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Carbene iridium catalyst and preparation method and application thereof

A catalyst, carbene iridium technology, applied in the field of carbene iridium catalyst preparation, can solve the problems of high energy consumption, easy precipitation and deactivation of metal iridium, equipment corrosion, etc., achieves good reaction stability, solves the problem of long production process route and low cost. Effect

Active Publication Date: 2020-04-28
NANJING YANCHANG REACTION TECH RES INST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, iridium-based catalysts still have problems such as severe corrosion of equipment by the reaction system, easy precipitation and deactivation of metal iridium, and high energy consumption caused by a certain amount of water in the reaction system.

Method used

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  • Carbene iridium catalyst and preparation method and application thereof
  • Carbene iridium catalyst and preparation method and application thereof
  • Carbene iridium catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Embodiment 1 prepares carbene iridium catalyst

[0049] In the glove box, accurately measure 0.2006g CAAC ligand, 0.1097g KHMDS and 0.1678g [Ir(COD)Cl] 2 Place in a 100 mL Shrek bottle, place the Shrek bottle in a Dewar bottle, and replace the reaction system with nitrogen. Then, add 100mL of acetone to the Dewar bottle, and then add liquid nitrogen to the acetone until the acetone is frozen into ice. At this time, the temperature of the reaction system drops to -78°C, and slowly add about 40mL of tetrahydrofuran after dehydration to the Shrek bottle. . After the reaction system returned to room temperature naturally, it was reacted overnight to obtain the crude product of CAAC-IrCl(COD).

[0050] Dissolve the crude CAAC-IrCl(COD) with a small amount of dichloromethane, then filter the desalinated product with diatomaceous earth, and then purify the desalted crude CAAC-IrCl(COD) with a silica gel column, benzene:n-hexane=1:1 As an eluent, after rotary evaporation and...

Embodiment 2

[0052] Embodiment 2 prepares carbene iridium catalyst

[0053] In the glove box, accurately measure 0.4012g CAAC ligand, 0.2194g KHMDS and 0.3356g [Ir(COD)Cl] 2 Place in a 100 mL Shrek bottle, place the Shrek bottle in a Dewar bottle, and replace the reaction system with nitrogen. Then, add 100mL of acetone to the Dewar bottle, and then add liquid nitrogen to the acetone until the acetone is frozen into ice. At this time, the temperature of the reaction system drops to -78°C, and slowly add about 50mL of tetrahydrofuran after dehydration to the Shrek bottle. . After the reaction system returned to room temperature naturally, it was reacted overnight to obtain the crude product of CAAC-IrCl(COD).

[0054] Dissolve the crude CAAC-IrCl(COD) with a small amount of dichloromethane, then filter the desalinated product with diatomaceous earth, and then purify the desalted crude CAAC-IrCl(COD) with a silica gel column, benzene:n-hexane=1:1 As an eluent, after rotary evaporation and...

Embodiment 3

[0056] Embodiment 3 methanol carbonylation prepares methyl acetate

[0057] Take by weighing the CAAC-IrCl (COD) 80mg of embodiment 1 and place in the autoclave, add methanol 5mL therein, iodomethane 0.2mL, pass into CO replacement 3 times, make the pressure in the reaction system reach 2.0MPa, at a temperature of React at 120°C for 20 hours, stir with magnetic force at a stirring speed of 500 rpm, and the total pressure of the system at this time is about 2.5 MPa. After the reaction, the autoclave was cooled to room temperature.

[0058] Analyzed by gas chromatography, see figure 1 , the conversion rate of methanol is 81%, and the selectivity of methyl acetate is as high as 97%.

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Abstract

The invention provides a carbene iridium catalyst and a preparation method and application thereof, the carbene iridium catalyst has good application in preparation of methyl acetate through methanolcarbonylation, and the carbene iridium catalyst is mainly prepared from a CAAC ligand, 1, 5-cyclooctadiene iridium chloride and bis(trimethylsilane) amino potassium as raw materials. The preparation method comprises the following steps: drying raw materials for preparing the carbene iridium catalyst, replacing with nitrogen, sequentially adding acetone and liquid nitrogen, performing reacting at-78 DEG C, and extracting a reaction product with a solvent. According to the invention, the CAAC-IrCl (COD) catalyst of the CAAC ligand with relatively strong electron donating capability is applied tothe aspect of preparing methyl acetate through methanol carbonylation, so that the stability of the catalyst is improved, the methyl acetate is directly prepared under relatively mild and anhydrous conditions, the preparation process is simplified, and the operation cost is reduced.

Description

technical field [0001] The invention relates to the field of preparation of carbene iridium catalysts, in particular to a carbene iridium catalyst and its preparation method and application. Background technique [0002] Methyl acetate is a very important chemical product, which is widely used in the production process of resins, adhesives, leather and polyurethane foam blowing agents. At present, the production of methyl acetate is industrially prepared by esterification reaction of methanol and acetic acid under the catalysis of concentrated sulfuric acid, and the whole reaction system corrodes the equipment more seriously. [0003] Industrial methanol carbonylation catalysts for the production of acetic acid have gone through three stages: the cobalt-based catalyst developed by BASF, the rhodium-based catalyst developed by Monsanto, and the iridium-based catalyst developed by BP. Among them, the iridium-based catalyst has relatively cheap price and low water content. As ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C67/36C07C69/14C07F15/00
CPCB01J31/2265C07C67/36C07F15/0033B01J2531/827C07C69/14Y02P20/584
Inventor 张志炳张德谨胡兴邦周政杨国强
Owner NANJING YANCHANG REACTION TECH RES INST CO LTD
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