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A kind of preparation method of rhodium octanoate

A technology of octylic acid rhodium and octanoic acid, applied in the field of catalyst preparation, can solve the problems such as cumbersome yield steps of rhodium trichloride trihydrate, separation method separating octanoic acid and octylic acid rhodium, reducing purity and yield, etc., so as to reduce reaction steps and Loss of rhodium, short reaction time, high product yield and effect of purity

Active Publication Date: 2018-08-10
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Pan Lijuan and others used a special solvent to synthesize rhodium octanoate from rhodium acetate, which also had the problem of low rhodium utilization [Pan Lijuan, Wang Hui, Wang Zhaowen, etc. Synthesis of octanoic rhodium dimer [J]. Industrial Catalysis, 2014, (03):232-234.]
Liu Guihua et al. proposed the method of using trihydrate rhodium trichloride directly to react with octanoic acid to prepare rhodium octanoate in the patent CN101891606B and literature, but the method used excessive octanoate, rhodium octanoate has good solubility in octanoic acid, and the purity will be reduced during separation and yield, and the preparation steps from rhodium to trihydrate rhodium trichloride are cumbersome, the yield is not high, and the utilization rate of rhodium is limited [Liu Guihua, Ye Qingsong, Pan Zaifu, etc. Synthesis and structure of rhodium octanoate (Ⅱ) Characterization[J]. Precious Metals, 2012(4):18-21.]
The patent application CN102786406A uses a synthetic method using sodium chlororhodium acid as a raw material, but also uses an excessive amount of octanoic acid, and does not use an effective separation method to separate octanoic acid and rhodium octanoate, which affects the yield and purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: Add 25mmol rhodium hydroxide to a 100mL reaction flask, add 150mmol octanoic acid, heat to 100°C in an oil bath, stir and react for 7 hours to obtain a green solution, add 50mL ethanol and heat to dissolve, then use 1mol / L sodium hydroxide Adjust the pH of the ethanol solution to 9, and a white sodium octanoate solid precipitates. After filtration, heat and concentrate the filtrate until a green solid precipitates. Cool in an ice-water bath to 0°C. After the green solid is filtered out, the green solid is dried in an oven at 80°C for 2 hours to obtain a green rhodium octanoate solid. 9.64g, yield 99.13%; the elemental composition of the product was analyzed, wherein the carbon and hydrogen content was measured by an elemental analyzer, and the rhodium content was measured by an atomic absorption spectrometer. The measurement results were as follows: measured value C, 49.46%; H, 7.81%; Rh, 26.32%; Theoretical value C, 49.36%; H, 7.77%; Rh, 26.43%; The measured ...

Embodiment 2

[0015] Example 2: Add 100mmol rhodium hydroxide to a 250mL reaction flask, add 650mmol octanoic acid, heat to 110°C in an oil bath, stir and react for 5 hours to obtain a green solution, add 150mL ethanol and heat to dissolve, then use 1.5mol / L sodium hydroxide Adjust the pH of the ethanol solution to 10, and white sodium octanoate solids precipitated. After filtration, the filtrate was heated and concentrated until a green solid precipitated, cooled in an ice-water bath to 0°C, and the green solid was filtered out, then vacuum-dried in an oven at 80°C for 2 hours to obtain a green rhodium octanoate solid. 38.49g, yield 98.84%; the elemental composition analysis results of the product are as follows: measured value C, 49.62%; H, 7.82%; Rh, 26.28%; measured value is consistent with theoretical value, and the purity is 99.3%.

Embodiment 3

[0016] Example 3: Add 0.3 mol of rhodium hydroxide to a 1L reaction flask, add 1.5 mol of octanoic acid, heat to 105°C in an oil bath, stir and react for 6 hours to obtain a green solution, add 600 mL of ethanol to dissolve, and use 0.5 mol / L hydrogen Sodium oxide ethanol solution adjusted pH to 11, white sodium octanoate solid precipitated, filtered, heated and concentrated filtrate until green solid precipitated, cooled in ice-water bath to 0°C, filtered the green solid, dried in oven at 80°C for 3 hours in vacuum to obtain green octanoic acid Rhodium solid 115.9g, yield 99.24%; product element composition analysis results are as follows: measured value C, 49.55%; H, 7.80%; Rh, 26.31%; The measured value is consistent with the theoretical value, and the purity is 99.0%.

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Abstract

The invention discloses a preparation method of rhodium octanoate dimmer.The method includes the steps of adding octanoic acid to rhodium hydroxide to be heated to 90-110 DEG C through an oil bath to react for 4-8 hours, adding ethyl alcohol after reaction ends to be heated and dissolved, adjusting pH to be 8-11 through a sodium hydroxide ethanol solution after dissolving, conducting filtering, heating and concentrating on filtrate, conducting cooling to separate out green solid, and conducting vacuum drying on the solid after filtering to obtain green rhodium octanoate dimmer solid.Rhodium hydroxide serves as the raw material, and the method is rapid in reaction speed, little in pollution, high in yield (larger than 98.0%), high in purity (larger than 99.0%), and suitable for industrial production.

Description

technical field [0001] The invention discloses a preparation method of a precious metal rhodium catalyst, in particular to a synthesis method of rhodium octanoate. Background technique [0002] Rhodium octanoate is an important rhodium homogeneous catalyst, which has remarkable catalytic activity for cyclopropanation reaction, olefin hydroformylation reaction, ring closure reaction, etc., and is widely used in the fields of basic chemical industry, pharmaceutical and chemical industry. On electron-deficient alkenes and heterocyclic alkenes, only rhodium has a catalytic effect, and hydroformylation can convert alkenes produced by oil refining into more valuable aldehydes. With the rapid development of the domestic chemical industry, the demand for high-quality rhodium octanoate is also gradually increasing. As a rare and expensive metal, rhodium must also focus on the utilization rate of rhodium when it is used to make rhodium octanoate. Therefore, a high-efficiency, Environ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/41C07C53/126
CPCC07C51/412C07C53/126
Inventor 高传柱余从涛
Owner KUNMING UNIV OF SCI & TECH
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