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Niacin method for preparing aromatic nitrocompound of alkali sulfide

A technology for aromatic nitro group and compound is applied in the field of aromatic nitro compound for preparing alkali sulfide by nicotinic acid method, and can solve the problems of serious pollution and high energy consumption

Inactive Publication Date: 2017-03-08
YANCHENG OUHUA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The production areas of soda sulfide are concentrated in Shanxi, Inner Mongolia, Xinjiang, Sichuan and other western regions, and more than 90% of soda sulfide is produced by reducing mirabilite with pulverized coal, causing extremely serious pollution and high energy consumption

Method used

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  • Niacin method for preparing aromatic nitrocompound of alkali sulfide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment one, such as figure 1 As shown, the preparation of the reducing solution in step 1: dissolve the nicotinic acid powder in a sodium chloride solution with a mass percent concentration of 15% at 160°C, and the ratio of the amount of nicotinic acid powder to sodium chloride is 0.8 : 1, for subsequent use, the niacin powder can also be replaced by soda ash, baking soda or ammonia;

[0017] Step 2 Reduction: put the aromatic nitro compound into the reducing solution prepared above, heat up to 295°C to carry out the reduction reaction, and obtain the aromatic amino compound, the ratio of the amount of niacin powder to the aromatic nitro compound It is 2.5:1, and the described reaction reacts under normal pressure or pressure.

Embodiment 2

[0018] Embodiment two, such as figure 1 As shown, the preparation of the reducing solution in step 1: dissolve the niacin powder in a sodium chloride solution with a mass percent concentration of 25% at 180°C, and the ratio of the amount of niacin powder to sodium chloride is 1 : 1, for subsequent use, the niacin powder can also be replaced by soda ash, baking soda or ammonia;

[0019] Step 2 Reduction: Put the aromatic nitro compound into the above-mentioned prepared reducing solution, heat up to 300°C for reduction reaction, and obtain the aromatic amino compound, the ratio of the amount of niacin powder to the aromatic nitro compound It is 3.5:1, according to step 2, the described reaction reacts under normal pressure or pressure.

Embodiment 3

[0020] Embodiment three, such as figure 1 As shown, the preparation of the reducing solution in Step 1: dissolve the nicotinic acid powder in a sodium chloride solution with a mass percent concentration of 45% at 200°C, and the ratio of the amount of nicotinic acid powder to sodium chloride is 2 : 1, for subsequent use, the niacin powder can also be replaced by soda ash, baking soda or ammonia;

[0021] Step 2 Reduction: Put the aromatic nitro compound into the above-mentioned prepared reducing solution, heat up to 325°C for reduction reaction, and obtain the aromatic amino compound, the ratio of the amount of niacin powder to the aromatic nitro compound It is 4:1, and the described reaction reacts under normal pressure or pressure.

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Abstract

The invention discloses a niacin method for preparing an aromatic nitrocompound of alkali sulfide. A reduction liquid is prepared as follows: niacin powder is dissolved in a sodium chloride solution with the concentration being 15%-45% in mass percentage at the temperature of 160-200 DEG C for later use, and the amount-of-substance ratio of the niacin powder to sodium chloride is (0.8-2):1. The niacin method for preparing the aromatic nitrocompound of alkali sulfide is provided, and the aromatic nitrocompound of alkali sulfide is prepared with the niacin method and can replace high-pollution and high-energy-consumption alkali sulfide almost in all niacin powder application fields.

Description

technical field [0001] The invention relates to a reduction method, in particular to a method for preparing aromatic nitro compounds of sodium sulfide by nicotinic acid method. Background technique [0002] The methods for the amination of aromatic nitro compounds include reducing agent reduction, catalytic hydrogenation reduction, electrolytic reduction and high-pressure ammonium decomposition. Among them, reducing agent reduction is a traditional method, and reducing agents include: iron powder, zinc powder, tin particles, low-priced sulfides, hydrazine hydrate, etc. Generally speaking, the wastewater generated by reducing agent reduction is seriously polluted, difficult to treat, and expensive . Hydrogenation reduction, electrochemical reduction, high-pressure ammonolysis and other cleaning processes cannot be applied to the reduction reactions of many compounds. The reduction of aromatic nitro compounds with low-priced sulfides, especially alkali sulfide, is still wide...

Claims

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Application Information

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IPC IPC(8): C07C209/36C07C211/43C07B43/04
Inventor 卢圣茂王志伟郭宇时娇娇
Owner YANCHENG OUHUA CHEM IND