Preparation method of rhodium compounds

A rhodium compound and compound technology, applied in the field of preparation of rhodium compounds, can solve problems such as unfavorable production and low yield, and achieve the effects of simple operation, high purity and good catalytic effect

Inactive Publication Date: 2016-05-18
JIANGXI HANS PRECIOUS METALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, about the preparation method of bis(1,5-cyclooctadiene) rhodium tetrafluoroborate compound, all are few documents that report the preparation in its laboratory, and the yield is low, which is relatively expensive for the price and resources Not much rhodium metal, not conducive to production

Method used

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  • Preparation method of rhodium compounds

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Dissolve 10 grams of rhodium trichloride trihydrate in 100 milliliters of absolute ethanol and 20 milliliters of water, measure 37.4 milliliters of 1,5-cyclooctadiene in a constant pressure funnel, and replace it with nitrogen for protection, and start to drop 1,5-cyclooctadiene Octadiene, after the dropwise addition, the temperature was raised to 82°C and kept stirring for 18 hours. The reaction solution was concentrated by rotary evaporation, cooled and filtered to obtain 1,5-cyclooctadiene rhodium chloride dimer. Then all the above solids were dissolved in 240 milliliters of dichloromethane and 17.7 milliliters of 1,5-cyclooctadiene, under nitrogen protection, slowly added dropwise at 20°C 60 milliliters of acetone solution containing 7.5 grams of silver tetrafluoroborate, dropwise After heating up to 35°C for reaction for 24 hours, filter, concentrate by rotary evaporation, filter, rinse with methyl tert-butyl ether, and dry under vacuum at room temperature to obtai...

Embodiment 2

[0028] Dissolve 100 grams of rhodium trichloride trihydrate in 1000 milliliters of absolute ethanol and 200 milliliters of water, measure 370 milliliters of 1,5-cyclooctadiene in a constant pressure funnel, and replace it with nitrogen to protect it, and start to add 1,5-cyclooctadiene dropwise. After the addition of octadiene, the temperature was raised to 82°C and kept stirring for 24 hours, concentrated by rotary evaporation, cooled and filtered to obtain 1,5-cyclooctadiene rhodium chloride dimer. It is all dissolved in 2400 milliliters of methylene chloride and 160 milliliters of 1,5 cyclooctadiene, under nitrogen protection, slowly add dropwise 600 milliliters of acetone solution containing 75 grams of silver tetrafluoroborate at 20 ° C, in Reflux at 45°C for 36 hours, filter, concentrate by rotary evaporation, filter, rinse with methyl tert-butyl ether, and dry under vacuum at room temperature to obtain 141.05 g of bis-1,5-cyclooctadiene rhodium tetrafluoroborate. The me...

Embodiment 3

[0030] Dissolve 100 grams of rhodium trichloride trihydrate in 1000 milliliters of absolute ethanol and 200 milliliters of water, measure 374 milliliters of 1,5-cyclooctadiene in a constant pressure funnel, and start to drop 1,5-cyclooctadiene under nitrogen protection. After the addition of octadiene, the temperature was raised to 82°C and kept stirring for 24 hours, concentrated by rotary evaporation, and filtered to obtain 1,5-cyclooctadiene rhodium chloride dimer. Then it was all dissolved in 2000 milliliters of methylene chloride and 160 milliliters of 1,5 cyclooctadiene, under the protection of nitrogen, slowly added dropwise at 20 ℃ containing 600 milliliters of acetone solution containing 75 grams of silver tetrafluoroborate, in Reflux at 45°C for 30 hours, filter, concentrate by rotary evaporation, filter, rinse with methyl tert-butyl ether, and dry under vacuum at room temperature to obtain 138 g of bis-1,5-cyclooctadiene rhodium tetrafluoroborate. The measured metal...

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Abstract

The invention discloses a preparation method of rhodium compounds. According to the method, bis(1.5-cyclooctadiene) rhodium(I) tetrafluoroborate compounds are synthesized in two steps, firstly, 1.5-cyclooctadiene rhodium chloride dimmers are synthesized with rhodium chloride trihydrate as raw materials; secondly, the bis(1.5-cyclooctadiene) rhodium(I) tetrafluoroborate compounds are synthesized with the 1.5-cyclooctadiene rhodium chloride dimmers as raw materials. The one-way total yield is 93% or above, operation is easy, industrial production can be achieved, and certain economic benefits are achieved.

Description

technical field [0001] The invention belongs to the technical field of preparation of precious metal catalysts for organic catalysis, and in particular relates to a preparation method of a rhodium compound. technical background [0002] Rhodium compounds, as noble metal homogeneous catalysts, are widely used in important chemical production processes such as hydroformylation, hydrogenation, and oxo synthesis. For example: three (triphenylphosphine) rhodium chloride is used in industry as an efficient olefin hydrogenation catalyst, rhodium acetylacetonate dicarbonyl, triphenylphosphine acetylacetonate carbonyl rhodium, tris (triphenylphosphine) carbonyl hydrogen rhodium, etc. High-efficiency olefin hydroformylation catalysts are used in olefin hydroformylation industrial units. [0003] At present, about the preparation method of bis(1,5-cyclooctadiene) rhodium tetrafluoroborate compound, all are few documents that report the preparation in its laboratory, and the yield is l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00B01J31/22
CPCC07F15/0073B01J31/2295
Inventor 相亚波李永敏郁丰善何治鸿赵栋云
Owner JIANGXI HANS PRECIOUS METALS CO LTD
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