Method for preparing amino aromatic substitute by reducing nitro aromatic substitute

A nitroaromatic and substituted technology is applied in the field of amino aromatic substituted synthesis, which can solve the problems of aromatic amine-containing iron sludge and wastewater environmental pollution, high labor intensity of workers, low automation level, and the like, and achieves short reaction time, Simple production process and good product quality

Inactive Publication Date: 2019-05-17
HEBEI CHENGXIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method consumes a lot of energy and is currently only used in laboratory synthesis and semi-industrial production.
[0006] The traditional iron powder reduction process is more classic, has a strong reduction ability, and is basically suitable for the reduction of all nitro compounds, but the production has a low level of automation, high labor intensity, and the produced iron sludge and wastewater containing aromatic amines serious environmental pollution

Method used

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  • Method for preparing amino aromatic substitute by reducing nitro aromatic substitute
  • Method for preparing amino aromatic substitute by reducing nitro aromatic substitute
  • Method for preparing amino aromatic substitute by reducing nitro aromatic substitute

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Embodiment 1

[0044] The embodiment of the present invention provides a method for preparing aminoaromatic substitution co-production ultrafine iron black, comprising the following steps:

[0045] Step a, 500mL of water, 2g of nano ferric oxide and 1.5g of polyethylene glycol dialkyl ether are added to an open and stirred 1000mL four-necked reaction flask, and the temperature of the four-necked reaction flask is raised to 60 -70°C, add 30g of reduced iron agent secondary reduced iron powder, adjust the pH value to 8-9, maintain the reaction temperature and pH value, add 4,4'-dinitrostilbene-2,2'-di 25g of sulfonic acid is continuously added to the four-necked reaction flask within 3-4 hours, and after the addition is completed, the heat preservation reaction is carried out at 60-70°C for 0.5 hours to obtain the reaction feed liquid;

[0046] Step b, adjust the pH value of the reaction feed solution to 12-13 with sodium hydroxide, continue the heat preservation reaction at 60-70°C for 1 hour...

Embodiment 2

[0050] The embodiment of the present invention provides a method for preparing aminoaromatic substitution co-production ultrafine iron black, comprising the following steps:

[0051] Step a. Add 400mL of water and 20g of ferric oxide into an open and stirred 1000mL four-necked reaction flask, and raise the temperature of the four-necked reaction flask to 80-90°C, and add 20g of iron powder ore, an iron reducing agent. , adjust the pH value to 5-6, maintain the reaction temperature and pH value, add 30g of 4,4'-dinitrostilbene-2,2'-dicarboxylic acid continuously into the four-necked reaction flask within 2-3h , after the addition is completed, the heat preservation reaction is carried out at 80-90 ° C for 1 h to obtain the reaction feed liquid;

[0052] Step b, adjust the pH value of the reaction feed liquid to 12-12.5 with potassium hydroxide, continue the heat preservation reaction at 80-90°C for 1h, add 4g of potassium sulfite after the reaction, stir evenly, filter, and wat...

Embodiment 3

[0056] The embodiment of the present invention provides a method for preparing aminoaromatic substitution co-production ultrafine iron black, comprising the following steps:

[0057] Step a, add 350mL of water, 10g of ferric oxide and 6g of polyethylene glycol dialkyl ether into an open and stirred 1000mL four-necked reaction flask, and raise the temperature of the four-necked reaction flask to 90-100 ℃, add 30g of reducing iron agent sponge iron powder, adjust the pH value to 6-7, maintain the reaction temperature and pH value, add 40g of 5-nitro-2-propyl-benzoylnitrile continuously within 2.5-3h In the four-necked reaction flask, after the addition, the heat preservation reaction was carried out at 90-100°C for 2 hours to obtain the reaction feed liquid;

[0058] Step b, adjust the pH value of the reaction feed solution to 9-10 with sodium carbonate, add 8 g of ascorbic acid, stir evenly, filter, wash with water, and obtain the first product containing 5-amino-2-propyl-benzo...

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Abstract

The invention relates to the technical field of synthesis of amino aromatic substitutes, in particular discloses a method for preparing an amino aromatic substitute by reducing a nitro aromatic substitute. The method comprises the following steps that water and a catalyst are added into a first reactor, the reactor is heated, a reduced iron agent is added, the pH value is adjusted, meanwhile, thenitro aromatic substitute is added into the first reactor, and heat preservation reaction is carried out so as to obtain reaction feed liquid; the pH value of the reaction feed liquid is adjusted, heat preservation reaction is carried out, and a stabilizer is added so as to obtain a first solution containing the amino aromatic substitute and an iron black crude product; and the pH value of the first solution is adjusted, and solid-liquid separation is carried out so as to obtain the amino aromatic substitute. The production technological method provided by the invention is simple, continuous production can be realized, the operation safety and the selectivity is relatively high, the reaction time is short, the yield reaches up to 90% or above, the product quality is good, and the content reaches 98% or above.

Description

technical field [0001] The invention relates to the technical field of synthesis of aminoaromatic substitutes, in particular to a method for preparing aminoaromatic substitutes by reducing nitroaromatic substitutes. Background technique [0002] Amino aromatic substituents are widely used in dyes, rubber, medicine, pesticides, pigments, additives, chemical reagents and other fields. They are important intermediates in organic synthesis and are obtained by catalytic reduction of nitroaromatic substituents. In the prior art, there are many methods for producing aminoaromatic substitutes, which can be divided into several methods such as alkali sulfide reduction, catalytic hydrogenation reduction, electrochemical reduction, and iron powder reduction. [0003] Alkali sulfide reduction method is a relatively mature production process with relatively mild reaction, good selectivity, easy separation of products, easy realization of closed production, short production cycle, and low...

Claims

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Application Information

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IPC IPC(8): C07C303/22C07C309/46C07C227/04C07C229/60C07C253/30C07C255/42C07C213/02C07C217/84C07C221/00C07C225/22C07C209/36C07C211/59C07B43/04
Inventor 魏雨张辰亮程丽华彭艳丽康茹梦琚朋朋董津陈雨佳梁兵
Owner HEBEI CHENGXIN
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