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Purifying method for acetylacetonatodicarbonyl rhodium

A technology of acetone dicarbonyl rhodium and acetyl is applied in the field of purifying hydroformylation reaction catalyst acetylacetonate dicarbonyl rhodium, and can solve problems such as deactivation

Inactive Publication Date: 2015-05-13
KUNMING INST OF PRECIOUS METALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to solve the problem that the rhodium acetylacetonate dicarbonyl catalyst is susceptible to the inactivation of chloride ions in the hydroformylation reaction, and to provide an effective method for purifying rhodium acetylacetonate dicarbonyl, which can be convenient, simple, quick and effective Reduce the chloride ion content to less than 50ppm without additional economic cost, suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 50.0 grams of rhodium trichloride hydrate (the rhodium content is 38.2%), join in 1 liter of dimethylformamide, after stirring for 10 minutes, slowly heat to reflux, add 100 milliliters of acetylacetone and continue the reflux reaction for 1 hour, Cool to room temperature, add 5 liters of deionized water, filter, and wash with 200 ml of water to obtain a red crude rhodium acetylacetonate dicarbonyl.

[0025] Add 100ml of deionized water to the above crude rhodium acetylacetonate dicarbonyl, fully stir, and let it stand, after the rhodium acetylacetonate dicarbonyl begins to precipitate (partially float), add dropwise a silver nitrate solution with a mass concentration of 0.5% until the supernatant After turbidity occurs again, add 10% of the added amount dropwise, fully stir, filter, and wash twice with 200ml deionized water.

[0026] Add the filter cake to 1.5 liters of n-hexane, add anhydrous sodium carbonate under constant stirring, add 50% of the added amount ...

Embodiment 2

[0033]Weigh 100.0 grams of rhodium trichloride hydrate (rhodium content is 38.2%), join in 2 liters of dimethylformamide, after stirring for 10 minutes, slowly heat to reflux, add 200ml acetylacetone and continue the reflux reaction for 1 hour, cool To room temperature, 10 liters of deionized water was added, filtered, and washed with 200 ml of water to obtain a red crude rhodium acetylacetonate dicarbonyl.

[0034] Add 200ml of deionized water to the above crude rhodium acetylacetonate dicarbonyl, fully stir, and let it stand until the rhodium acetylacetonate dicarbonyl starts to precipitate (partially floats), then add dropwise a silver nitrate solution with a mass concentration of 2% until the supernatant is no longer After turbidity occurs again, add 30% of the added amount dropwise, fully stir, filter, and wash twice with 200ml deionized water.

[0035] The filter cake is added in 4 liters of cyclohexane, anhydrous potassium carbonate is added under constant stirring, and...

Embodiment 3

[0039] Weigh 50.0 grams of rhodium trichloride hydrate (the rhodium content is 38.2%), join in 1 liter of dimethylformamide, after stirring for 10 minutes, slowly heat to reflux, add 100 milliliters of acetylacetone and continue the reflux reaction for 1 hour, Cool to room temperature, add 5 liters of deionized water, filter, and wash with 200 ml of water to obtain a red crude rhodium acetylacetonate dicarbonyl.

[0040] Add 100ml of deionized water to the crude rhodium acetylacetonate dicarbonyl, fully stir, and let it stand until the rhodium acetylacetonate dicarbonyl starts to precipitate (partially floats), then add dropwise a silver nitrate solution with a mass concentration of 1% until the supernatant is no longer After turbidity occurs again, add 50% of the added amount dropwise, fully stir, filter, and wash twice with 200ml deionized water.

[0041] Add the filter cake to 1.5 liters of n-hexane, add anhydrous sodium carbonate under continuous stirring, add 10% of the a...

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PUM

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Abstract

The invention relates to a purifying method for acetylacetonatodicarbonyl rhodium. The method comprises the following concrete steps: (1) adding deionized water into a crude acetylacetonatodicarbonyl rhodium product, carrying out full stirring, then carrying out standing, dropwise adding a silver nitrate solution until supernatant is no longer turbid, then replenishing a certain amount of the silver nitrate solution, carrying out stirring and filtering, and washing the obtained filter cake with water; and (2) adding the filter cake into an appropriate organic solvent, adding a moisture scavenger under stirring, carrying out filtering, and treating the obtained filtrate in the manners like concentrating crystallization or cooling crystallization so as to obtain solid acetylacetonatodicarbonyl rhodium, or using the obtained filtrate as a further reaction solution for the preparation of acetylacetonatocarbonyltriphenylp hosphinerhodium. The method provided by the invention omits the step of drying in conventional preparation of acetylacetonatodicarbonyl rhodium; under the condition of no additional operation process, the problem of inactivation of an acetylacetonatodicarbonyl rhodium catalyst in hydroformylation reaction due to susceptibility to affection by chloride ions can be conveniently, quickly and effectively overcome; meanwhile, the method is applicable to industrial production.

Description

technical field [0001] The invention relates to a method for purifying rhodium acetylacetonate dicarbonyl, a catalyst for hydroformylation reaction, and belongs to the field of chemical engineering. Background technique [0002] The hydroformylation reaction refers to the reaction of alkenes with CO and H 2 A reaction in which an aldehyde is formed under the action of a catalyst. Since aldehydes and their downstream products are the starting materials for the production of various detergents, surfactants, pharmaceuticals and fragrances and other high-value-added fine chemicals, hydroformylation has become one of the most important industrial homogeneous catalytic reactions , the global annual production of aldehydes and alcohols through hydroformylation has exceeded 10 million tons. [0003] Rhodium acetylacetonate dicarbonyl (chemical formula is Rh(C 5 h 7 o 2 )(CO) 2 ) is an important catalytic precursor compound for catalyzing hydroformylation reactions. For exampl...

Claims

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Application Information

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IPC IPC(8): C07F15/00
CPCC07F15/008
Inventor 叶青松刘伟平余娟常桥稳姜婧晏彩先
Owner KUNMING INST OF PRECIOUS METALS
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