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Preparation method of arylamine

A technology of aromatic amines and aromatic nitro groups, which is applied in the field of preparation of aromatic amines as intermediates in organic synthesis, can solve the problems of a large amount of solvents, hydrazine hydrate, and long-term use, and achieve the effects of low cost, reasonable synthesis process, and high quality

Inactive Publication Date: 2012-08-01
LIANYUNGANG JINDUN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the main problems of the reduction of aromatic nitro compounds with hydrazine hydrate are: the reaction requires a large amount of solvent and a long time, and the consumption of hydrazine hydrate is relatively large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1, a kind of preparation method of aromatic amine, its steps are as follows:

[0018] (1) Preparation of catalyst: FeCl 3 ·6H 2 Dissolve O in an appropriate amount of distilled water, add NaOH or KOH aqueous solution dropwise while stirring to adjust the pH to 7; slowly heat up to 55°C within 110 minutes, and keep at this temperature for 12h; filter with suction, and dry the filter cake at 120°C 3.5h, grind to obtain catalyst iron oxyhydroxide powder;

[0019] (2) In a reactor with a thermometer and a dropping funnel, add a certain amount of aromatic nitro compounds, an appropriate amount of distilled water and a catalyst, ferric oxyhydroxide, heat to 60°C, and add 80% of the mass concentration within 30 minutes Hydrazine hydrate; after adding, continue to react at this temperature for 5 hours; after the reaction is over, let stand, separate layers, and add an appropriate amount of water to wash to obtain the corresponding aromatic amine of the aromatic nit...

Embodiment 2

[0021] Embodiment 2, a kind of preparation method of aromatic amine, its steps are as follows:

[0022] (1) Preparation of catalyst: FeCl 3 ·6H 2 O was dissolved in an appropriate amount of distilled water, and NaOH or KOH aqueous solution was added dropwise while stirring to adjust the pH to 8; within 130 minutes, the temperature was slowly raised to 65 °C, and kept at this temperature for 16 h; Dry for 4.5h, and grind to obtain catalyst ferric oxyhydroxide powder;

[0023] (2) In a reactor with a thermometer and a dropping funnel, add a certain amount of aromatic nitro compounds, an appropriate amount of distilled water and the catalyst ferric oxyhydroxide, heat to 100°C, and add 85% of the mass concentration within 80 minutes Hydrazine hydrate; after adding, continue to react at this temperature for 7 hours; after the reaction is over, let stand, separate layers, and add an appropriate amount of water to wash to obtain the corresponding aromatic amine of the aromatic nitr...

Embodiment 3

[0025] Embodiment 3, a kind of preparation method of aromatic amine, its steps are as follows:

[0026] (1) Preparation of catalyst: FeCl 3 ·6H 2 O was dissolved in an appropriate amount of distilled water, and NaOH or KOH aqueous solution was added dropwise while stirring to adjust the pH to 7.5; within 120 minutes, the temperature was slowly raised to 60 °C, and kept at this temperature for 14 h; Drying for 4.0h, grinding to obtain catalyst ferric oxyhydroxide powder;

[0027] (2) In a reactor with a thermometer and a dropping funnel, add a certain amount of aromatic nitro compounds, an appropriate amount of distilled water and the catalyst ferric oxyhydroxide, heat to 80°C, and add 85% of the mass concentration within 50 minutes Hydrazine hydrate; after adding, continue to react at this temperature for 6 hours; after the reaction is over, let stand, separate layers, and add an appropriate amount of water to wash to obtain the corresponding aromatic amine of the aromatic n...

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PUM

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Abstract

The invention relates to a preparation method of arylamine. The preparation method includes dissolving ferric trichloride-water (1 / 6) in distilled water, and adding dropwise an aqueous solution of sodium hydroxide or potassium hydroxide so that the pH is within the range of 7 to 8; slowly heating the solution so that the temperature is within the range of 55 DEG C to 65 DEG C, preserving heat, leaching, drying filter cakes, and grinding to obtain iron oxide hydroxide powder serving as a catalyst; and adding an aromatic nitro compound, distilled water and the catalyst into a reactor, heating the reactor to the temperature between 60 DEG C and 100 DEG C, adding hydrazine hydrate to react, allowing the reactor to stand, layering, adding an appropriate amount of water, and washing to obtain the arylamine corresponding to the aromatic nitro compound. The preparation method is safe, simple and convenient to operation, few in the three wastes, environment-friendly, high in yield and applicable to industrial production, and the product quality meets national standard.

Description

technical field [0001] The invention relates to a process for preparing an organic synthesis intermediate aromatic amine. Background technique [0002] Aromatic amines are important intermediates in organic synthesis, which are mainly obtained by reducing aromatic nitro compounds. Since the active metal reduction method and the sulfur compound reduction method will cause serious pollution, they are gradually eliminated; the hydrogenation reduction method has high efficiency and no pollution, but it must be carried out under a certain pressure, which requires high equipment requirements. Hydrazine hydrate reduction method has attracted much attention due to its non-pollution, high yield and mild reaction conditions. The catalysts used in this type of reaction include noble metal catalysts, iron compound catalysts and zeolite catalysts. Due to the good catalytic effect of cheap iron compounds, mild reaction conditions and simple equipment requirements, the hydrazine hydrate...

Claims

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Application Information

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IPC IPC(8): C07C211/47C07C211/52C07C209/36C07C213/02C07C217/84
Inventor 王耀良季政石卫兵刘旭冉
Owner LIANYUNGANG JINDUN AGROCHEMICAL CO LTD
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