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Method for preparing N,N-diethyl-1,4-phenylenediamine sulphate

A technology of diethylaniline and phenylenediamine, applied in the field of N, can solve problems such as unsatisfactory requirements, high impurity content, complicated process, etc., and achieve the effect of stable and reliable quality, high purity, and good reduction performance

Inactive Publication Date: 2009-12-23
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing N,N-diethyl-1,4-phenylenediamine sulfate preparation method has high impurity content, low purity, poor stability and complicated process, which cannot meet the requirements for reagents in the field of environmental monitoring

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A kind of N, the preparation method of N-diethyl-1,4-phenylenediamine sulfate, this preparation method comprises the following steps:

[0027] (1). Nitrosation step:

[0028] In a 10-liter three-necked flask, add 1500ml of water and 610ml of concentrated hydrochloric acid, then add 375ml of diethylaniline, mix, and cool to 5°C. An aqueous solution of sodium nitrite prepared from 370 g of sodium nitrite and 530 ml of water was added dropwise with stirring. The reaction temperature was maintained at 5°C. After adding the aqueous sodium nitrite solution, the stirring reaction was continued for 3 hours. An aqueous solution of p-nitroso-N,N-diethylaniline was obtained.

[0029] (2). Restore steps:

[0030] In the reaction solution of step (1), add 1500ml of water and 500ml of concentrated hydrochloric acid and gradually add 460g of zinc powder under stirring.

[0031] (3). Purification steps:

[0032] In the above reaction solution, an appropriate amount of sodium hydr...

Embodiment 2

[0036] A kind of N, the preparation method of N-diethyl-1,4-phenylenediamine sulfate, this preparation method comprises the following steps:

[0037] (1). Nitrosation step:

[0038] In a 5-liter three-necked flask, add 750ml of water and 305ml of concentrated hydrochloric acid, then add 187ml of diethylaniline, mix, and cool to 8°C. An aqueous solution of sodium nitrite prepared from 135 g of sodium nitrite and 265 ml of water was added dropwise with stirring. The reaction temperature was maintained at 8°C. After adding the aqueous sodium nitrite solution, the stirring reaction was continued for 2.8 hours. An aqueous solution of p-nitroso-N,N-diethylaniline was obtained.

[0039] (2). Restore steps:

[0040] In the reaction solution of step (1), add 750ml of water and 250ml of concentrated hydrochloric acid and gradually add 230g of zinc powder under stirring.

[0041] (3). Purification steps:

[0042] In the above reaction solution, an appropriate amount of sodium hydro...

Embodiment 3

[0046] A kind of N, the preparation method of N-diethyl-1,4-phenylenediamine sulfate, this preparation method comprises the following steps:

[0047] (1). Nitrosation step:

[0048] In a 1-liter three-necked flask, add 150ml of water and 61ml of concentrated hydrochloric acid, then add 37ml of diethylaniline, mix, and cool to 0°C. An aqueous solution of sodium nitrite prepared from 37 g of sodium nitrite and 53 ml of water was added dropwise with stirring. The reaction temperature was maintained at 0°C. After adding the aqueous sodium nitrite solution, the stirring reaction was continued for 2.5 hours. An aqueous solution of p-nitroso-N,N-diethylaniline was obtained.

[0049] (2). Restore steps:

[0050] In the reaction solution of step (1), add 150ml of water and 50ml of concentrated hydrochloric acid and gradually add 46g of zinc powder under stirring.

[0051] (3). Purification steps:

[0052] In the above reaction solution, an appropriate amount of sodium hydroxide w...

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PUM

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Abstract

The invention relates to a method for preparing N,N-diethyl-1,4-phenylenediamine sulphate, which comprises the following steps of nitration, reduction, purification and salification. The method uses diethyl aniline for nitrosification and reduction to generate N,N-diethyl-1,4-phenylenediamine; and the N,N-diethyl-1,4-phenylenediamine is subjected to purification and then the N,N-diethyl-1,4-phenylenediamine is reacted with sulfuric acid to prepare the N,N-diethyl-1,4-phenylenediamine sulphate with high purity. The preparation method is simple, convenient and feasible; and the synthesized product has high purity and stable and reliable quality and is suitable for the high standard special requirement of environmental monitoring.

Description

technical field [0001] The invention belongs to the field of environmental protection reagents, in particular to a preparation method of N,N-diethyl-1,4-phenylenediamine sulfate. Background technique [0002] At present, drinking water, hospital sewage, papermaking wastewater, and printing and dyeing wastewater mostly contain residual chlorine. The main sources are: adding chlorine to drinking water or sewage to kill or inhibit microorganisms; adding chlorine to wastewater to decompose toxic cyanide. Residual chlorine in water will cause phenolic water to produce chlorophenol odor, and can also generate organic chlorides, causing water pollution. Moreover, due to the presence of combined chlorine in water, it is very easy to have harmful effects on aquatic organisms. Therefore, in the field of environmental protection monitoring, the monitoring of residual chlorine in water is very important. At present, the most commonly used methods for determining residual chlorine in w...

Claims

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Application Information

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IPC IPC(8): C07C211/50C07C209/38
Inventor 邹政红闫汝连何金
Owner TIANJIN CHEM REAGENT RES INST
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