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Preparation method of 1, 4-naphthalene dicarboxylic acid

A technology of naphthalene dicarboxylic acid and naphthalene ethyl ketone, applied in the field of preparation of 1,4-naphthalene dicarboxylic acid, achieving good economic benefits, easy operation, and simple preparation steps

Pending Publication Date: 2020-10-09
黄石市利福达医药化工有限公司
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  • Abstract
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  • Claims
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Problems solved by technology

The method provided by the invention uses 1-methyl-4-naphthyl ethyl ketone as a starting material to directly prepare 1,4-naphthalene dicarboxylic acid through oxygen oxidation, which solves the problem of raw material supply, and 1-methyl-4 - The price of naphthalene ethyl ketone is lower than that of 1-methyl-4-naphthoic acid, and the economic benefit is better

Method used

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  • Preparation method of 1, 4-naphthalene dicarboxylic acid

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[0018] The invention provides a preparation method of 1,4-naphthalenedicarboxylic acid, comprising the following steps:

[0019] Mix 1-methyl-4-naphthalene ethyl ketone, a solvent and a catalyst, and feed oxygen into the obtained mixed solution to make 1-methyl-4-naphthalene ethyl ketone undergo an oxidation reaction to obtain 1,4-naphthalenedicarboxylic acid .

[0020] In the present invention, the catalyst includes cobalt acetate, manganese acetate and potassium bromide, and the present invention simultaneously uses the above three substances as catalysts, which can catalyze the oxidation reaction to proceed smoothly.

[0021] In the present invention, the solvent is glacial acetic acid; the mass ratio of the 1-methyl-4-naphthoethyl ketone, cobalt acetate, manganese acetate, potassium bromide, glacial acetic acid and oxygen is preferably 100:(3~5 ):(3-5):(3-5):(1400-1600):(80-100), more preferably 100:4:4:4:1500:90.

[0022] In the present invention, the introduction rate ...

Embodiment 1

[0037] Drop into 100kg 1-methyl-4-naphthalene ethyl ketone, 4kg cobalt acetate, 4kg manganese acetate, 4kg potassium bromide, 1500kg glacial acetic acid in the glass-lined reactor of 2000L band condenser, oxygen supply pipe and tail gas absorption device, start Stir and heat up to 100 ° C, feed 90 kg of oxygen at a constant speed, stop the oxygen when the 1-methyl-4-naphthoethyl ketone is controlled to be less than 0.5% in the sampling, cool down to 30 ° C, and spin dry to obtain a crude wet weight of 150 kg to be refined; Into the reactor, measure the water content and add acetic anhydride according to the water content in the mother liquor, if the mother liquor is not enough, add glacial acetic acid to 1500L, add 0.2kg cobalt acetate, 0.2kg manganese acetate, 0.2kg potassium bromide, 100kg 1 -Methyl-4-naphthoethyl ketone, then operate with the batch reaction.

[0038] Add 150kg of the above-mentioned crude product and 2000L of water to the 3000L glass-lined reactor, heat up ...

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Abstract

The invention belongs to the technical field of organic synthesis and provides a preparation method of 1, 4-naphthalene dicarboxylic acid. According to the preparation method of the invention, with the 1-methyl-4-acetonaphthone adopted as an initial raw material, oxygen oxidation is directly performed to prepare the 1, 4-naphthalene dicarboxylic acid. The preparation method is simple in preparation steps and is easy in operation. With the preparation method adopted, the problem of raw material supply is solved; the price of 1-methyl-4-naphthalene dicarboxylic acid is 50,000 yuan lower than that of 1-methyl-4-naphthoic acid per ton; the total cost of the 1, 4-naphthalene dicarboxylic acid can be reduced by 40,000 yuan, and therefore, the preparation method has good economic benefits.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of 1,4-naphthalene dicarboxylic acid. Background technique [0002] 1,4-Naphthalenedicarboxylic acid has a wide range of applications in chemical production. Specifically, it can be used as an intermediate for dyes and plastic processing aids, or for the production of fluorescent whitening agents and dye intermediates. [0003] In the prior art, 1-methyl-4-naphthoic acid is used as starting material to prepare 1,4-naphthalene dicarboxylic acid, and 1-methyl-4-naphthoic acid is prepared from 1-methyl-4-naphthoethyl ketone It is obtained by reacting with sodium hypochlorite. During the reaction process, chloroform will be produced as a by-product, and a large amount of salt-containing wastewater will be produced. higher, and it is difficult to buy 1-methyl-4-naphthoic acid in the market, which directly affects the market demand of 1,4-naphthalenedica...

Claims

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Application Information

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