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A kind of preparation method of 1,5-dihydroxynaphthalene

A technology of dihydroxynaphthalene and refined naphthalene, which is applied in 1 field, can solve problems such as high temperature and high pressure, and achieve the effects of reducing equipment requirements, reducing emissions, and being easy to operate

Active Publication Date: 2016-05-04
QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Compared with the existing domestic literature reports, the alkali fusion process also has the problem of high temperature and high pressure

Method used

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  • A kind of preparation method of 1,5-dihydroxynaphthalene

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preparation example Construction

[0025] The invention discloses a preparation method of 1,5-dihydroxynaphthalene, comprising the following steps:

[0026] A) After sulfonation reaction of refined naphthalene and sulfonating agent, salting out to obtain reaction solid and reaction liquid;

[0027] B) Under the action of a catalyst, the reaction solid obtained in the above step A), water and inorganic strong base are heated and reacted to obtain 1,5-dihydroxynaphthalene;

[0028] The catalyst is one or more of methanol, ethanol and propanol.

[0029] The present invention reduces the reaction temperature of the alkali fusion step in the production process of 1,5-dihydroxynaphthalene by adding a catalyst in the reaction process, thereby reducing the requirements for equipment, and also reducing the risk factor in actual production, so that the reaction conditions are mild , Easy to operate.

[0030] All the raw materials of the present invention have no special limitation on their sources, they can be purchase...

Embodiment 1

[0048] First, put 180g of 20% oleum into a 500ml three-necked bottle, and use an ice-water bath to control the temperature to 15°C. Under stirring conditions, slowly add 30.3g of refined naphthalene, complete the addition within 40 minutes, and then stir for 30 minutes Finally, raise the temperature of the above reaction system to 55°C for sulfonation reaction, after 4 hours of reaction, cool down to 30°C, slowly pour the sulfonation solution into 400g of 20% salt water for salting out, and then filter the salting out mixture , to obtain a reaction solution and a reaction solid.

[0049] The above reaction solid was dissolved in 300ml hot water, and then the pH of the solution was adjusted to 6 with sodium hydroxide, and then the temperature was lowered to 15°C for filtration to obtain a white solid, namely 1,5-naphthalene disulfonic acid. Carry out HPLC analysis to it, the result shows that the purity of 1,5-naphthalene disulfonic acid is more than or equal to 98%, it is test...

Embodiment 2

[0054] First, put 220g of sulfuric acid into a 500ml three-neck bottle, use an ice-water bath to cool and control the temperature to 18°C, and slowly add 30.3g of refined naphthalene under stirring conditions, and complete the addition within 40 minutes. After stirring for another 30 minutes, the above The temperature of the reaction system was raised to 55°C for sulfonation reaction. After 4 hours of reaction, the temperature was lowered to 30°C, and the sulfonation solution was slowly poured into 340g of 20% salt water for salting out, and then the salting out mixture was filtered through pressure to obtain a reaction liquid and react solids.

[0055] The above reaction solid was dissolved in 300ml hot water, and then the pH of the solution was adjusted to 6 with sodium hydroxide, and then the temperature was lowered to 15°C for filtration to obtain a white solid, namely 1,5-naphthalene disulfonic acid. Carry out HPLC analysis to it, the result shows that the purity of 1,5-n...

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Abstract

The invention provides a preparation method of 1,5-dihydroxy naphthalene. The preparation method comprises the following steps: after sulfonation reaction between refined naphthalene and sulfonating agents, salting out to obtain reaction solid and reaction liquid; in the presence of catalysts, heating the reaction solid obtained in the former step, water and inorganic strong alkali to react to obtain1,5-dihydroxy naphthalene, wherein the catalysts are one or more of methanol, ethanol and propanol. The preparation method provided by the invention has the beneficial effects that the reaction temperature in the alkali fusion step in the 1,5-dihydroxy naphthalene production process is reduced, thus reducing the requirements of equipment and reducing the danger coefficient in actual production, so that the reaction conditions are mild and the preparation method is easy to operate.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a preparation method of 1,5-dihydroxynaphthalene. Background technique [0002] 1,5-dihydroxynaphthalene, also known as 1,5-naphthalenediol, has the structure of formula I, soluble in ether and acetone, slightly soluble in alcohol and acetic acid, hardly soluble in water, insoluble in benzene and petroleum ether, its alkaline The solution turned brown in air. [0003] [0004] 1,5-Dihydroxynaphthalene is an important chemical intermediate, which is mostly used in organic synthesis, dye intermediates, pharmaceutical intermediates, and photographic industries, among which it is mainly used as an important intermediate for acid dye mordant black PV and hair dyes. With the increasing variety and quantity of dyes, the market demand for 1,5-dihydroxynaphthalene is increasing day by day, but the domestic production level of 1,5-dihydroxynaphthalene is not high enough to me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/14C07C37/04
CPCC07C37/04C07C303/06C07C39/14C07C309/35
Inventor 杨伦花林凤章史红叶张淑丽
Owner QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP
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