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Method for preparing acetic acid through carbonylation reaction

A technology of carbonylation reaction and acetic acid, applied in carbon monoxide reaction to prepare carboxylic acid, chemical instruments and methods, organic chemistry, etc., can solve problems such as adverse effects of reaction equipment materials, and achieve the effect of increasing the rate of carbonylation reaction

Active Publication Date: 2015-06-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Accelerators can increase the carbonylation reaction rate of the iridium catalyst system, but at the same time may have a potential adverse effect on the material of the reaction equipment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Will contain 60g of acetic acid, 12g of methyl iodide, 45g of methyl acetate, 7.5g of water, Ru(CO) 4 I 2 1.05g (equivalent to 1500ppm Ru content), CeO 2 The mixture of 0.18g (equivalent to Ce content is 1000ppm) is added in the 300ml zirconium material autoclave, and acetic acid 18g, water 3.6g and H 2 IrCl 6 0.72g (equivalent to 2000ppm Ir content) was added to the liquid injection system. After pressure test and slow air replacement, 0.6MPa of CO is introduced, heated to 190°C under stirring at 750 rpm, and then CO is introduced to about 2.5MPa and stabilized for 30 minutes, and the liquid is injected into the system with 3.0MPa of carbon monoxide gas The catalyst solution was added to the autoclave and the reaction started. Containing 20 wt% MeOAc and 6.26 wt% H in the corresponding liquid reaction mixture 2 At O, the carbonylation reaction rate was measured to be 34.2mol / (L·hr); in the corresponding liquid reaction mixture containing 15wt% MeOAc and 5.05wt%...

Embodiment 2

[0037] Will contain 60g of acetic acid, 12g of methyl iodide, 45g of methyl acetate, 7.5g of water, Ru(CO) 4 I 2 2.10g (equivalent to 3000ppm Ru content), CeO 2 The mixture of 0.36g (equivalent to Ce content is 2000ppm) is added in the 300ml zirconium material autoclave, and acetic acid 18g, water 3.6g and H 2 IrCl 6 0.72g (equivalent to 2000ppm Ir content) was added to the liquid injection system. After pressure test and slow air replacement, 0.6MPa of CO is introduced, heated to 190°C under stirring at 750 rpm, and then CO is introduced to about 2.5MPa and stabilized for 30 minutes, and the liquid is injected into the system with 3.0MPa of carbon monoxide gas The catalyst solution was added to the autoclave and the reaction started. Containing 20 wt% MeOAc and 6.26 wt% H in the corresponding liquid reaction mixture 2 At O, the carbonylation reaction rate was measured to be 38.7mol / (L·hr); in the corresponding liquid reaction mixture containing 15wt% MeOAc and 5.05wt%...

Embodiment 3

[0039] Carry out catalysis methyl acetate to prepare acetic acid according to the method for embodiment 1, difference is to use CeO 2 0.09g (equivalent to Ce content of 500ppm), Sm 2 o 3 0.08g (equivalent to Sm content of 500ppm) instead of 0.18g CeO 2. Containing 20 wt% MeOAc and 6.26 wt% H in the corresponding liquid reaction mixture 2 At O, the carbonylation reaction rate was measured to be 35.6mol / (L·hr); in the corresponding liquid reaction mixture containing 15wt% MeOAc and 5.05wt% H 2 O, the measured carbonylation reaction rate was 26.2mol / (L·hr); in the corresponding liquid reaction mixture containing 10wt% MeOAc and 3.87wt% H 2 At 0, the measured carbonylation reaction rate was 14.7 mol / (L·hr). The liquid sample after the reaction was taken for testing, and the selectivity of acetic acid in the product was 99.9%. Visual inspection of the reaction tube revealed no precipitation.

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Abstract

The invention provides a method for preparing acetic acid through a carbonylation reaction. Under the existences of water, an iridium catalyst system, and an organic solvent, methanol and / or methyl acetate contact carbon monoxide. The iridium catalyst system comprises an iridium-containing compound, a halogen cocatalyst, an accelerant containing ruthenium and / or osmium, and a rare earth oxide. With the method provided by the invention for preparing acetic acid through a carbonylation reaction, the adopted iridium catalyst system comprises the rare earth oxide, such that carbonylation reaction speed can be increased. When the content of carbon monoxide is low, no precipitate is formed in a liquid reaction mixture. Therefore, when the liquid reaction mixture is subjected to flash evaporation and acetic acid is separated, the mixture can be utilized as a catalyst system again.

Description

technical field [0001] The invention relates to a method for preparing acetic acid by carbonylation reaction. Background technique [0002] As an important basic organic chemical raw material, acetic acid is widely used in various fields such as fibers, plasticizers, paints, adhesives, and copolymer resins. It is a chemical product with a rapid increase in production capacity in recent years. At present, the main methods of producing acetic acid in the world are acetaldehyde oxidation, butane and light oil oxidation and methanol carbonylation. Among them, the production of acetic acid by methanol carbonylation has accounted for more than 70% of the world's acetic acid production. [0003] The production of acetic acid by catalyzing the carbonylation of methanol with an iridium catalyst system is known and has been applied in industrial production. As early as the development of rhodium-based carbonylation catalysts by Monsanto, research on iridium-based carbonylation catal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/08C07C51/12B01J31/28B01J23/63B01J23/96
CPCY02P20/584
Inventor 刘博吕顺丰王世亮李彤秦燕璜
Owner CHINA PETROLEUM & CHEM CORP