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Method for synthesizing 2-methyl-1, 4-naphthoquinone

A synthetic method and technology of methylnaphthalene, applied in the preparation of quinone oxide, organic chemistry, etc., can solve the problems of heavy metal ion pollution, high production cost, low process yield, etc., and achieve improved production efficiency, low cost, and good selectivity Effect

Inactive Publication Date: 2012-06-27
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006]Technical problem: the present invention aims at the disadvantages of low yield, high production cost and serious pollution of heavy metal ions in the traditional process, and provides a synthetic 2-methyl-1,4 - Naphthoquinone method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a 100mL four-necked flask, add 2.5g of 2-methylnaphthalene, 75mL of solvent, and 1.5mL of concentrated sulfuric acid. With stirring, the temperature is raised to 40°C, and 30mL of hydrogen peroxide (H 2 o 2 The volume fraction is 30%), the dropping rate is 1mL / min, after dropping, keep warm for 1.0h. After the reaction was completed, the feed solution was concentrated to 1 / 2 of the original volume, then poured into about 100 mL of ice water and left to stand, a large amount of yellow solids precipitated. Suction filtration and drying to obtain 2-methyl-1,4-naphthoquinone. The yield was 87.4%.

Embodiment 2

[0028] In a 250mL four-necked flask, add 5.0g of 2-methylnaphthalene, 120mL of solvent, and 2.5mL of concentrated sulfuric acid, raise the temperature of the feed solution to 60°C under stirring, and start adding hydrogen peroxide (H 2 o 2 The volume fraction is 30%) 60mL, the dropping rate is 1mL / min, and keep warm for 2.0h after dropping. After the reaction, the feed liquid was concentrated to 1 / 2 of the original volume, then poured into ice water with a volume of about 200 mL, and left to stand, a large amount of yellow solids precipitated. Suction filtration and drying to obtain 2-methyl-1,4-naphthoquinone. The yield was 85.3%.

Embodiment 3

[0030] In a 100mL four-necked flask, add 2.5g of 2-methylnaphthalene, 55mL of solvent, and 0.5mL of concentrated sulfuric acid. With stirring, the temperature is raised to 80°C, and hydrogen peroxide (H 2 o 2 The volume fraction is 30%) 30mL, the dropping rate is 1mL / min, and keep warm for 1.0h after dropping. After the reaction, the feed liquid was concentrated to 1 / 3 of the original volume, then poured into ice water with a volume of about 100 mL, and left to stand, a large amount of yellow solids precipitated. Suction filtration and drying to obtain 2-methyl-1,4-naphthoquinone. The yield was 90.5%.

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Abstract

The invention relates to a method for synthesizing 2-methyl-1, 4-naphthoquinone through taking 2-methylnaphthalene as a raw material, which comprises the following steps of: taking the 2-methylnaphthalene as the raw material, taking glacial acetic acid as a solvent, taking hydrogen peroxide as an oxidizing agent and catalyzing with a catalyst to synthesize the 2-methyl-1, 4-naphthoquinone. The reaction temperature is 20-80 DEG C, and the dripping rate is 0.02-1 mL / min. After the end of dripping, the temperature is preserved for 0.5-4 hours. After the reaction is ended, and feed liquid is concentrated to 1 / 2-1 / 6 of the original volume, the feed liquid is poured into ice water with the volume being 3-6 times that of the feed liquid and is then stewed, filtered and dried to obtain the 2-methyl-1, 4-naphthoquinone. The method has the beneficial effects that a mixed acid catalytic system is used; compared with a traditional chromate oxidation method, the method has the advantages of good selectivity and high yield; and the pollution to a large quantity of chromium metal ions generated in the traditional industrial production can be avoided, and therefore, the industrial application value is higher.

Description

technical field [0001] The invention relates to a method for catalytically synthesizing 2-methyl-1,4-naphthoquinone by using sulfuric acid as a catalyst, wherein 2-methylnaphthalene is used as a reaction raw material, and the oxidizing agent is hydrogen peroxide, which belongs to the field of fine chemical synthesis. Background technique [0002] 2-Methyl-1,4-naphthoquinone (2-Methyl-1,4-naphthoquinone, abbreviated as 2-MNQ) is an important compound for the synthesis of vitamin K 3 And a series of important intermediates of vitamin K. [0003] There are three main methods for producing 2-methyl-1,4-naphthoquinone: gas-phase oxidation, liquid-phase oxidation and electrolytic oxidation. The gas phase oxidation method is prone to deep oxidation due to the high reaction temperature; the electrolytic oxidation method consumes a lot of power and is suitable for small-tonnage industrial production. The liquid phase oxidation method can overcome the shortcomings of both. The meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C50/10C07C46/04
Inventor 肖国民颜廷凤牛磊高李璟
Owner SOUTHEAST UNIV
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