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Synthetic method of 2,6 dihydroxy naphthlene

A technology of dihydroxynaphthalene and a synthesis method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of uneven mixing of materials, difficult separation, and high consumption of alkali, and achieves convenient synthesis steps, It is not easy to separate and the effect of uniform reaction

Active Publication Date: 2015-08-19
柏盛新材料(甘肃)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the high-temperature alkali medium alkali fusion method and the organic solvent medium alkali fusion method of 2,6-naphthalene disulfonate have been applied in production, there are, for example, too much alkali consumption in the alkali medium alkali fusion method, and the material mixing is not uniform problems, and the solvents of the organic solvent medium alkali fusion method are easy to oxidize and decompose, are not easy to separate, and the problems of high cost require technical improvement to be solved

Method used

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  • Synthetic method of 2,6 dihydroxy naphthlene
  • Synthetic method of 2,6 dihydroxy naphthlene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put 166g of sodium 2,6-naphthalene disulfonate, 100g of solid sodium hydroxide, 166g of potassium nitrate, sodium nitrite and a mixture of sodium nitrate (88g of potassium nitrate, 66g of sodium nitrite, and 12g of sodium nitrate) into the alkali melting pot , then slowly heat up to 150°C, stir, continue to heat up to 320°C, and keep the alkali fusion at 320°C-325°C for 3 hours. Then lower the temperature to 200°C, slowly add 450g of water dropwise to dilute, and extract 2,6-sodium naphthalenediol with 700mL trioctane tertiary amine solvent.

[0025] The extracted sodium 2,6-naphthalenediol was acidified with sulfuric acid, filtered, and the filter cake was refined with 300 mL of ethanol-water mixed solvent to obtain 2,6-dihydroxynaphthalene, the purity of which was analyzed by liquid chromatography was above 99%, and the yield was 75%. %.

Embodiment 2

[0027] Put 166g2,6-sodium naphthalene disulfonate, 115g solid sodium hydroxide, a mixture of 182g potassium nitrate, sodium nitrite and sodium nitrate (wherein potassium nitrate 92g, sodium nitrite 76g, sodium nitrate 14g) in the alkali melting pot, Then slowly raise the temperature to 150°C, stir, continue to heat up to 310°C, and keep it at 310°C-320°C for alkali fusion for 3.5 hours; then cool down to 200°C, slowly add 450g of water to dilute, and use 700mL trioctane tertiary amine Solvent extraction of sodium 2,6-naphthalene diphenol;

[0028] The extracted sodium 2,6-naphthalene diphenol was acidified with sulfuric acid, filtered, and the filter cake was refined with 300 mL of ethanol-water mixed solvent to obtain 2,6-dihydroxynaphthalene, the purity of which was analyzed by liquid chromatography was over 99%, and the yield was 76% %.

Embodiment 3

[0030] Put 166g of sodium 2,6-naphthalene disulfonate, 83g of solid sodium hydroxide, 135g of potassium nitrate, sodium nitrite and a mixture of sodium nitrate into the alkali melting pot (65g of potassium nitrate, 60g of sodium nitrite, and 10g of sodium nitrate) , then slowly raise the temperature to 150°C, stir, continue to heat up to 320°C, and keep it at 320°C-330°C for alkali fusion for 2.5 hours; then cool down to 200°C, slowly add 450g of water to explain, and use 700mL of Amine solvent extraction of sodium 2,6-naphthalenediol.

[0031] The extracted sodium 2,6-naphthalenediol was acidified with sulfuric acid, filtered, and the filter cake was refined with 300 mL of ethanol-water mixed solvent to obtain 2,6-dihydroxynaphthalene, the purity of which was analyzed by liquid chromatography was above 99%, and the yield was 77% %.

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Abstract

The invention discloses a synthetic method of 2,6 dihydroxy naphthalene, which comprises the following steps: placing 2,6 dihydroxy naphthalene in an alkali fusion pan, then a mixture of solid sodium hydroxide and nitrate is placed, Slowly heating to 150-170 DEG C, stirring, continuously heating to 320 DEG C, insulating for fusing alkali for 2.5-3.5 hours at 310-330 DEG C, then cooling to 200 DEG C, slowly dropping 450g of water for diluting, using a tri(octyl-decyl)amine solution for extracting 2,6-dihydroxy naphthalene, then acidifying the extracted 2, 6-dihydroxy naphthalene by sulfuric acid, and filtering and refining filter cake by an ethanol water mixed solvent to obtain 2,6-dihydroxy naphthalene. According to the synthetic method of 2,6-dihydroxy naphthalene, the used inorganic solvent is a mixture of potassium nitrate, sodium nitrite and sodium nitrate. According to the invention, viscosity of an alkali fusion material is low, fluidity is good, material can be uniformly mixed, and alkali fusion effect is good. In addition, under high temperature condition for alkali fusion, no decomposition problem of oxidation organic matter is generated, and no difficult separating problem is generated for the mixture.

Description

technical field [0001] The invention belongs to the preparation method of organic hydroxyl compound. In particular, a synthetic method for preparing 2,6-dihydroxynaphthalene by alkali-melting naphthalenesulfonic acid in an inorganic solvent is proposed. Background technique [0002] 2,6-Dihydroxynaphthalene is a fine chemical raw material with important application value in polymer synthesis, medicine, dyestuff, rubber and other industries. At present, there are few production enterprises at home and abroad, but this product is indeed a product that is urgently needed by enterprises. Domestic consumption of 2,6-dihydroxynaphthalene is not much, and the main sales volume of 2,6-dihydroxynaphthalene is in the export market. [0003] According to the different raw materials used, there are two main methods for the synthesis of 2,6-dihydroxynaphthalene. One is the high temperature alkali fusion method of sodium 2,6-naphthalene disulfonate. The other is the oxidation and acid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/14C07C37/055
CPCC07C37/055C07C37/64C07C39/14
Inventor 袁仲飞张天永黄彩红
Owner 柏盛新材料(甘肃)有限公司
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