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Aromatic polycarboxylic acid manufacturing method

A technology of polycarboxylic acid and manufacturing method, applied in the direction of carboxylate preparation, organic chemical method, chemical instrument and method, etc., can solve the problems such as difficult to obtain high yield and obtain target compound, so as to improve selectivity and reduce residue Quantitative and efficient manufacturing effects

Inactive Publication Date: 2011-05-18
DAICEL CHEM IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, a large amount of methyltricarboxybenzene, which is an intermediate product of the oxidation reaction, remains, so it is difficult to obtain the target compound, pyromellitic acid, in high yield.

Method used

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  • Aromatic polycarboxylic acid manufacturing method
  • Aromatic polycarboxylic acid manufacturing method
  • Aromatic polycarboxylic acid manufacturing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0122] Embodiment 1 (reaction temperature 80 ℃ → 120 ℃ → 130 ℃)

[0123] Add 40 g (0.30 mol) of durene, 320 g of acetic acid, 0.19 g (0.7 mmol) of cobalt acetate (2 valence), 0.55 g (2.2 mmol) of manganese acetate (2 valence), zirconium sulfate into the air circulation reactor. 1.06g (3.0 mmol), the pressure was raised to 0.8MPa with nitrogen, and heated to 80°C.

[0124] Add 14.8 g (60 mmol) of N, N'-dihydroxypyromellitic acid diimide to 300 g of acetic acid to obtain a slurry, and start supplying the slurry and the gas obtained by mixing air and nitrogen into the reactor to trigger a reaction. The above-mentioned slurry was fed into the reactor by using a slurry pump for 5 hours, and the gas supply was adjusted so that the oxygen concentration in the outlet gas was 2-8%. After the reaction started, the reaction temperature was raised to 120° C. over 0.5 hour, and the above state was maintained for 1.5 hours. Here, samples were taken for HPLC analysis, and then the reactio...

reference example 1

[0127] Reference example 1 (reaction temperature 130°C → 160°C)

[0128] Add 40 g (0.30 mol) of durene, 320 g of acetic acid, 0.19 g (0.7 mmol) of cobalt acetate (2 valence), 0.55 g (2.2 mmol) of manganese acetate (2 valence), zirconium sulfate into the air circulation reactor. 1.06g (3.0mmol), the pressure was raised to 0.8MPa with nitrogen, and heated to 130°C.

[0129] Add 14.8 g (60 mmol) of N, N'-dihydroxypyromellitic acid diimide to 300 g of acetic acid to obtain a slurry, and start supplying the slurry and the gas obtained by mixing air and nitrogen into the reactor to trigger a reaction. The above-mentioned slurry was fed into the reactor using a slurry pump for 5 hours, and the gas supply was adjusted so that the oxygen concentration in the off-gas was 2 to 8%. After the reaction started, the reaction temperature was raised to 160° C. over 0.5 hour, and the above state was maintained for 4.5 hours. During the reaction, the gas and catalyst supply are adjusted as ne...

Embodiment 2

[0132] Example 2 (reaction temperature 80°C → 120°C → 130°C, pressure 2MPa)

[0133] Add 40 g (0.30 mol) of durene, 320 g of acetic acid, 0.19 g (0.7 mmol) of cobalt acetate (2 valence), 0.55 g (2.2 mmol) of manganese acetate (2 valence), zirconium sulfate into the air circulation reactor. 1.06g (3.0 mmol), the pressure was raised to 2MPa with nitrogen, and heated to 80°C.

[0134]Add 14.8 g (60 mmol) of N, N'-dihydroxypyromellitic acid diimide to 300 g of acetic acid to obtain a slurry, and start supplying the slurry and the gas obtained by mixing air and nitrogen into the reactor to trigger a reaction. The above-mentioned slurry was fed into the reactor by using a slurry pump for 5 hours, and the gas supply was adjusted so that the oxygen concentration in the outlet gas was 2-8%. After the reaction started, the reaction temperature was raised to 120° C. over 0.5 hour, and the above state was maintained for 1.5 hours. Here, samples were taken for HPLC analysis, and then th...

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Abstract

Disclosed is a method by which the amount of residual intermediate product can be reduced and an aromatic polycarboxylic acid can be manufactured wherein all of the alkyl groups are converted into carboxy groups at a high yield. In the presence of a catalyst having ring-shaped imino units having an N-OR group (R is a hydrogen atom or a protective hydroxy group) and a transition metal co-catalyst (for example, a cobalt compound, manganese compound, or zirconium compound), an aromatic compound that has multiple alkyl groups (durene or the like) is heated in a low temperature range and then a high temperature range to undergo oxygen oxidization, to manufacture an aromatic polycarboxylic acid wherein the multiple alkyl groups are oxidized into carboxy groups. In the initial stage of the reaction, the reaction may be carried out in a first low temperature range with a reaction temperature of 60-120 DEG C and in a second low temperature range (intermediate temperature range) with a reaction temperature of 100-140 DEG C. Then, in the later stage of the reaction, the reaction may be carried out in a high temperature range with a reaction temperature of 110-150 DEG C.

Description

technical field [0001] The present invention relates to a method for producing aromatic polycarboxylic acid. The method utilizes molecular oxygen to catalyze oxidation of aromatic compounds (aromatic compounds, etc.) having multiple alkyl groups, thereby producing aromatic polycarboxylic acid. Background technique [0002] Various methods have been known as methods for producing aromatic polycarboxylic acids by catalytic oxidation of alkylbenzenes with molecular oxygen. For example, U.S. Patent No. 5,041,633 specification (Patent Document 1) discloses the following method: 2-6 Aromatic compounds (durene, etc.) Heating is carried out to produce aromatic polycarboxylic acid. In this method, after reacting at 93-199°C, water is added while raising the temperature to at least 14°C, and reaction is carried out at 176-249°C to produce aromatic polycarboxylic acid. An example of using zirconium as a catalyst is also described in this document. In addition, this document also des...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/265B01J31/02C07C63/307C07C63/313C07C65/34C07B61/00
CPCC07C51/265Y02P20/55C07C63/313C07C65/34C07C63/307
Inventor 芝本明弘岩浜隆裕
Owner DAICEL CHEM IND LTD
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