Preparation method of 1,4-naphthoquinone

A naphthoquinone and oil phase technology, applied in the field of organic compound preparation, can solve the problems of large consumption of organic solvents, complicated post-treatment process, low space-time yield and the like, and achieve the effects of increasing concentration, avoiding loss and reducing consumption

Inactive Publication Date: 2019-03-01
四川锐华科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the low space-time yield of 1,4-naphthoquinone prepared by the liquid phase oxidation method in the prior art, the consumption of organic solvent is large, the post-treatment process of the product is complicated, a large amount of waste water will be generated during the preparation process, and the pollution is serious The shortcoming of a kind of improvement naphthalene liquid phase method is provided to prepare 1, the method for space-time yield of 4 naphthoquinone, by this method, speed of reaction is improved, by-product is reduced, consumption of organic solvent is small, waste liquid zero discharge, no pollution to environment , while omitting the extraction stage of the old process, the product post-treatment process is simple, and the space-time yield of naphthoquinone is improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 1200ml of sulfuric acid solution with a concentration of 1mol / l to a three-necked flask with a capacity of 2000ml and equipped with a stirrer and a condensing reflux device, dissolve 180g of cerium sulfate in it, start stirring, and heat to 65°C; add naphthalene to another 500ml beaker 12g, 240ml cyclohexane, heated to 65°C under stirring, when the temperature in the three-necked flask reached 65°C, add the cyclohexane containing naphthalene into the three-necked flask, and add the emulsifier alkylphenol poly Oxyethylene ether 0.336g, control the temperature at 65°C and react for 30 minutes. After the reaction, place the three-necked flask in a cooling device to cool down to 20°C, stir during the cooling process, and filter after the temperature reaches 20°C for 8 minutes. Washed with purified water and dried under reduced pressure at 40°C to obtain 12.68g of yellow 1,4-naphthoquinone with a content of 96.3% and a yield of 85.6%; the space-time yield of 1,4-naphthoqu...

Embodiment 2

[0035]Add 1200ml of sulfuric acid solution with a concentration of 1mol / l to a three-neck flask with a capacity of 2000ml and equipped with a stirrer and a condensing reflux device, dissolve 180g of cerium sulfate in it, start stirring, and heat to 60°C; add naphthalene to another 500ml beaker 12g, 240ml of cyclohexane, heated to 60°C under stirring, when the temperature in the three-necked flask reached 60°C, add the cyclohexane containing naphthalene into the three-necked flask, add the emulsifier alkylphenol poly Oxyethylene ether 0.2g, control the temperature at 61°C and react for 30min. After the reaction, place the three-necked flask in a cooling device to cool down to 20°C, keep the temperature for 8min, filter, wash with a small amount of purified water, and dry under reduced pressure at 40°C to obtain yellow The 1,4-naphthoquinone was 12.44g, the content was 95.2%, and the yield was 84%; the space-time yield of 1,4-naphthoquinone was 12g / L·h.

Embodiment 3

[0037] Add 1200ml of sulfuric acid solution with a concentration of 1mol / l to a three-neck flask with a capacity of 2000ml and equipped with a stirrer and a condensing reflux device, dissolve 260g of cerium sulfate in it, start stirring, and heat to 68°C; add naphthalene to another 500ml beaker 12g, 240ml of cyclohexane, heated to 68°C under stirring, when the temperature in the three-necked flask reached 68°C, add the cyclohexane containing naphthalene into the three-necked flask, add the emulsifier alkylphenol poly Oxyethylene ether 0.366g, control the temperature at 72°C and react for 20 minutes. After the reaction is completed, place the three-neck flask in a cooling device to cool down to 20°C, keep the temperature for 8 minutes, filter, wash with a small amount of purified water, and dry under reduced pressure at 40°C to obtain yellow The 1,4-naphthoquinone was 12.88g, the content was 96.8%, and the yield was 87%; the space-time yield of 1,4-naphthoquinone was 16.26g / L·h....

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Abstract

The invention discloses a preparation method of 1,4-naphthoquinone. The preparation method comprises the following steps: taking ceric sulfate as an oxidizing agent, and dissolving the ceric sulfate into a sulfuric acid solution, thus forming a water phase; dissolving naphthalene into an organic solvent, thus forming an oil phase; mixing the water phase with the oil phase, adding an emulsifying agent, and carrying out oxidation reaction under the conditions of carrying out heat preservation and stirring; after completing the reaction, integrally cooling the water phase and the oil phase untilafter-filtration is carried out on all cerous sulfate, thus obtaining solid 1,4-naphthoquinone; separating the water phase from the oil phase, recycling the oil phase, and recycling the water phase after carrying out electrolytic regeneration on the water phase. According to the preparation method disclosed by the invention, the reaction speed is increased, and byproducts are reduced; an extraction phase of an old technology is omitted, and meanwhile, the recovery rate of naphthoquinone is increased; meanwhile, the water phase and the oil phase are both completely recycled and reused, zero emission of liquid waste is realized, the environment is not polluted, and a production method of the 1,4-naphthoquinone is economical and environment-friendly.

Description

technical field [0001] The invention relates to the technical field of preparation of organic compounds, in particular to a preparation method of 1,4 naphthoquinone. Background technique [0002] 1,4-Naphthoquinone, also known as α-naphthoquinone, is a yellow crystal with a special smell of naphthoquinone. It has a flash point of 141°C, a density of 1.422, and a melting point of 126-128°C. It sublimates when the temperature exceeds 100°C. It is slightly soluble in water. And gasoline, soluble in ethanol when heated, soluble in ether, chloroform, benzene, glacial acetic acid and carbon disulfide. The 2,3-dichloronaphthoquinone produced by the chlorination reaction of naphthoquinone is an important agricultural fungicide, which is used to prevent and control wheat smut, rice blast, potato late blight, and blight of vegetable seedlings. Naphthoquinone is used in organic synthesis, it can be used to make dye intermediate anthraquinone, pesticide fungicide, herbicide, used in sy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C46/04C07C46/10C07C50/12
CPCC07C46/04C07C46/10C07C50/12
Inventor 王彬
Owner 四川锐华科技有限公司
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