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Synthesis method of tri-nuclear rhodium acetate (III)

A technology of rhodium acetate and glacial acetic acid, which is applied in the field of synthesis of rhodium compound, i.e., trinuclear rhodium (III) acetate, can solve the problems of many by-products, low yield, high price, etc., and achieve high reaction yield, high product purity, Simple operation effect

Active Publication Date: 2014-06-25
KUNMING INST OF PRECIOUS METALS
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Problems solved by technology

[0005] The preparation method reported in the literature is to use rhodium acetate (II) dimer as a raw material, and use ozone as an oxidant in acetic acid solution to oxidize divalent rhodium to trivalent rhodium, thereby obtaining the trinuclear rhodium acetate (III) product, however , there are two obvious disadvantages in this method: (1) the yield reported in the literature is low, only 32%, indicating that the reaction is very incomplete, which will inevitably lead to many by-products and difficult subsequent purification of the product; (2) the used Rhodium(II) acetate dimer is not a common rhodium compound, and generally needs to be prepared from rhodium trichloride hydrate, and its preparation yield is about 76%.
Rhodium is a very rare metal and is very expensive. Therefore, from the perspective of preparation cost, it is difficult to carry out industrial production with such a low yield

Method used

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  • Synthesis method of tri-nuclear rhodium acetate (III)
  • Synthesis method of tri-nuclear rhodium acetate (III)
  • Synthesis method of tri-nuclear rhodium acetate (III)

Examples

Experimental program
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Embodiment 1

[0013] Example 1 Weigh 40.0 g (0.152 mol) of rhodium trichloride trihydrate and dissolve it in 150 ml of distilled water, slowly add a solution of 38.3 g of sodium bicarbonate dissolved in 400 ml of distilled water under constant stirring, and stir and react at room temperature for 2 hours , stand still, filter, wash with water until no chloride ions can be detected in the washing solution, and dry at 100°C for 3 hours to obtain a yellow rhodium hydroxide solid. The obtained rhodium hydroxide solid was added to 50 ml of glacial acetic acid, stirred and reacted at 60° C. for 3 hours, filtered, the filtrate was concentrated to dryness, and dried at 60° C. for 3 hours to obtain 36.5 grams of brown-red powder, with a yield of 91%.

[0014] Characteristic structural parameters: Elemental analysis: measured values ​​C20.9%, H3.5%, Rh38.8% are consistent with theoretical values ​​C21.2%, H3.4%, Rh39.0%. MS-ESI + m / z:733([M–CH 3 COO] + ). IR(cm -1 ,KBr):3420(s,ν O-H ),1601,1526...

Embodiment 2

[0015] Example 2 Weigh 100.0 g (0.38 mol) of rhodium trichloride trihydrate and dissolve it in 500 ml of distilled water, slowly add a solution of 95.7 g of sodium bicarbonate dissolved in 1000 ml of distilled water under continuous stirring, and stir at 50°C for reaction 1 hours, let stand, filter, wash with water until no chloride ions can be detected in the lotion, and dry at 100°C for 3 hours to obtain a yellow rhodium hydroxide solid. The obtained rhodium hydroxide solid was added to 100 ml of glacial acetic acid, stirred and reacted at 80° C. for 2 hours, filtered, the filtrate was concentrated to dryness, and dried at 60° C. for 3 hours to obtain 95.2 grams of brown-red powder, with a yield of 95%.

[0016] Characteristic structural parameters: Elemental analysis: measured values ​​C20.8%, H3.5%, Rh38.9% are consistent with theoretical values ​​C21.2%, H3.4%, Rh39.0%. MS-ESI + m / z:733([M–CH 3 COO] + ). IR(cm -1 ,KBr):3420(s,ν O-H ),1601,1526(s,ν asC=O ),1418,135...

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Abstract

The invention relates to a novel method for synthesizing trivalent rhodium acetate (III). The method is characterized by comprising the following two steps: (1) dissolving a certain amount of rhodium trichloride hydrate in proper amount of distilled water, adding a sodium hydrogen carbonate water solution according to a stoichiometric ratio, stirring and reacting for 1-2 hours at 20-60 DEG C, and filtering to obtain a yellow rhodium hydroxide solid; (2) stirring and reacting the rhodium hydroxide solid and glacial acetic acid which is 1-5 times as much as a stoichiometric ratio of the rhodium hydroxide solid at 50-100 DEG C for 2-4 hours, filtering, concentrating filtrate to be dry, and drying to obtain a tri-nuclear rhodium acetate (III) product. The tri-nuclear rhodium acetate (III) product is prepared by the method from common rhodium trichloride hydrate through a two-step reaction. The synthesis method disclosed by the invention is simple to operate, high in reaction yield (more than 90%), nearly free from byproduct in reaction and high in product purity (more than 99.0%); the synthesis method is applicable to industrial production.

Description

technical field [0001] The invention relates to a synthesis technology of a rhodium compound, i.e. trinuclear rhodium (III) acetate, belonging to the field of chemistry and chemical engineering. Background technique [0002] Trinuclear rhodium(III) acetate, the chemical name is acetic acid [hexaacetate-μ3-oxygen-trirhodium(III) trihydrate], and its molecular structure is as follows: [0003] [0004] The three rhodium atoms in the molecule of trinuclear rhodium (III) acetate are connected by an oxygen bridge, and every two rhodium atoms are connected by two acetate bridges, and finally each rhodium atom in the molecule is connected by a water molecule. position to form the six-coordinated configuration common to trivalent rhodium. Trinuclear rhodium(III) acetate can catalyze various reactions of olefins and aromatic hydrocarbons, and is an important homogeneous catalyst for the industrial synthesis of various pharmaceutical and chemical products. In addition, trinuclear...

Claims

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Application Information

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IPC IPC(8): C07F15/00
Inventor 叶青松刘伟平余娟常桥稳晏彩先姜婧
Owner KUNMING INST OF PRECIOUS METALS
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