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Preparation method of octachloronaphthalene

A technology of chloronaphthalene and naphthol, applied in the field of preparation of octachloronaphthalene, can solve the problems of difficult control of decachloronaphthalene, long reaction time, low yield, etc., and achieves a product content that does not require purification, rapid reaction, and high product content. Effect

Active Publication Date: 2022-03-25
山东博苑医药化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the problem of this technology is that the reaction time is long and the yield is low. After verification, it is found that the by-product of decachlornaphthalene is difficult to control, and the crude product needs to be refined to meet the purity requirements.

Method used

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  • Preparation method of octachloronaphthalene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Chlorination stage: add 173g of dichloroethane and 57.67g (0.4mol) of 2-naphthol to the reaction bottle, connect ventilation equipment, stirring device, condenser, thermometer, safety bottle and tail gas absorption device, oil bath After raising the temperature to 85°C, start to ventilate 200g (2.8mol) to react for 8h;

[0029] (2) Hydroxychloride belt stage: Nitrogen gas is passed into the reaction bottle after the completion of chlorine passage to effectively replace residual chlorine gas, then 125g (0.6mol) of phosphorus pentachloride with 1 times the mass of 2-naphthol is added, and the temperature is raised to 90°C , followed by HPLC until the reaction was complete.

[0030] (3) After the reaction was completed, the temperature was lowered to room temperature, and a large amount of solids were precipitated, which were separated by filtration to obtain 148.56 g of the product.

[0031] The yield was 92%, and the HPLC content was 99.1%.

Embodiment 2

[0033] (1) Chlorination stage: add chloroform 865g, 2-naphthol 57.67g (0.4mol) in reaction bottle, connect aeration equipment, stirring device, condenser, thermometer, safety bottle and tail gas absorption device, oil bath is heated up to 70 After ℃, start to ventilate 285g (4mol) to react for 6h;

[0034] (2) Hydroxychloride belt stage: feed nitrogen into the reaction flask after the completion of chlorine passage to effectively replace residual chlorine, then add 164.8g (1.2mol) of phosphorus trichloride with 3 times the mass of 2-naphthol, and heat up to 70 °C, followed by HPLC until the reaction was complete.

[0035] (3) After the reaction was completed, the temperature was lowered to room temperature, and a large amount of solids were precipitated, which were separated by filtration to obtain 145.33 g of the product.

[0036] The yield was 90%, and the HPLC content was 99.2%.

Embodiment 3

[0038] (1) Chlorine passage stage: add tetrachlorethylene 460g, 2-naphthol 57.67g (0.4mol) in reaction bottle, connect ventilation equipment, stirring device, condenser, thermometer, safety bottle and tail gas absorption device, oil bath heats up After reaching 120°C, start to ventilate 227g to react for 4h;

[0039] (2) Hydroxychloride belt stage: Nitrogen gas is passed into the reaction bottle after the completion of chlorine passage to effectively replace the residual chlorine gas, then 92g (0.6mol) of phosphorus oxychloride 1.5 times the amount of 2-naphthol is added, and the temperature is raised to 130°C , followed by HPLC until the reaction was complete.

[0040] (3) After the reaction was completed, the temperature was lowered to room temperature, and a large amount of solids were precipitated, which were separated by filtration to obtain 153.4 g of the product.

[0041] Yield 95%, HPLC content 99%.

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Abstract

The invention discloses a preparation method of octachloronaphthalene, which comprises the following steps: by taking 2-naphthol as a raw material, introducing chlorine into a solvent for chlorination, introducing nitrogen after chlorine introduction is completed to effectively replace residual chlorine, then adding a chlorination reagent into a system, continuing heating reaction, after the reaction is completed, cooling for devitrification, and separating a product through filtration. The preparation method designed by the invention has the advantages of no side reaction, no need of a catalyst, fast reaction, high product content, no need of refining and the like.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of octachloronaphthalene. Background technique [0002] Octachloronaphthalene, full name "1,2,3,4,5,6,7,8-octachloronaphthalene", also known as "perchloronaphthalene", CAS No. 2234-13-1, is the octachloronaphthalene of naphthalene Substitutes, with good chemical stability and thermal stability, used as insulating materials in the electrical industry, additives for grinding wheel media and cutting oil coolants, and also used in the synthesis of fungicides and algicides. Regarding the preparation of octachloronaphthalene, the synthesis method reported in Chinese patent CN101844964A is: in an organic solvent, under the action of a metal catalyst, naphthalene is controlled at a temperature of 60 to 130°C, and chlorine gas is introduced to react. 8.0 to 10.0 times the amount of naphthalene, and the reaction time is 6 to 24 hours. After the reaction, the reaction ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/16C07C25/22C07C37/62C07C39/38
CPCC07C17/16C07C37/62C07C25/22C07C39/38
Inventor 于龙张杰周丽娜郭钦武翰
Owner 山东博苑医药化学股份有限公司
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