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Method for preparing high-purity hydrochloride naphthodiamide

A naphthalene ethylenediamine hydrochloride, high-purity technology, applied in the preparation of amino compounds from amines, chemical recovery, organic chemistry, etc., can solve impurities, naphthalene ethylenediamine hydrochloride solubility, sensitivity, blank value and poor reproducibility , poor quality, etc.

Inactive Publication Date: 2009-04-01
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the quality of naphthaleneethylenediamine hydrochloride products produced by general manufacturers is relatively poor, and most of them contain impurities, which cause the solubility, sensitivity, blank value and reproducibility of naphthaleneethylenediamine hydrochloride to be very poor, thereby affecting the monitoring accuracy and cannot meet the requirements. Environmental Monitoring Requirements

Method used

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  • Method for preparing high-purity hydrochloride naphthodiamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The preparation of high-purity naphthalene ethylenediamine hydrochloride:

[0026] (1). Add 69 grams of bromonaphthalene and 160 grams of ethylenediamine to a reaction kettle equipped with a mechanical stirring cooling reflux device, heat the mixture to 110°C, keep the temperature at reflux for 10 hours, and then cool to 70°C ;

[0027] (2). After mixing copper powder and copper oxide powder in a weight ratio of 100:5, take a catalytic amount of the mixture and add it to the reactor, reflux for 10 hours, and cool naturally;

[0028] (3). Excessive ethylenediamine is reclaimed by vacuum distillation;

[0029] (4). Extract the reactant with benzene, filter, and reclaim benzene by distillation under reduced pressure;

[0030] (5). Underpressure distillation obtains product naphthalene ethylenediamine;

[0031] (6). Naphthalene ethylenediamine was added to the reagent hydrochloric acid solution with a concentration of 4M, the temperature was cooled to 0°C, and the crysta...

Embodiment 2

[0034] The preparation of high-purity naphthalene ethylenediamine hydrochloride:

[0035] (1). Add 414 kg of bromonaphthalene and 960 kg of ethylenediamine to a reaction kettle equipped with a mechanical stirring cooling reflux device, heat the mixture to 130°C, keep the temperature at reflux for 6 hours, and then cool to 80°C ;

[0036] (2). After mixing copper powder and copper oxide powder in a weight ratio of 100:30, take a catalytic amount of the mixture and add it to the reactor, reflux for 6 hours, and cool naturally;

[0037] (3). Excessive ethylenediamine is reclaimed by vacuum distillation;

[0038] (4). Extract the reactant with ethanol, filter, and reclaim ethanol by distillation under reduced pressure;

[0039] (5). Underpressure distillation obtains product naphthalene ethylenediamine;

[0040] (6). Naphthalene ethylenediamine was added to the reagent hydrochloric acid solution with a concentration of 8M, cooled to 5° C. with ice, and crystallized by filtratio...

Embodiment 3

[0043] The preparation of high-purity naphthalene ethylenediamine hydrochloride:

[0044] (1). Add 207 kg of bromonaphthalene and 480 kg of ethylenediamine to a reaction kettle equipped with a mechanical stirring cooling reflux device, heat the mixture to 120°C, keep the temperature at reflux for 8 hours, and then cool to 75°C ;

[0045] (2). After mixing copper powder and copper oxide powder in a weight ratio of 100:20, take a catalytic amount of the mixture and add it to the reactor, reflux for 8 hours, and cool naturally;

[0046] (3). Excessive ethylenediamine is reclaimed by vacuum distillation;

[0047] (4). Extract the reactant with benzene, filter, and reclaim benzene by distillation under reduced pressure;

[0048] (5). Underpressure distillation obtains product naphthalene ethylenediamine;

[0049] (6). Add naphthalene ethylenediamine to the reagent hydrochloric acid solution with a concentration of 6M, cool to 4° C. with ice, and filter to crystallize;

[0050] ...

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Abstract

The invention relates to a preparation method of high-purity naphthyl ethylenediamine hydrochloride. The method uses bromonaphthalene and ethylenediamine for carrying out the alkylation reaction under the action of a copper-copper oxide catalyst, thereby generating naphthyl ethylenediamine; and the reaction products are purified by using benzene, ethanol and other organic solvents, and the products after the purification are dissolved in hydrochloric acid, thereby generating the high-purity naphthyl ethylenediamine hydrochloride. The method is simple and easy, the generated naphthyl ethylenediamine hydrochloride not only has high purity, but also is applicable to the environmental monitoring; furthermore, the various reagents can be recycled during the reaction process, and the residual reagents can be reused, thereby saving the cost.

Description

technical field [0001] The invention relates to the technical field of preparation and purification of organic compounds, in particular to a preparation method of high-purity naphthaleneethylenediamine hydrochloride which can meet the requirements of environmental protection monitoring. Background technique [0002] N-(1-naphthyl)ethylenedimine dihydrochloride is an important environmental detection reagent for monitoring nitrogen oxides, aniline, methyl parathion in air and exhaust gas, and nitric acid in precipitation It can also monitor nitrate nitrogen, nitrite nitrogen, and aniline and nitrobenzene compounds in water and wastewater. However, the quality of naphthaleneethylenediamine hydrochloride products produced by general manufacturers is relatively poor, and most of them contain impurities, which cause the solubility, sensitivity, blank value and reproducibility of naphthaleneethylenediamine hydrochloride to be very poor, thereby affecting the monitoring accuracy an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/53C07C209/68
CPCY02P20/582
Inventor 阎汝连邹政红何金
Owner TIANJIN CHEM REAGENT RES INST
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