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Method for preparing 2-methyl-1,4-naphthoquinone through microwave radiation

A technology of microwave radiation and methylnaphthalene, applied in the preparation of quinone oxide, organic chemistry, etc., can solve the problems of producing a large amount of chromium-containing wastewater, high environmental corrosion resistance requirements, and high preparation costs

Inactive Publication Date: 2016-06-15
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main disadvantage of this method: chromium salts are corrosive and require high corrosion resistance to the environment. A large amount of chromium-containing wastewater will be generated during the production process, which will seriously pollute the environment.
However, the price of titanium-silicon molecular sieve TS-1 is high, the cost of preparation is high, and there are certain difficulties in its wide use.
Another example is that Chinese patent document 201410091125.X discloses a new synthesis method of 2-methyl-1,4-naphthoquinone, using m-chloroperbenzoic acid as an oxidant to oxidize 2-methylnaphthalene to prepare 2-methyl-1 , 4-naphthoquinone, avoiding the direct use of hydrogen peroxide as an oxidant, but the yield is low, about 31%

Method used

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  • Method for preparing 2-methyl-1,4-naphthoquinone through microwave radiation
  • Method for preparing 2-methyl-1,4-naphthoquinone through microwave radiation

Examples

Experimental program
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Effect test

Embodiment 1

[0036] Preparation of polystyrene polymer peroxyacid:

[0037]1) Add 100g of dichloromethane and 65g of cross-linked polystyrene into a 1000mL four-necked reaction flask equipped with a reflux condenser, thermometer, and stirrer, stir and swell for 6 hours at room temperature; add 125g of anhydrous aluminum trichloride, dropwise 150g of acetyl chloride, heated up to 50°C, and reacted for 2 hours; after the reaction, washed with tetrahydrofuran, 5% hydrochloric acid, and distilled water in sequence until there were no chloride ions, washed with methanol three times, and dried in vacuum to obtain acetylated cross-linked polystyrene;

[0038] 2) Add 200mL of chlorobenzene, 400mL of water, 92g of sulfuric acid with a mass concentration of 50% in a 2000mL four-necked reaction flask equipped with a reflux condenser, a thermometer, and an agitator, and 80g of acetylated cross-linked polystyrene. After heating to boiling, Add 600g of potassium permanganate in batches, reflux for 5 hou...

Embodiment 2

[0043] Preparation of polystyrene polymer peroxyacid:

[0044] 1) Add 100g of dichloromethane and 70g of cross-linked polystyrene into a 1000mL four-necked reaction flask equipped with a reflux condenser, thermometer, and stirrer, stir and swell at room temperature for 6 hours; add 123g of anhydrous aluminum trichloride, dropwise 130g of acetyl chloride, heated up to 50°C, and reacted for 2 hours; after the reaction, washed with tetrahydrofuran, 5% hydrochloric acid, and distilled water in sequence until there was no chloride ion, washed with methanol three times, and dried in vacuum to obtain acetylated cross-linked polystyrene;

[0045] 2) Add 200mL of chlorobenzene, 400mL of water, 96g of sulfuric acid with a mass concentration of 50% in a 2000mL four-necked reaction flask equipped with a reflux condenser, a thermometer, and an agitator, and 90g of acetylated cross-linked polystyrene, and heat to boiling. Add 600g of potassium permanganate in batches, reflux for 5 hours; fi...

Embodiment 3

[0050] Preparation of polystyrene polymer peroxyacid:

[0051] 1) Add 100g of dichloromethane and 65g of cross-linked polystyrene into a 1000mL four-necked reaction flask equipped with a reflux condenser, thermometer, and stirrer, stir and swell for 6 hours at room temperature; add 125g of anhydrous aluminum trichloride, dropwise 150g of acetyl chloride, heated up to 50°C, and reacted for 2 hours; after the reaction, washed with tetrahydrofuran, 5% hydrochloric acid, and distilled water in sequence until there were no chloride ions, washed with methanol three times, and dried in vacuum to obtain acetylated cross-linked polystyrene;

[0052] 2) Add 200mL of chlorobenzene, 400mL of water, 98g of sulfuric acid with a mass concentration of 50% into a 2000mL four-necked reaction flask equipped with a reflux condenser, a thermometer, and an agitator, and 80g of acetylated cross-linked polystyrene. After heating to boiling, Add 600g of potassium permanganate in batches, reflux for 5 ...

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Abstract

The invention relates to a method for preparing 2-methyl-1,4-naphthoquinone through microwave radiation. The 2-methyl-1,4-naphthoquinone is prepared from beta-methylnaphthalene in a solvent acetate acid gracial under the action of microwave radiation with a polystyrene type polymeric peroxy acid as an oxidant, and the yield reaches 65.0% or above. Microwave radiation heating is adopted, so the reaction time is obviously shortened, and the product yield is improved; and the polymeric peroxy acid oxidant is adopted, so the method has the advantages of high product yield, convenient post-treatment , avoiding of heavy metal pollution of chromium salt oxidants, environmental protection, and important application values.

Description

technical field [0001] The invention relates to a preparation method of 2-methyl-1,4-naphthoquinone, in particular to a method for preparing 2-methyl-1,4-naphthoquinone by catalyzing β-methylnaphthalene with microwave radiation. Background technique [0002] 2-Methyl-1,4-naphthoquinone, also known as 2-menaquinone, β-menaquinone, is a synthetic vitamin K 3 It is an important intermediate and has a wide range of uses in medicine and feed additives. In the current industrial production, the main synthesis method of 2-methyl-1,4-naphthoquinone is the liquid-phase oxidation method using β-methylnaphthalene as raw material and chromium salt as oxidant. The main disadvantage of this method is that the chromium salt is corrosive and requires high corrosion resistance to the environment, and a large amount of chromium-containing wastewater will be generated during the production process, which seriously pollutes the environment. [0003] For this reason, people explore the method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C46/04C07C50/10C08F12/08C08F8/10C08F8/06
CPCC07C46/04C08F8/10C08F8/06C08F12/08C07C50/10
Inventor 陶绪泉胡大伟郭丽和陈汪洋崔慧
Owner LIAOCHENG UNIV
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