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Method for preparing iron oxide red pigment and synchronously producing aromatic amine

A technology of red iron oxide and aromatic amine, applied in the field of fine chemicals, can solve the problems of large alkali consumption, polluted environment, poor reduction selectivity, etc. Effect

Active Publication Date: 2020-06-05
HEBEI CAIKE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have their own advantages and disadvantages: catalytic hydrogenation is the cleanest and easiest reduction method, but when there are functional groups sensitive to hydrogenation in the molecule, such as halogens, double bonds and triple bonds, the reduction selectivity is poor; The reduction method has a certain selectivity for the reduction of polynitro groups, but the waste water produced will pollute the environment; the hydrogen transfer reagents commonly used in the hydrogen transfer reduction method include hydrazine hydrate, sodium borohydride, formic acid and its salts, hypophosphorous acid and isopropanol etc., it is characterized in that reaction conditions are gentle and selectivity is high, but the price of hydrogen transfer reagent is generally higher, does not have cost advantage in industrial production; Iron powder reduction method is basically applicable to the reduction process of all nitro compounds, CN101037393A has reported Preparation of Aromatic Diamines by Reduction of Aromatic Nitro Compounds by Coupling Process of Iron Powder Reduction and Hydrazine Hydrate Reduction
CN101376634A has reported the method for iron powder reduction to produce o-chloroaniline, which is characterized in that o-nitrochlorobenzene, water, hydrochloric acid and iron powder are added to the reactor, and after the reduction reaction at 90-100 ° C, the iron is separated by rake vacuum drying Mud, but neither described the whereabouts of solid waste
However, this method consumes a lot of alkali, and the saline mother liquor needs to be desalted, so there is no cost advantage

Method used

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  • Method for preparing iron oxide red pigment and synchronously producing aromatic amine
  • Method for preparing iron oxide red pigment and synchronously producing aromatic amine
  • Method for preparing iron oxide red pigment and synchronously producing aromatic amine

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add 500mm of bottom water to a stirring reduction reactor with a diameter of 3000mm and a height of 3600mm and heat up to 80-85°C, 2800kg of solid FeSO 4 ·7H 2 Add water and heat up to about 70°C to dissolve O completely, and the volume is fixed to 3.76m³. Add 842Kg of DNS (4,4′-dinitrostilbene-2,2′-disulfonic acid) to 95°C to dissolve it completely and set the volume to 3.1m³. Add DNS and ferrous sulfate solution to the reactor at the same time and control the time at about 50 minutes, control the temperature at 85-87°C, and use lye to control the pH of the reaction system at 4-4.1. After adding the ferrous sulfate solution, add iron powder (80 mesh) for the first time, and after 10 minutes of reaction, control the time of adding the remaining DNS at 210 minutes, and control the temperature at 87-88°C, and the second and third times at 70 minutes and 140 minutes, respectively. Add the remaining iron powder three times. After adding DNS, keep it warm for 40 minutes an...

Embodiment 2

[0029] Add 500mm of bottom water to the reduction reactor with a diameter of 3000mm and a height of 3600mm with stirring and raise the temperature to 80-85°C to obtain 3.41m³ of ferrous chloride solution with a concentration of 2.8mol / L. DNS (4,4′-dinitrostilbene-2,2′-disulfonic acid) 842Kg, add water and raise the temperature to 95°C to dissolve it completely and set the volume to 3.1m³. DNS and ferrous chloride solution are added to the reactor at the same time, the time is controlled at about 50 minutes, the temperature is controlled at 85-87°C, and the pH is controlled at 4-4.1 by using lye. After adding the ferrous chloride solution, add iron powder (80 mesh) for the first time, and after 10 minutes of reaction, add the remaining DNS dropwise for 210 minutes, and control the temperature at 87-88°C, 70min and 140min for the second and third time Add the remaining iron powder three times. After adding DNS, keep it warm for 50 minutes and let it pour. Use plate and frame filt...

Embodiment 3

[0031] Add 500mm of bottom water to a stirring reduction reactor with a diameter of 3000mm and a height of 3600mm and raise the temperature to 80-85°C, FeSO 4 ·7H 2 Add 2800kg of water and raise the temperature to about 70°C to completely dissolve and set the volume to 3.76m³. DNS (4,4′-dinitrostilbene-2,2′-disulfonic acid) 842Kg is added to water and heated to 95°C, and the total dissolved volume is 3.1m³. DNS and ferrous sulfate solution are added to the reactor at the same time, the time is controlled at about 50 minutes, the temperature is controlled at 85-87 °C, and the pH is controlled at 4-4.1 with lye. After adding the ferrous sulfate solution, add iron powder (200 mesh) for the first time, and after 10 minutes of reaction, add the remaining DNS time control for 210 minutes, temperature control 87-88°C, 70min and 140min for the second and third time Add the remaining iron powder, after adding DNS, keep it warm for 30 minutes and let it pour. Plate and frame filtrati...

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Abstract

The invention relates to the technical field of fine chemicals, in particular to a method for preparing iron oxide red pigment and synchronously producing aromatic amine. The method comprises the following steps: preparing an iron oxide red seed crystal from an oxidant nitro aromatic compound and ferrous iron under the action of a catalyst, reducing the nitro aromatic compound by using iron powder, synchronously generating iron oxide in situ, and growing iron oxide red with pigment performance on the seed crystal. The method particularly provides a clean and economic way for preparing aromaticamine by reducing aromatic rings containing other easy-to-reduce substituent groups.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a method for preparing iron oxide red pigment and synchronously producing aromatic amines. Background technique [0002] Aromatic amines are important chemical intermediates, which can be used to synthesize fine chemicals such as dyes, medicines, and pesticides. Aromatic amines are mainly prepared by reducing aromatic nitro compounds. The main preparation methods are catalytic hydrogenation, iron powder / acid, alkali sulfide and hydrogen transfer reduction. These methods have their own advantages and disadvantages: catalytic hydrogenation is the cleanest and easiest reduction method, but when there are functional groups sensitive to hydrogenation in the molecule, such as halogens, double bonds and triple bonds, the reduction selectivity is poor; The reduction method has a certain selectivity for the reduction of polynitro groups, but the waste water produced will pollute t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/06C07C303/22C07C309/46
CPCC01G49/06C07C303/22C01P2004/03C01P2004/62C01P2004/32C07C309/46C01P2006/62C01P2006/63C01P2006/64C01P2006/80C07C209/36
Inventor 段卫东张国福魏雨
Owner HEBEI CAIKE CHEM CO LTD
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