Process for producing 2,6-naphthalenedicarboxylic acid

A technology of naphthalene dicarboxylic acid and aliphatic carboxylic acid, applied in the field of compound preparation, can solve problems such as failure to achieve, and achieve the effects of reducing consumption, reducing production, and avoiding transitional oxidation

Inactive Publication Date: 2008-08-20
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The commercial value of 2,6-NDCA has become more and more obvious since 1950, and various companies are devoting themselves to the research and development of industrialized production routes of 2,6-NDCA, but due to economic and technical reasons, it has not been realized so far. 2, The large-scale production of 6-NDCA, so it is of great significance to research and develop a more economically feasible 2,6-NDCA synthesis technology in industry
[0003] At present, the domestic development work on the liquid-phase oxidation of alkylnaphthalene to 2,6-naphthalene dicarboxylic acid is basically in a blank state, and there are only some review reports

Method used

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  • Process for producing 2,6-naphthalenedicarboxylic acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 150g glacial acetic acid ((Co+Mn) / solvent is 0.016), 4.98g cobalt acetate tetrahydrate, 4.91g manganese acetate tetrahydrate (Co / Mn molar ratio is 1), 7.14g potassium bromide (Br / Co molar ratio For 3), 5.90g of potassium acetate (cocatalyst / (Co+Mn) molar ratio is 3) is added in the titanium reactor (the molar ratio of the solvent to the whole system material is 0.85), first use N 2 After exhausting the air in the kettle, pressurize to 2.4MPa, stir and heat to 200°C at the same time, and the pressure is 3.0MPa. Increase stirring speed to 800r / min, continuously supply compressed air with 3.0Nl / min, 2,6-diisopropylnaphthalene 44.67g ((Co+Mn) / 2,6-DIPN molar ratio is 0.19) in 4 hours Continuously feed in, continue to oxidize for 1 hour after the end of feeding to stop the reaction (the molar ratio of the total amount of oxygen introduced to 2,6-diisopropylnaphthalene is 40). After cooling and pressure relief, the reaction liquid was released, subjected to solid-liquid separ...

Embodiment 2

[0026] With 112.5g glacial acetic acid ((Co+Mn) / solvent molar ratio is 0.022), 37.5g propionic acid (glacial acetic acid: propionic acid weight ratio is 3), 6.73g cobalt acetate tetrahydrate, 6.62g manganese acetate tetrahydrate, 6.43 g potassium bromide (Br / Co molar ratio is 2), 5.30g potassium acetate (co-catalyst / (Co+Mn) molar ratio is 2) is added in the titanium material reactor (the molar ratio of the solvent to the whole system material is 0.86) , use N first 2 After exhausting the air in the kettle, pressurize to 2.4MPa, stir and heat to 200°C at the same time, and the pressure is 3.0MPa. Increase the stirring speed to 900r / min, continuously supply compressed air at 4.0Nl / min, and continuously supply 40.17g of 2,6-diisopropylnaphthalene dissolved in chlorobenzene within four hours, and continue to oxidize for one hour after the supply is completed. Reaction (the molar ratio of the total oxygen feed to 2,6-diisopropylnaphthalene is 53.3). After cooling and pressure rel...

Embodiment 3

[0030] Add 150g of glacial acetic acid ((Co+Mn) / solvent molar ratio is 0.022), 6.73g of cobalt acetate tetrahydrate, 6.62g of manganese acetate tetrahydrate, 6.43g of potassium bromide, and 5.30g of potassium acetate into the titanium reactor. use N 2 After exhausting the air in the kettle, pressurize to 2.4MPa, stir and heat to 200°C at the same time, and the pressure is 3.0MPa. Increase stirring speed to 900r / min, continuously supply the compressed air that is mixed with 20% (volume) carbon dioxide with 3.0Nl / min, 2,6-diisopropyl naphthalene 40.34g is continuously supplied in four hours, continue after supplying Oxidation for one hour stopped the reaction. After cooling and depressurization, the reaction liquid was released and subjected to solid-liquid separation, washed with glacial acetic acid and hot distilled water, and dried to obtain 35.07 g of earthy white solid powder. The purity and yield of 2,6-naphthalene dicarboxylic acid were analyzed to be 96.9%, respectively...

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Abstract

The invention discloses a method for preparing 2, 6-naphthalene formic acid, which comprises a method for oxidizing 2, 6-diisopropyl naphthalene in liquid phase by using gas with oxygen in stirring and bubbling reactor, and using alkali metal compound or nickel compound as cocatalyst and using lower category aliphatic carboxyl acid under the condition with the existence of catalyst with cobalt compound, manganese compound and bromine compound. The method for preparing the 2, 6-naphthalene formic acid has the advantages of reducing the consumption of lower category aliphatic carboxyl acid, preparing the 2, 6-naphthalene formic acid product with high quality, and satisfying the need for producing naphthalene formic acid glycol ester with high quality.

Description

technical field [0001] The present invention relates to a preparation process of a compound, specifically, it involves the oxidation of an oxygen-containing gas through a Co-Mn-Br series catalyst to prepare the target product 2,6-naphthalene dicarboxylic acid, which is realized by using a stirred bubbling reactor an oxidation reaction. Background technique [0002] 2,6-Naphthalene dicarboxylic acid is an important monomer for the preparation of various polyesters, polyurethane materials and liquid crystal polymers, and is also widely used in the fields of dyes and medicine. Due to the high symmetry in the structure of 2,6-naphthalene dicarboxylic acid, polyethylene 2,6-naphthalene dicarboxylate (PEN) obtained by reacting with ethylene glycol has the characteristics of a linear polymer and is a kind of rigid , high-performance materials with high strength and excellent thermal processing performance. Compared with polyethylene terephthalate (PET), PEN has superior heat resi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/265C07C63/38
Inventor 靳海波杨春育韩占生李达仁吴志强
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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