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Method for preparing 2, 6-naphthalene dicarboxylic acid by oxidizing 2, 6-diisopropylnaphthalene

A technology of diisopropylnaphthalene and naphthalene dicarboxylic acid, applied in chemical instruments and methods, preparation of organic compounds, catalytic reactions, etc., can solve the problem of low purity of 2,6-NDA and low yield of 2,6-NDA problem, to achieve the effect of reducing difficulty and good technical effect

Pending Publication Date: 2021-04-13
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
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  • Application Information

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Problems solved by technology

[0003] The present invention mainly solves the problems of low 2,6-NDA yield and low 2,6-NDA purity when 2,6-diisopropylnaphthalene is oxidized to prepare 2,6-naphthalene dicarboxylic acid, and provides a 2,6- A method for preparing 2,6-naphthalene dicarboxylic acid by oxidation of diisopropylnaphthalene, the method has the advantages of high 2,6-NDA yield and high 2,6-NDA purity

Method used

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  • Method for preparing 2, 6-naphthalene dicarboxylic acid by oxidizing 2, 6-diisopropylnaphthalene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 124.5gCo(OAc) 2 4H 2 O, 122.5gMn(OAc) 2 4H 2 O, 119gKBr, 147.2gCH 3 COOK, 2g of 2,6-naphthalene dicarboxylic acid and 5000g of acetic acid were mixed and added into the reactor, then the stirring was started and the temperature was raised to 200°C, the pressure of the reactor was controlled at 2.75MPa, and 1000g of 2,6-diisopropylnaphthalene was heated to Molten state, enters in the reaction kettle with the speed of 8g / min then, feeds the air of 80L / min simultaneously to react, after feeding finishes, feeds air under the maintenance reaction temperature and pressure to continue reaction 1h, after reaction finishes, will contain The reaction product mixture of crude 2,6-naphthalene dicarboxylic acid was vacuum filtered, and washed with acetic acid at 60°C and water at 80°C respectively. The amount of acetic acid for washing was 1000g, and the amount of washing water was 1000g. After sampling and drying, analyze the obtained 2, The purity and yield of 6-naphthalene di...

Embodiment 2

[0031] 166.05gCo(OAc) 2 4H 2 O, 81.7gMn(OAc) 2 4H 2 O, 119gKBr, 147.2gCH 3 COOK, 2g of 2,6-naphthalene dicarboxylic acid and 5000g of acetic acid were mixed and added into the reactor, then the stirring was started and the temperature was raised to 200°C, the pressure of the reactor was controlled at 2.75MPa, and 1000g of 2,6-diisopropylnaphthalene was heated to Molten state, enters in the reactor with the rate of 8g / min then, feeds the air of 80L / min simultaneously and reacts, and after feeding finishes, maintains reaction temperature and pressure and continues reaction 1h, and after reaction finishes, will contain crude 2,6 -The reaction product mixture of naphthalene dicarboxylic acid was vacuum filtered, and washed with acetic acid at 60°C and water at 80°C respectively. The amount of acetic acid for washing was 1000g, and the amount of washing water was 1000g. The obtained 2,6-naphthalene dicarboxylic acid was analyzed after sampling and drying. The purity of formic a...

Embodiment 3

[0034] 83.03gCo(OAc) 2 4H 2 O, 163.4gMn(OAc) 2 4H 2 O, 119gKBr, 147.2gCH 3 COOK, 2g of 2,6-naphthalene dicarboxylic acid and 5000g of acetic acid were mixed and added into the reactor, then the stirring was started and the temperature was raised to 200°C, the pressure of the reactor was controlled at 2.75MPa, and 1000g of 2,6-diisopropylnaphthalene was heated to Molten state, enters in the reactor with the rate of 8g / min then, feeds the air of 80L / min simultaneously and reacts, and after feeding finishes, maintains reaction temperature and pressure and continues reaction 1h, and after reaction finishes, will contain crude 2,6 -The reaction product mixture of naphthalene dicarboxylic acid was vacuum filtered, and washed with acetic acid at 60°C and water at 80°C respectively. The amount of acetic acid for washing was 1000g, and the amount of washing water was 1000g. The obtained 2,6-naphthalene dicarboxylic acid was analyzed after sampling and drying. The purity of formic a...

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Abstract

The invention relates to a method for preparing 2, 6-naphthalene dicarboxylic acid by oxidizing 2, 6-diisopropylnaphthalene, and mainly solves the problems of low 2, 6-NDA yield and low 2, 6-NDA purity in the process of preparing 2, 6-naphthalene dicarboxylic acid by oxidizing 2, 6-diisopropylnaphthalene. The method for preparing 2, 6-naphthalene dicarboxylic acid by oxidizing 2, 6-diisopropylnaphthalene comprises the following steps of: (1) adding a catalyst, a solvent and 2, 6-naphthalene dicarboxylic acid into a reactor, and controlling the temperature in the reaction kettle to be 160-220 DEG C and the reaction pressure to be 2-3 MPa; (2) adding 2, 6-diisopropylnaphthalene into the reaction kettle, and simultaneously introducing gas containing free oxygen for reaction; and (3) after the 2, 6-diisopropylnaphthalene is fed, continuing reaction for 0.5-2 h to obtain a product 2, 6-naphthalene dicarboxylic acid mixture. The catalyst in the step (1) contains Co, Mn, Br and K. According to the technical scheme, the problems are better solved.

Description

technical field [0001] The invention relates to a method for preparing 2,6-naphthalene dicarboxylic acid by oxidation of 2,6-diisopropylnaphthalene, in particular to a method for preparing 2,6-naphthalene dicarboxylic acid by air oxidation of 2,6-diisopropylnaphthalene. Background technique [0002] 2,6-Naphthalene dicarboxylic acid (2,6-NDA) and its derivatives are important monomers for the preparation of various polyesters, polyurethane materials and liquid crystal polymers (LCP), especially 2,6-NDA and ethylene dicarboxylate Polyethylene naphthalate (PEN) prepared by alcohol polycondensation has broad application prospects in films, packaging containers (especially beer bottles) and industrial fibers. Due to the high symmetry in the structure of 2,6-NDA. It makes PEN have the characteristics of linear polymer, and it is a high-performance material with good rigidity, high strength and excellent thermal processing performance. Compared with polyethylene terephthalate (P...

Claims

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Application Information

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IPC IPC(8): C07C51/265C07C63/38B01J31/32
CPCC07C51/265B01J31/32B01J2231/70C07C63/38
Inventor 朱庆才畅延青肖忠斌
Owner CHINA PETROLEUM & CHEM CORP
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