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Method for producing acetic acid by carbonylation of methanol as well as special catalyst and preparation method thereof

A methanol carbonylation and catalyst technology, which is applied to the preparation of carboxylic acid by carbon monoxide reaction, physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, etc. Selective, highly adaptive effects

Active Publication Date: 2008-05-21
INST OF CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore in industrial production, generally adopt to keep the partial pressure of carbon monoxide or add excessive hydrogen iodide to protect the existence of rhodium (I) complex, but this has greatly increased the corrosive action of reaction medium again to equipment

Method used

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  • Method for producing acetic acid by carbonylation of methanol as well as special catalyst and preparation method thereof
  • Method for producing acetic acid by carbonylation of methanol as well as special catalyst and preparation method thereof
  • Method for producing acetic acid by carbonylation of methanol as well as special catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Embodiment 1, the preparation of catalyst

[0064] Dissolve 0.01 mole of allanine and 0.01 mole of lithium hydroxide in 100ml of methanol, stir at 30°C for 30 minutes at high speed to form a methanol solution of lithium allanate; dissolve 0.005 mole of dirhodium tetracarbonyl dichloride In 50ml of methanol, slowly add the methanol solution of lithium allanylpropionate under stirring, and continue to stir for 40 minutes at 40°C to form a lithium-rhodium aminopropionate complex; dissolve 0.01 mole of potassium iodide in 50ml of methanol, and stir Add it into the above-mentioned complex solution at 40° C. and continue to stir for 30 minutes to obtain the catalyst solution to be prepared, which is designated as catalyst (I).

[0065] Dissolve 0.01 mole of aminobutyric acid and 0.01 mole of lithium hydroxide in 100ml of methanol, stir at 40°C for 40 minutes at high speed to form a methanol solution of lithium aminobutyrate; dissolve 0.005 mole of dirhodium tetracarbonyl dich...

Embodiment 2

[0069] Embodiment 2, catalytic reaction

[0070] The catalyst used is the catalyst (I) prepared in Example 1. The batch test is carried out in a 250ml zirconium autoclave, and different reaction results can be obtained by controlling the composition of different reaction systems. The performance of the catalyst is discussed below through the reaction data in Table 1. The yield of acetic acid refers to the percentage of acetic acid produced from raw material methanol.

[0071] Methanol is the raw material of reaction, and the addition of methyl acetate is mainly in order to regulate the water content of medium in the reaction process, and the higher the addition of methyl acetate, the lower actual water content in the reaction. The remainder of the reaction medium is acetic acid. The content of the rhodium complex catalyst of lithium aminocarboxylate (prepared in Example 1) is calculated by the mass fraction (ppm) of rhodium in the reaction system. The reactor pressure of t...

Embodiment 3

[0075] Embodiment 3, catalytic reaction

[0076] The catalyst used is the catalyst (II) prepared in Example 1. The continuous use performance of the methanol carbonylation catalyst was evaluated using a batch model test device. In this device, the catalytic reaction is carried out in a 250ml reactor. After a period of time, the reaction mother liquid is discharged and enters a glass multistage rectification device. After a certain amount of mother liquid (mainly methyl iodide and acetic acid) is steamed, the remaining Catalyst mother liquid together with a certain amount of methyl iodide enters a stainless steel high-pressure tank, and is pressed into the reactor by high-pressure carbon monoxide gas, and the temperature rises to start a new reaction, and the cycle repeats. The activity of the reaction can be calculated by the absorption rate of carbon monoxide and the amount of acetic acid product in the reaction, the selectivity of the reaction can be calculated by analyzing...

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Abstract

The invention discloses a method for producing acetic acid by carbonylation of methanol, a special catalyst and a preparation method thereof. The aminocarboxylate lithium rhodium complex of the present invention has a structure as shown in formula I, wherein, X=BPh4 or I; n=1, 2 or 3. In the present invention, lithium aminocarboxylate is used as a ligand and a rhodium complex to form a positive ion active center structure of a strong and weak coordination bond chelation type, and the positive ion part contains a strongly coordinated N→Rh bond and a weakly coordinated O→Rh bond, The stability and activity of the active center are guaranteed. Lithium metal and rhodium metal are co-located in the structure of the active center, which can form a synergistic catalytic effect; moreover, it can also be used in combination with other catalysts to improve its catalytic activity; The strong catalytic effect of the reaction provides a basis for the excellent performance of the catalyst; at the same time, the combination of lithium iodide, lithium acetate and phosphate is used as a promoter, so that the catalyst of the present invention can catalyze the carbonylation of methanol to produce acetic acid. Excellent overall performance.

Description

technical field [0001] The invention relates to a method for producing acetic acid by carbonylation of methanol, a special catalyst and a preparation method thereof. Background technique [0002] Acetic acid is an important organic chemical raw material, mainly used in the production of vinyl acetate monomer, acetic anhydride, terephthalic acid (PTA), polyvinyl alcohol, acetate esters, cellulose acetate, etc. It is widely used in chemical industry, light textile, medicine, dyestuff and other industries. In recent years, due to the development of PTA and downstream products of acetic acid, acetic acid has become one of the few petrochemical products whose output and demand are growing rapidly. [0003] In the production technology of methanol carbonylation to produce acetic acid, the research on catalyst is one of the most important contents. The reaction of carbon monoxide with methanol to prepare acetic acid under the action of a catalyst is an oxo synthesis method develo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F19/00C07F15/00C07C53/08C07C51/12B01J31/22B01J31/28
Inventor 袁国卿钱庆利蒋小川闫芳
Owner INST OF CHEM CHINESE ACAD OF SCI
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