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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  • 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 p

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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Example Embodiment

[0038] Example 1

[0039] Add 437 mg of rhodium iodide (rhodium content 20wt%) to a 200ml zirconium autoclave equipped with a pressure gauge, and add triphenylphosphine oxide and ruthenium acetate precursor to make the molar ratio of rhodium catalyst: triphenylphosphine oxide: ruthenium It is 1:5:2, 15g methyl iodide, 7.5g distilled water, 25g methyl acetate, 7.5g lithium iodide, and the rest is acetic acid solvent. The total weight is 125g. Keep reaction temperature 190℃, reaction pressure 30bar, 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. After the reaction, the content of propionic acid is determined to be 200 ppm. After the reaction, the reaction solution was continuously heated for 12 hours under simulated flash evaporation conditions, and the rhodium catalyst precipitation rate was 10%.

Example Embodiment

[0040] Example 2

[0041] Add 624mg of rhodium iodide (rhodium content 20wt%) to a 200ml zirconium autoclave equipped with a pressure gauge, and add triphenylphosphine oxide and ruthenium acetate precursor to make the molar ratio of rhodium catalyst: triphenylphosphine oxide: ruthenium It is 1:5:2, 15g methyl iodide, 7.5g distilled water, 25g methyl acetate, 7.5g lithium iodide, and the rest is acetic acid solvent. The total weight is 125g. Keep reaction temperature 190℃, reaction pressure 30bar, 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. After the reaction, the content of propionic acid is determined to be 205 ppm. After the reaction, the reaction solution was continuously heated for 12 hours under simulated flash evaporation conditions, and the rhodium catalyst precipitation rate was 12%.

Example Embodiment

[0042] Example 3

[0043] Add 437mg rhodium iodide (rhodium content 20wt%) to a 200ml zirconium autoclave equipped with a pressure gauge, add lithium dibutylphosphonate and iridium acetate precursor, so that the rhodium catalyst: lithium dibutylphosphonate: iridium The molar ratio is 1:5:2, 15g methyl iodide, 7.5g distilled water, 25g methyl acetate, 7.5g lithium iodide, the rest is acetic acid solvent, the total weight is 125g, the reaction temperature is 190℃, and the reaction pressure is 30bar. The average STY is 8.5 mol / lh, and the STY at 3% ester concentration and 1.7% water content is 7.1 mol / lh. After the reaction, the content of propionic acid is determined to be 200 ppm. After the reaction, the reaction solution was continuously heated for 12 hours under simulated flash evaporation conditions, and the rhodium catalyst precipitation rate 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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