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A kind of recovery regeneration method of 1,5-cyclooctadiene iridium chloride dimer

A technology of cyclooctadiene iridium chloride and cyclooctadiene, which is applied in the field of recovery and regeneration of 1,5-cyclooctadiene iridium chloride dimer, which can solve the problems of loss of catalytic activity, high cost, easy oxidation, etc. problems, to achieve the effect of simple operation process, lower production cost and higher utilization rate

Active Publication Date: 2016-09-14
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[(COD)IrCl] 2 It is an air-sensitive compound. When it is placed for a long time or stored improperly, it is easy to oxidize and cause loss or partial loss of catalytic activity.
For example, in the industrial production process of refined metolachlor, the newly prepared [(COD)IrCl] 2 When catalyzing the hydrogenation of imines, the amount of catalyst used is only 1 / 500,000 of the molar amount of imines; long-term storage of [(COD)IrCl] is used 2 In catalytic hydrogenation, the amount of catalyst needs to be more than one hundred thousandth of the molar amount of imine, and the cost is very high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] In the reactor, put 2 g of inactivated [(COD)IrCl] 2 and 10 milliliters of 20% (mass) hydrochloric acid, heated to reflux for 4 hours. After cooling, the solution was transferred to a separatory funnel, and extracted with 10 ml of diethyl ether. The liquid was separated, the lower aqueous phase was collected, and the water was distilled off under reduced pressure to obtain a black solid. The black solid was collected in a reactor, 2.5 ml of 1,5-cyclooctadiene, 8 ml of isopropanol and 30 ml of water were added, and refluxed for 12 hours under nitrogen atmosphere. Let it stand and cool down to room temperature naturally, a red solid precipitates out in the lower part of the reactor, filter it, rinse the filter cake with a small amount of water and cold methanol, and vacuum-dry the filter cake to obtain 1.8 g of active [(COD)IrCl] 2 Compound, content 98.1%, yield 90%. After the filtrate is collected, it is concentrated or evaporated to dryness, and the above process is ...

Embodiment 2

[0017] In the reactor, put 2 g of inactivated [(COD)IrCl] 2 and 10 milliliters of 20% (mass) hydrochloric acid, heated to reflux for 4 hours. After cooling, the solution was transferred to a separatory funnel, and extracted with 10 ml of diethyl ether. The liquid was separated, the lower aqueous phase was collected, and the water was distilled off under reduced pressure to obtain a black solid. The black solid was collected in a reactor, 2 ml of 1,5-cyclooctadiene, 6 ml of ethanol and 30 ml of water were added, and the mixture was refluxed for 12 hours under nitrogen atmosphere. Leave to stand and cool down to room temperature naturally, a red solid precipitates out in the lower part of the reactor, filter, rinse the filter cake with a small amount of water and cold methanol, and vacuum-dry the filter cake to obtain 1.4 g of active [(COD)IrCl] 2 Compound, content 98.3%, yield 70%.

Embodiment 3

[0019] In the reactor, put 2 g of inactivated [(COD)IrCl] 2 And 8 milliliters of 5% (mass) hydrochloric acid, heated to reflux for 4 hours. After cooling, the solution was transferred to a separatory funnel, and extracted with 10 ml of diethyl ether. The liquid was separated, the lower aqueous phase was collected, and the water was distilled off under reduced pressure to obtain a black solid. The black solid was collected in a reactor, 3 ml of 1,5-cyclooctadiene, 8 ml of isopropanol and 30 ml of water were added, and refluxed for 12 hours under nitrogen atmosphere. Let it stand and cool down to room temperature naturally, a red solid precipitated from the lower part of the reactor, filtered, rinsed the filter cake with a small amount of water and cold methanol, and vacuum-dried the filter cake to obtain 0.9 g of active [(COD)IrCl] 2 Compound, content 98.1%, yield 45%.

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Abstract

The invention discloses a 1,5-cyclooctadiene iridium chloride dimer [(COD)IrCl] 2 The recovery and regeneration method: the inactivated or partially inactivated [(COD)IrCl] 2 Convert in hydrochloric acid to obtain iridium chloride mixture, react iridium chloride mixture and 1,5-cyclooctadiene in alcohol-water system to regain activity [(COD)IrCl] 2 compound. The recovery and regeneration method of 1,5-cyclooctadiene iridium chloride dimer disclosed by the invention can improve the utilization rate of precious metal iridium and effectively reduce production cost. The method has simple operation process, high recovery rate and mild conditions. The invention is suitable for the recovery of precious metal iridium catalysts.

Description

technical field [0001] The invention belongs to the technical field of recovery of precious metal catalysts, and in particular relates to a method for recovery and regeneration of 1,5-cyclooctadiene iridium chloride dimer. technical background [0002] 1,5-cyclooctadiene iridium chloride dimer ([(COD)IrCl] 2 ) is an important noble metal catalyst, which is widely used in the catalytic synthesis process of various C-C bonds, C-O bonds and C-N bonds and the catalytic hydrogenation process of double bonds. In the industrial production process of the herbicide (S)-metolachlor (smart metolachlor), the catalyst for the key asymmetric hydrogenation reaction is the use of [(COD)IrCl] 2 As a precursor (C.R. Chimie 2002, 5, 379.). [(COD)IrCl] 2 Generally prepared from iridium chloride (Inorg. Chim. Acta 2006, 359, 3800; EP1116742). [(COD)IrCl] 2 It is an air-sensitive compound. When it is placed for a long time or stored improperly, it is easy to oxidize and cause loss or partial...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/02B01J31/40B01J31/16
CPCY02P20/584
Inventor 王月梅林双政徐泽刚宁斌科杨翠凤卫天琪张媛媛
Owner XIAN MODERN CHEM RES INST
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