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Method for maintaining or generating positive-monovalent rhodium catalyst active center

A rhodium catalyst and active technology, applied in the field of maintaining or generating positive monovalent rhodium catalyst active centers, can solve the problems of low carbonylation reaction activity, inability to maintain active centers, etc. Effect

Inactive Publication Date: 2017-11-17
SHANGHAI HUAYI GRP CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by this invention is that the rhodium catalyst cannot maintain the active center [Rh(CO) under low water and low CO partial pressure in the prior art. 2 I 2 ] - , leading to the problem of low carbonylation reaction activity, providing a new method for maintaining or generating positive monovalent rhodium catalyst active centers

Method used

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  • Method for maintaining or generating positive-monovalent rhodium catalyst active center
  • Method for maintaining or generating positive-monovalent rhodium catalyst active center

Examples

Experimental program
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Effect test

Embodiment 1

[0038] The positive trivalent trans-[Rh(CO) of the rhodium mass content of the prepared 5000ppm 2 I 4 ] - Add the mass content of ruthenium [Ru(CO) of 5000ppm 3 I 3 ] - , the water content in the system is 4%, adding lithium iodide, the mass content of lithium is about 3360×10 -6 , the rest is acetic acid solution, replaced with nitrogen to ensure that there is no CO in the system, heated at 120°C for 4h, and carried out NMR 13 C NMR analysis, trans-[Rh(CO) 2 I 4 ] - Completely disappear, all generate positive monovalent cis-[Rh(CO) 2 I 2 ] - , δ184.2, J Rh-CO = 72Hz.

Embodiment 2

[0040] RhI 3 solid added to 13 [Ru( 13 CO) 3 I 3 ] - In the solution, wherein the mass content of rhodium is 2000ppm, the water content in the system is 4%, and lithium iodide is added, and the mass content of lithium is about 3360×10 -6 , the rest is acetic acid solution, replaced with nitrogen to ensure that there is no 13 CO, heated at 120°C for 4h, and carried out NMR 13 C NMR analysis, only the cis-[Rh( 13 CO) 2 I 2 ] - Generation, δ183.5, J Rh-CO = 72Hz.

Embodiment 3

[0042] The trans-[Rh(CO) of the positive trivalent rhodium mass content of the prepared 1250ppm 2 I 4 ] - Mo(CO) added to a Mo mass content of 5000ppm 6 , the water content in the system is 4%, adding lithium iodide, the mass content of lithium is about 3360×10 -6 , the rest is acetic acid solution, replaced with nitrogen to ensure that there is no CO in the system, heated at 120°C for 4h, and carried out NMR 13 C NMR analysis, trans-[Rh(CO) 2 I 4 ] - Completely disappear, all generate positive monovalent cis-[Rh(CO) 2 I 2 ] - , δ184.0, J Rh-CO = 72Hz.

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Abstract

The invention relates to a method for maintaining or generating a positive-monovalent rhodium catalyst active center. The method mainly solves the problem of low carbonylation reaction activity since the rhodium catalyst can not maintain the active center [Rh(CO)2I2]<-> under the conditions of low water and low CO partial pressure in the prior art. According to the method for maintaining or generating the positive-monovalent rhodium catalyst active center, a carbonyl donor is added, so that the rhodium catalyst maintains the high-concentration active center [Rh(CO)2I2]<-> in a carboxylic acid solution under the conditions of low water and low CO partial pressure, wherein the carbonyl donor is at least one of metal carbonyl complexes and organic amide compounds. The technical scheme well solves the problem, and can be used for maintaining or generating the positive-monovalent rhodium catalyst active center.

Description

technical field [0001] The invention relates to a method for maintaining or generating positive monovalent rhodium catalyst active centers. Background technique [0002] Carbonylation catalysts can directly react alcohols, esters and CO to synthesize basic chemicals such as carboxylic acids and acid anhydrides at a certain temperature and pressure. For example, carbonylation reaction catalysts can be used in carbonylation reactions such as methanol carbonylation to acetic acid, methyl acetate carbonylation to acetic anhydride, and ethanol carbonylation to propionic acid. [0003] The continuous production of acetic acid by the carbonylation reaction of methanol or methyl acetate with carbon monoxide is the most important method for producing acetic acid in the prior art, and the active center of the catalyst is positive monovalent [Rh(CO) 2 I 2 ] - . Patent EP0055618A1 has reported that the rhodium catalyst can promote the reaction under the action of organic iodine such...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/20C07C51/56C07C53/12
CPCB01J31/20B01J2531/0213B01J2531/822C07C51/56C07C53/12
Inventor 赖春波高山林李媛王苏陈毅立
Owner SHANGHAI HUAYI GRP CO
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