the rhodium in the solution cannot be completely converted into rhodium gel, and some Exist in the solution, and each step of the process will have a certain amount of rhodium loss, resulting in a lower yield per pass for the preparation of rhodium trichloride hydrate. The yield of rhodium chloride hydrate produced by the above method is generally not more than 65%.