Preparation method of acetylacetone dicarbonyl rhodium and mixed C4 hydroformylation method

A technology of acetone dicarbonyl rhodium and acetylacetone, applied in the field of formylation catalysts, can solve the problems of high reaction temperature, low yield and high chlorine content in products, and achieves the effects of mild reaction conditions, high reaction rate and high catalytic activity

Active Publication Date: 2020-06-26
CHINA NAT OFFSHORE OIL CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcoming that existing production technology of rhodium acetylacetonate dicarbonyl has long reaction time, high reaction temperature, complicated post-treatment steps, low yield, and high chlorine content of the product leading to poor catalytic activity. Method for preparing rhodium acetylacetonate dicarbonyl with low chlorine content in higher yield under reaction conditions

Method used

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  • Preparation method of acetylacetone dicarbonyl rhodium and mixed C4 hydroformylation method
  • Preparation method of acetylacetone dicarbonyl rhodium and mixed C4 hydroformylation method
  • Preparation method of acetylacetone dicarbonyl rhodium and mixed C4 hydroformylation method

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preparation example Construction

[0016] The invention provides a method for preparing rhodium dicarbonyl acetylacetonate, which comprises the following steps: stirring and mixing an aqueous solution of rhodium oxide hydrate, an organic carboxylic acid catalyst and acetylacetone, heating to 60-120°C, preferably 80-100°C, and then feeding Carbon monoxide is reacted, and after the reaction is completed, the reaction liquid is cooled and filtered, the filter cake is washed with deionized water, and the wet base product of rhodium acetylacetonedicarbonyl is obtained after suction filtration, which can be used for rhodium in mixed carbon tetrahydroformylation reactions. catalyst. The concentration of the hydrated rhodium oxide aqueous solution is 0.010-2.00 mol / liter, preferably 0.10-1.00 mol / liter; the amount of acetylacetone added is such that the molar ratio of acetylacetone to rhodium is 1.0-10.0, preferably 3.0-8.0, More preferably 4.0~6.0; The organic carboxylic acid is selected from one or more of C2~C20 org...

Embodiment 1

[0031] This embodiment is used to illustrate the preparation method of rhodium acetylacetonate dicarbonyl provided by the present invention.

[0032] In a round-bottomed three-neck flask equipped with a condenser tube and gas inlet and outlet pipelines, dissolve rhodium oxide hydrate containing 0.03mol rhodium in 300mL deionized water, add 0.0003mol acetic acid and 0.24mol acetylacetone, stir and mix, and replace with nitrogen three times Afterwards, be warming up to 100 ℃, pass into carbon monoxide (purity 99.9 volume %) gas with the flow rate of 15 milliliters / minute, react under stirring for 2 hours, after the completion of the reaction, the reaction solution is cooled, and a blood-red solid is separated out, filtered, washed with deionized water, After suction filtration, the rhodium dicarbonyl acetylacetonate wet base is obtained, and the rhodium dicarbonyl acetylacetonate yield can be calculated by detecting the rhodium content in the product and the raw material. The yi...

Embodiment 2

[0034] This embodiment is used to illustrate the preparation method of rhodium acetylacetonate dicarbonyl provided by the present invention.

[0035] In a round-bottomed three-neck flask equipped with a condenser tube and gas inlet and outlet pipelines, dissolve hydrated rhodium oxide containing 0.03mol rhodium in 30mL deionized water, add 0.003mol propionic acid and 0.18mol acetylacetone, stir and mix, and replace with nitrogen After three times, heat up to 80°C, feed carbon monoxide (purity 99.9% by volume) gas at a flow rate of 15 ml / min, and react for 2 hours under stirring. After the reaction is completed, the reaction liquid is cooled, and a blood-red solid is precipitated, filtered, and washed with deionized water After suction filtration, the rhodium dicarbonyl acetylacetonate wet base is obtained, and the rhodium dicarbonyl acetylacetonate yield can be calculated by detecting the rhodium content in the product and the raw material. The yield and product analysis resul...

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Abstract

The invention discloses a preparation method of acetylacetone dicarbonyl rhodium and a mixed C4 hydroformylation method. The preparation method comprises the following steps of: stirring and mixing arhodium oxide hydrate aqueous solution, an organic carboxylic acid catalyst and acetylacetone, performing heating to a reaction temperature, introducing carbon monoxide for reaction, then conducting filtering at the end of the reaction, washing a filter cake with deionized water, and carrying out suction filtration to obtain acetylacetone dicarbonyl rhodium. The invention further discloses a mixedC4 hydroformylation method. The method comprises the preparation steps of acetylacetone dicarbonyl rhodium. According to the preparation method disclosed by the invention, the acetylacetone dicarbonyl rhodium with a low chlorine content can be prepared at high yield, meanwhile, due to mild reaction conditions, insoluble substances cannot be generated in a high-temperature reaction process, the obtained acetylacetone dicarbonyl rhodium product can be directly applied to a mixed C4 hydroformylation reaction, and the processes of product drying, recrystallization and the like are omitted.

Description

Technical field: [0001] The invention relates to the field of formylation catalysts, in particular to a preparation method of rhodium acetylacetonate dicarbonyl and a method for hydroformylation reaction of n-butene and synthesis gas in mixed C4 catalyzed by the prepared rhodium acetylacetonate dicarbonyl. Background technique: [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 hydroformylation, and many of them have been used in industrial production. For example: Tris (triphenylphosphine) rhodium chloride is used in industry as an efficient olefin hydrogenation catalyst, rhodium acetylacetonate dicarbonyl [Rh(acac)(CO) 2 ], triphenylphosphine acetylacetonate carbonyl rhodium, tris (triphenylphosphine) carbonyl hydrogen rhodium, three [tris (m-sulfonate phenyl) phosphine] carbonyl rhodiu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00B01J31/22B01J31/20C07C45/50C07C47/02
CPCC07F15/008B01J31/2213B01J31/20C07C45/505B01J2531/822B01J2531/0238B01J2231/321C07C47/02Y02P20/584
Inventor 吴青李晨蒋凌云王鹏飞郝婷婷王本雷李继霞臧甲忠
Owner CHINA NAT OFFSHORE OIL CORP
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