Preparation method of 1,4-naphthalenedicarboxylic acid

A technology of naphthalene dicarboxylic acid and naphthoic acid, which is applied in the direction of carboxylate preparation, organic compound preparation, chemical instruments and methods, etc., can solve the problems of expensive raw materials, large energy consumption, environmental pollution, etc., and achieve abundant resources, Effects of reducing discards and reducing costs

Active Publication Date: 2014-04-23
黄石市利福达医药化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing 1,4-naphthalene dicarboxylic acid preparation process is that 1-methyl-4-naphthoic acid is produced in alkaline aqueous solution through potassium permanganate, and the unit consumption of potassium permanganate in the preparation process is 2.37 ( T / T), the cost is 2.37T×16,000 yuan / T=37,920 yuan, the price of raw materials is expensive, and the amount of solid waste manganese dioxide produced by the existing process is relatively large, and it is difficult to dispose of a large amount of manganese mud solid waste, and A large amount of waste water is produced, which consumes a lot of energy and pollutes the environment seriously. It cannot meet the growing environmental protection requirements and does not meet the principles of energy saving, emission reduction and clean production.

Method used

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  • Preparation method of 1,4-naphthalenedicarboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The 1-methyl-4-naphthoic acid that 200kg concentration is 98% is dissolved in 300kg glacial acetic acid, and in mixed solution, add the cobalt acetate that mass ratio is 1:50, the manganese acetate that mass ratio is 1:50, mass ratio 1:50 sodium acetate, the amount of cobalt acetate, manganese acetate, and sodium acetate is based on the mass of 1-methyl-4-naphthoic acid, then start to heat up to 70°C until the materials are completely dissolved, and evenly introduce air , Sampling and analysis in the middle, the content of 1-methyl-4-naphthoic acid is less than 0.5% is the reaction end point, and the crude product of 1,4-naphthalene dicarboxylic acid with a content of more than 96% is obtained by cooling and filtration. Add acetic anhydride to the mother liquor to remove water, then add new 1-methyl-4-naphthoic acid according to the normal batch reaction (the amount added is the same as the batch), then add cobalt acetate, manganese acetate, acetic acid Sodium reaction,...

Embodiment 2

[0019] The 1-methyl-4-naphthoic acid that 100kg concentration is 98% is dissolved in the glacial acetic acid of 1500kg, in the mixed liquor, add the cobalt acetate that mass ratio is 1:40, the manganese acetate that mass ratio is 1:40, the mass ratio 1:40 sodium acetate, the amount of cobalt acetate, manganese acetate, and sodium acetate is based on the quality of 1-methyl-4-naphthoic acid, then start to heat up to 90 ° C until the materials are completely dissolved, and evenly introduce air , Sampling and analysis in the middle, the content of 1-methyl-4-naphthoic acid is less than 0.5% is the reaction end point, and the crude product of 1,4-naphthalene dicarboxylic acid with a content of more than 96% is obtained by cooling and filtration. Add acetic anhydride to the mother liquor to remove water, then add new 1-methyl-4-naphthoic acid according to the normal batch reaction (the amount added is the same as the batch), then add cobalt acetate, manganese acetate, acetic acid S...

Embodiment 3

[0021] The 1-methyl-4-naphthoic acid that 300kg concentration is 98% is dissolved in 4500kg glacial acetic acid, add the cobalt acetate that mass ratio is 1:30, the manganese acetate that mass ratio is 1:30, mass ratio 1:30 sodium acetate, the amount of cobalt acetate, manganese acetate, and sodium acetate is based on the quality of 1-methyl-4-naphthoic acid. Start to heat up to 78°C until the materials are completely dissolved, and then evenly pass in Air, midway sampling and analysis, 1-methyl-4-naphthoic acid content less than 0.5% is the reaction end point, cooling and filtering to obtain 1,4-naphthalene dicarboxylic acid crude product with content greater than 96%. Add acetic anhydride to the mother liquor to remove water, then add new 1-methyl-4-naphthoic acid according to the normal batch reaction (the amount added is the same as the batch), then add cobalt acetate, manganese acetate, acetic acid Sodium reaction, the amount added is 5% of the batch feed amount; 1,4-naph...

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Abstract

The invention discloses a preparation method of 1,4-naphthalenedicarboxylic acid. The preparation method comprises the following steps of dissolving 1-methyl-4-naphthoic acid into glacial acetic acid, adding cobalt acetate, manganese acetate and sodium acetate in a mass ratio of 1: 50 to the mixed liquor, heating to 90 DEG C until all the materials are dissolved, then adding a catalyst, heating to 130 DEG C, uniformly pumping air, and cooling and filtering to obtain a crude product of 1,4-naphthalenedicarboxylic acid; adding acetic anhydride and replenishing the catalyst to the mother liquor to react again with 1-methyl-4-naphthoic acid; dissolving the crude product of 1,4-naphthalenedicarboxylic acid into water, adding caustic soda flakes, heating to 70-90 DEG C, regulating the PH value to 7-8, adding activated carbon, after stirring and suction filtration, heating to 70-90 DEG C, regulating the PH value below 2, cooling to 20-30 DEG C to carry out centrifugal separation, washing the solid material until the solid material is neutral, and drying the material, thus obtaining a finished product. The preparation method adopts air and oxygen for oxidation, is abundant in resources and low in production cost, is free from waste residues, and is environment-friendly and energy-saving.

Description

[0001] technical field [0002] The present invention relates to a preparation method of 1,4-naphthalene dicarboxylic acid, in particular to a 1,4-naphthalene dicarboxylate that reduces the cost of raw materials, reduces the generation of "three wastes" in the preparation process, and has good environmental protection and energy saving effects Acid preparation method. [0003] Background technique [0004] Fluorescent whitening agent KCB prepared from 1,4-naphthalene dicarboxylic acid is an excellent upgraded product among whitening agents, which has a strong whitening and brightening effect. 1,4-naphthalene dicarboxylic acid is fluorescent whitening agent KCB Intermediates can also be used as liquid crystal raw materials. The existing 1,4-naphthalene dicarboxylic acid preparation process is that 1-methyl-4-naphthoic acid is produced in alkaline aqueous solution through potassium permanganate, and the unit consumption of potassium permanganate in the preparation process is...

Claims

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Application Information

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IPC IPC(8): C07C63/38C07C51/265
CPCC07C51/265C07C63/38
Inventor 成家钢方日青柯美街
Owner 黄石市利福达医药化工有限公司
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