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Method for synthesizing acetic acid through carbonylation

A technology of chemical synthesis and acetic acid, which is applied in the direction of chemical instruments and methods, carbon monoxide reaction to prepare carboxylic acid, organic compound/hydride/coordination complex catalyst, etc., which can solve the problems of increased energy consumption for separation, difficulty in continuous operation, and easy volatility, etc. problems, to achieve the effects of slowing down adverse effects, improving reactivity, and high stability

Active Publication Date: 2012-01-18
SHANGHAI HUAYI GRP CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, under low water conditions, noble metals, iridium and ruthenium are easy to volatilize, and in the presence of corrosive metals, there is a significant inhibitory effect on the reaction rate, and it is also easy to cause the precipitation of iridium catalyst and cocatalyst ruthenium, because the ester concentration in the reaction system is high. less than 8%, resulting in difficulties in continuous operation and increased energy consumption for separation

Method used

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  • Method for synthesizing acetic acid through carbonylation
  • Method for synthesizing acetic acid through carbonylation
  • Method for synthesizing acetic acid through carbonylation

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Add rhodium iodide (rhodium content 20wt%) 437mg in the zirconium material autoclave that pressure gauge is housed in 200ml, add triphenylphosphine oxide and ruthenium acetate precursor, make rhodium catalyst: triphenylphosphine oxide: the mol ratio of ruthenium 1:5:2, methyl iodide 15g, distilled water 7.5g, methyl acetate 25g, lithium iodide 7.5g, the rest is acetic acid solvent, the total weight is 125 grams, keep the reaction temperature 190 ℃, the reaction pressure 30bar, the average reaction The STY is 8.1 mol / lh, and the STY at 3% ester concentration and 1.7% water content is 7.0 mol / lh, and the content of propionic acid is 200ppm after the reaction. After the reaction, the reaction solution was heated continuously for 12 hours under simulated flash evaporation conditions, and the precipitation rate of the rhodium catalyst was 10%.

Embodiment 2

[0041] Add rhodium iodide (rhodium content 20wt%) 624mg in the zirconium material autoclave that pressure gauge is housed in 200ml, add triphenylphosphine oxide and ruthenium acetate precursor, make rhodium catalyst: triphenylphosphine oxide: the mol ratio of ruthenium 1:5:2, methyl iodide 15g, distilled water 7.5g, methyl acetate 25g, lithium iodide 7.5g, the rest is acetic acid solvent, the total weight is 125 grams, keep the reaction temperature 190 ℃, the reaction pressure 30bar, the average reaction The STY is 10.1 mol / lh, and the STY at 3% ester concentration and 1.7% water content is 7.6 mol / lh, and the content of propionic acid is 205ppm after the reaction. The reaction solution after the reaction was heated continuously for 12 hours under simulated flash evaporation conditions, and the precipitation rate of the rhodium catalyst was 12%.

Embodiment 3

[0043] Add rhodium iodide (rhodium content 20wt%) 437mg in the zirconium material autoclave that pressure gauge is housed in 200ml, add dibutyl lithium phosphonate and iridium acetate precursor, make rhodium catalyst: dibutyl lithium phosphonate: iridium The molar ratio is 1:5:2, methyl iodide 15g, distilled water 7.5g, methyl acetate 25g, lithium iodide 7.5g, all the other are acetic acid solvents, total weight is 125 grams, keep reaction temperature 190 ℃, reaction pressure 30bar, reaction The average STY is 8.5mol / lh, and the STY under 3% ester concentration and 1.7% water content is 7.1mol / lh, and the content of propionic acid measured after the reaction is 200ppm. After the reaction, the reaction solution was heated continuously for 12 hours under simulated flash evaporation conditions, and the precipitation rate of the rhodium catalyst was 25%.

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Abstract

The invention discloses a method for synthesizing acetic acid through carbonylation. The acetic acid is synthesized through carbonylation of methanol or derivatives of the methanol which are used as raw materials and a liquid reaction composition, wherein the reaction temperature is between 160 and 210 DEG C and the reaction pressure is 2.0 to 5.0 MPa; and the liquid reaction composition comprises a rhodium catalyst, an iodomethane cocatalyst, methyl acetate, acetic acid, water, alkali metal iodate, and organic hard base and variable valence metal salt which serve as stabilizing agents. Due to the addition of the organic hard base and variable valence metal salt, the rhodium catalyst can keep high stability under the condition of low water content, adverse influence of corroding metal on the stability of the rhodium catalyst can be retarded, the reaction activity under the condition of low water content can be improved, and the content of the byproducts such as propionic acid and unsaturated compounds can be reduced, so that the acetic acid can be produced with low energy consumption.

Description

technical field [0001] The present invention relates to a production method of acetic acid, in particular to a production method of carbonylation to synthesize acetic acid, in particular to a method for producing acetic acid with low energy consumption by adding an organic hard base and a metal salt containing variable valence to maintain the stability of the rhodium catalyst . Background technique [0002] Acetic acid is an environmentally friendly organic acid and an important chemical intermediate and solvent for chemical reactions, from which hundreds of downstream products can be derived, such as vinyl acetate monomer, cellulose acetate, acetic anhydride, acetate, chloroacetic acid, Terephthalic acid, polyvinyl alcohol and metal acetate are widely used in the synthesis of medicine, synthetic fibers, light industry, textiles, leather, pesticides, explosives, rubber and metal processing, food and fine organic chemicals. [0003] The continuous production of acetic acid b...

Claims

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Application Information

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IPC IPC(8): C07C53/08C07C51/12B01J31/26
Inventor 赖春波王苏高山林曾义红宁春利陈浩曹智龙张春雷
Owner SHANGHAI HUAYI GRP CO
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