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Preparation method of 1-bromonaphthalene

A technology for bromonaphthalene and industrial naphthalene is applied in the preparation field of synthesizing 1-bromonaphthalene, which can solve the problems of pollution and low utilization rate of bromine, and achieve the effects of less environmental pollution, convenient preparation process and low equipment requirements.

Inactive Publication Date: 2014-06-18
常州市正锋光电新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved by the present invention is: in the prior art, using bromine as a raw material, in the process of preparing 1-bromonaphthalene, the utilization rate of bromine is very low, and it is easy to bring certain pollution

Method used

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  • Preparation method of 1-bromonaphthalene
  • Preparation method of 1-bromonaphthalene
  • Preparation method of 1-bromonaphthalene

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Embodiment Construction

[0015] 128g of industrial naphthalene, 300ml of dichloroethane, and 167g of an aqueous solution of hydrobromic acid with a solute mass fraction of 48% were added to a 1000ml four-necked flask with a stirrer, a condenser and a thermometer, and 200ml of deionized water was added. Add 110g of 30% (solute mass fraction) hydrogen peroxide dropwise at 30-40°C, complete the dropwise addition for half an hour, and keep the reaction at 40-45°C after the drop is completed. During the reaction, follow the reaction with gas chromatography, and the reaction is complete in half an hour, and then separate it out. After dichloroethane was distilled from the water layer and the oil layer at atmospheric pressure, 192 g of 1-bromonaphthalene was obtained by distillation under reduced pressure, with a content of 98.5% (mass percentage) and a yield of 92% (calculated by the conversion rate of naphthalene).

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Abstract

The invention belongs to the field of organic chemical synthesis, and in particular relates to a preparation method of 1-bromonaphthalene synthesized of hydrobromic acid, hydrogen peroxide and the like. The preparation method disclosed by the invention comprises the following steps of: adding industrial naphthalene, dichloroethane and hydrobromic acid into a four-neck flask provided with a stirrer, a condenser pipe and a thermometer, adding water, dropwise adding hydrogen peroxide at normal temperature, reacting at 40-45 DEG C under heat-preserved condition; and at the end of the reaction, separating out a water layer, distilling out dichloroethane, distilling under reduced pressure to obtain 1-bromonaphthalene. The preparation method disclosed by the invention is convenient in preparation process, low in equipment requirement, hardly causes environmental pollution, can produce high-quality products and is applied to mass production; the utilization rate of the bromine resource is high; the residual Br is very low after reaction; environment pollution is hardly caused; and the prepared 1-bromonaphthalene is same as the standard sample through gas-phase and liquid-phase detection.

Description

Technical field [0001] The invention belongs to the field of organic chemical synthesis, and in particular relates to a preparation method for synthesizing 1-bromonaphthalene by utilizing hydrobromic acid, hydrogen peroxide and other raw materials. Background technique [0002] 1-Bronaphthalene is also called 1-bromonaphthalene or A-bromonaphthalene. Its structural formula is: [0003] [0004] It is a colorless or slightly yellow liquid, insoluble in water, but miscible with alcohol, ether and carbon tetrachloride. Its main uses are: organic synthesis raw materials, analytical reagents, used as refrigerants and solvents for substances with large molecular weights; 1-Bronaphthalene is also a heat carrier for dry items, and can also be used for refractive index measurement and high-magnification objective lenses of optical microscopes (100X) Using bronaphthalene as the refractive medium, the numerical aperture of the objective lens is increased to increase the magnificati...

Claims

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Application Information

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IPC IPC(8): C07C25/22C07C17/12
Inventor 徐小虎
Owner 常州市正锋光电新材料有限公司
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