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Method for synthesizing, separating and purifying diaminonaphthalene

A technology of diaminonaphthalene and a purification method, which is applied in the field of organic chemical synthesis, can solve the problems of high energy consumption, high process equipment requirements, environmental pollution and waste residue, etc., and achieves the effects of low energy consumption, low reaction risk and simple operation.

Active Publication Date: 2020-01-14
HUNAN BIDE BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims to provide a method for the synthesis, separation and purification of diaminonaphthalene to solve the technical problems such as waste residues polluting the environment, high requirements for process equipment, and large energy consumption in the existing reduction process

Method used

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  • Method for synthesizing, separating and purifying diaminonaphthalene
  • Method for synthesizing, separating and purifying diaminonaphthalene

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Experimental program
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Effect test

Embodiment 1

[0026] The alcoholic aqueous solution that 545kg dinitronaphthalene and 32kg sodium hydroxide, 300L ethanol+450L water are made into is added in the reduction kettle, under mechanical stirring and reflux temperature, 820kg zinc powder (dinitronaphthalene: zinc powder mol ratio =1:5) was added in 5 batches, and 250L of alcohol aqueous solution was supplemented, and the reaction was stopped when the reaction solution was refluxed for 6 hours until the reaction solution was nearly colorless or light yellow. Cool the colorless or light yellow reaction liquid to room temperature, pump the reaction material into the plate and frame filter press to filter, the filtrate enters the solvent recovery kettle, after collecting the filter residue, enter the electrolytic cell to recover zinc, recover the solvent and filter to obtain the crude product of diaminonaphthalene The crude product enters the rectifying tower for purification to obtain 1.8-diaminonaphthalene with a purity>99.5%. The m...

Embodiment 2

[0029] Add the aqueous solution made of 545kg of dinitronaphthalene, 32kg of sodium hydroxide and 300LDMF+450L water into the reduction kettle, turn on the stirring and jacket steam, control the temperature between 70~75°C, and add 650kg of zinc powder (dinitronaphthalene Base naphthalene:zinc powder molar ratio=1:4.0) was added in 5 batches, and kept for 8 hours until the reaction solution was nearly colorless or light yellow, then the reaction was stopped. Cool the colorless or light yellow reaction liquid to room temperature, pump the reaction material into the plate and frame filter press to filter, the filtrate enters the solvent recovery kettle, after collecting the filter residue, enter the electrolytic cell to recover zinc, recover the solvent and filter to obtain the crude product of diaminonaphthalene The crude product enters the rectifying tower for purification to obtain 1.8-diaminonaphthalene with a purity>99.7%. The material in the kettle is recrystallized with ch...

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Abstract

The invention discloses a method for synthesizing, separating and purifying diaminonaphthalene. Dinitronaphthalene is used as a raw material; and zinc powder is taken as a reducing agent. The method comprises following steps: carrying out reduction to obtain a mixed diaminonaphthalene in a system of an alkaline polar solvent and water, subjecting an obtained product to further distillation purification and recrystallization to obtain a high-purity diaminonaphthalene product, wherein in reduction process of zinc powder, zinc chloride is generated, after filtering, a filter cake is adopted to recovery zinc through electrolysis, so that cyclic utilization of zinc powder is achieved. According to the method, nitro is reduced into amino with zinc powder; the utilization rate of the raw materials is improved; three wastes are reduced, production cost is reduced; and meanwhile, the defects that iron mud difficult to treat generated by an iron powder reduction method pollutes the environment,a hydrogenation reduction method has high requirements on production equipment and a production process and needs an excellent hydrogen source, an electric reduction method is high in energy consumption, reaction conditions are harsh and the like are effectively avoided; zinc chloride is generated in the reduction process, and zinc is recycled in an electrolysis mode, so that cyclic utilization ofthe catalyst is achieved.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a method for synthesizing, separating and purifying diaminonaphthalene. Background technique [0002] Diaminonaphthalene is often used as an intermediate for dyes or pigments, and is also a raw material for synthetic resins and pesticides. Diaminonaphthalene mainly refers to 1,5-diaminonaphthalene and 1,8-diaminonaphthalene, of which 1,5-diaminonaphthalene is mainly used for the synthesis of azo dyes, and 1,8-diaminonaphthalene is mainly used for the synthesis of Dyes, such as solvent red 179, solvent red 135, solvent orange 60. [0003] The method that existing dinitronaphthalene is reduced into diaminonaphthalene all has defects: the iron powder reduction method produces the iron mud pollution environment that is difficult to handle, and the yield is low, belongs to elimination process; No pollution to the environment, but the use of precious metals requires high inv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/36C07C211/57C25C1/16
CPCC07C209/36C25C1/16C07C211/57Y02P20/584Y02P10/20
Inventor 曹胜文甘娟李华轩王宇
Owner HUNAN BIDE BIOTECH