Preparation of 1-naphthalene bromide

A technology of brominated naphthalene and refined naphthalene, which is applied in the field of preparation of 1-bromonaphthalene, can solve the problems of high raw material price and damage, and achieve the effect of reducing production cost and benefiting environmental protection

Active Publication Date: 2009-05-20
上海三爱思试剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the raw material carbon tetrachloride is a chemical that is strictly controlled inter

Method used

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  • Preparation of 1-naphthalene bromide

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Add 1.03mol refined naphthalene and 125 grams of mixed dichloroethane solvent (1,2-dichloroethane and 1,1-dichloroethane's weight ratio is 30%:70%) in reactor, heat up under stirring Dissolve, add 1.13 mol of bromine dropwise, after the addition, reflux at 75-95°C for 5 hours, and the reaction ends. Then change to a distillation device, recover the mixed dichloroethane solvent, and completely distill the mixed dichloroethane. Then add 40 grams of 30% by weight sodium hydroxide to the residue in the bottle, and remove the alkali water layer to obtain 201 grams of crude product 1-bromonaphthalene, which is moved into a fractionating bottle for fractional distillation under reduced pressure. 158.5 g of the main fraction was obtained by distillation under reduced pressure at 135°C, with a yield of 74.02%, and the quality met the national chemical purity standard.

Embodiment 2

[0020] Add 1.03mol refined naphthalene and 110 grams of mixed dichloroethane solvent (1,2-dichloroethane and 1,1-dichloroethane's weight ratio is 50%:50%) in reactor, heat up under stirring Dissolve, add 1.08 mol of bromine dropwise, after the addition, reflux at 75-95°C for 5 hours, and the reaction ends. Then change to a distillation device, recover the mixed dichloroethane solvent, and completely distill the mixed dichloroethane. Add 30 grams of 30% by weight sodium hydroxide to the residue in the bottle, separate the aqueous alkali layer to obtain 202.5 grams of crude product 1-bromonaphthalene, which is moved into a fractionating bottle for fractional distillation under reduced pressure. 159.5 g of the main fraction was obtained by distillation under reduced pressure at 135°C, with a yield of 74.52%, and the quality met the national chemical purity standard.

Embodiment 3

[0022] Add 1.03mol refined naphthalene and 95 grams of mixed dichloroethane solvent (1,2-dichloroethane and 1,1-dichloroethane's weight ratio is 30%:70%) in reactor, heat up under stirring Dissolve, add 1.05 mol of bromine dropwise, reflux at 75-95°C for 5 hours after addition, and the reaction ends. Then change to a distillation device, recover the mixed dichloroethane solvent, and completely distill the mixed dichloroethane. Add 20 grams of 30% by weight sodium hydroxide to the residue in the bottle, separate the aqueous alkali layer to obtain 209 grams of crude product 1-bromonaphthalene, which is moved into a fractionating bottle for fractional distillation under reduced pressure. 164 g of the main fraction was obtained by distillation under reduced pressure at 135°C, with a yield of 76.62%, and the quality met the national chemical purity standard.

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Abstract

A preparing method of 1-naphthalene bromide adopts refined naphthalene and the mixed solvent of 1, 2-dutch liquid and 1, 1-dutch liquid. After being stirred, the mixture is heated up and dissolved; bromine is added, and the temperature is kept between 75 and 95 DEG C; refluence reaction is kept for 4 to 6 hours, and then the mixture is distilled; solvent is recycled; sodium hydroxide is added for neutralizing hydrogen bromide in the reaction solution; after a lye layer is separated, a crude product can be obtained; and after decompression and fractionation, a chemically pure 1-naphthalene bromide product can be obtained from the crude product. The method is beneficial for environmental protection and reduces the producing cost, and the quality of the product complies with the national chemically pure standard.

Description

technical field [0001] The present invention relates to a kind of preparation method of 1-bromonaphthalene, specifically relate to a kind of method that prepares 1-bromonaphthalene by reaction of refined naphthalene and bromine. Background technique [0002] 1-Bromonaphthalene is a colorless or light yellow oily liquid with a pungent odor of refined naphthalene. It can be mixed with alcohol, ether and benzene, slightly soluble in water. The boiling point is 279 ° C ~ 282 ° C. [0003] The conventional preparation method of 1-bromonaphthalene ([1] Windholz Martha ed.The MerckIndex.llth ed.Rahway (New Jersey): Merck&Co., Inc., 1988.1413; [2] Han Guangdian, Fan Rulin, Li Shuwen compilation. Organic Handbook of Preparative Chemistry, Volume 1. New 1st Edition. Beijing: Chemical Industry Press, 1985.142) is refined naphthalene and bromine in carbon tetrachloride as a solvent, reacting at 80-95°C to generate 1-bromonaphthalene, which is removed by distillation Solvent, and then...

Claims

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Application Information

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IPC IPC(8): C07C25/18C07C17/12
Inventor 曾勇强祝友良顾震虎
Owner 上海三爱思试剂有限公司
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