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Method for producing nano-iron oxide red by using ferrous chloride recovered from waste pickling solution

A technology of ferrous chloride and red iron oxide, applied in the direction of iron oxide, iron oxide/iron hydroxide, fibrous filler, etc., can solve the problems of long reaction period, high roasting temperature, secondary pollution, etc., and reach the reaction temperature Wide range, good dispersion, strong tinting effect

Inactive Publication Date: 2011-12-14
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the Chinese Invention Patent Publication No. CN1434078, ferric salt is used as raw material, soluble alkali is added, and nano-iron oxide red is produced through processes such as stirring and heating. The production process will go through a washing process, and the resulting acidic waste liquid has no recycling value. It is easy to cause secondary pollution after direct discharge; in Chinese Invention Patent Publication No. CN85105994, iron oxide red is prepared by adding lime to the ammonia distillation tank, the reaction time is as long as 15 hours, the reaction cycle is long, and the energy consumption is high, so it is not suitable Large-scale and timely treatment of ferrous chloride recovered from waste pickling liquid in iron and steel plants; in the Chinese Invention Patent Publication No. CN87103373, iron red and ammonium sulfate are produced from sulfuric acid pickling waste liquid. To convert ferrous sulfate into red iron oxide, the roasting temperature is high, the time is long and the energy consumption is high

Method used

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  • Method for producing nano-iron oxide red by using ferrous chloride recovered from waste pickling solution
  • Method for producing nano-iron oxide red by using ferrous chloride recovered from waste pickling solution
  • Method for producing nano-iron oxide red by using ferrous chloride recovered from waste pickling solution

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Effect test

Embodiment 1

[0023] 200g of ferrous chloride was dissolved in 1.8L of water, then 1g of citrine seeds and a little iron sheet were added, stirred, and air was blown into below the liquid surface of the reaction solution; 82mL of ammonia water with a mass percentage concentration of 28% was mixed with 5L of water, Add the diluted ammonia water dropwise to the reaction system, and the dropwise addition is completed in 2 hours; continue to stir and ventilate the air for 2 hours, and stop stirring and ventilating when the pH value of the reaction system is 4 to 5; filter after standing , dried at 105°C for 1 hour, crushed and put into a drum-type programmable temperature-controlled furnace, pre-fired at a low temperature from room temperature to 200°C for 0.5 hours, then raised to 350°C at a heating rate of 5°C / min, calcined for 1.5 hours, and obtained nano-iron oxide after cooling down Red 81g.

Embodiment 2

[0025] Dissolve 250g of ferrous chloride in 1.75L of water, then add 0.6g of citrine seeds and a little iron sheet, stir, and blow air into the reaction liquid below the liquid surface; Mix, add the diluted ammonia water dropwise to the reaction system, and the dropwise addition is completed in 2.5 hours; continue to stir and pass in air for 3 hours, and stop stirring and ventilating when the pH value of the reaction system is 4 to 5; stand still After filtration, dry at 105°C for 1 hour, grind it and put it into a drum-type temperature-controlled furnace, pre-calcine at a low temperature from room temperature to 200°C for 0.5 hours, then increase the temperature at a rate of 5°C / min to 350°C, calcinate for 1.5 hours, and obtain nano Iron oxide red 100g.

Embodiment 3

[0027] Dissolve 200g of ferrous chloride in 1.8L of water, then add 1g of ferric citrine seeds and a little iron flakes, stir, and blow air into the reaction liquid below the liquid surface; dissolve 1.3kg of urea in 3.5L of water, add the urea aqueous solution dropwise To the reaction system, the dropwise addition is completed in 2 hours; continue to stir and pass in air for 2 hours, and stop stirring and ventilating when the pH value of the reaction system is 4 to 5; filter after standing, and dry at 105°C for 1 hour. After grinding, put it into a drum-type programmable temperature-controlled furnace, pre-calcine at a low temperature from room temperature to 200°C for 0.5 hours, then increase the temperature at a rate of 5°C / min to 350°C, and calcinate for 1.5 hours. After cooling down, 80g of nano-iron oxide red is obtained.

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Abstract

The invention discloses a method for producing nano-iron oxide red by using ferrous chloride recovered from waste pickling liquid in iron and steel plants, which comprises: mixing ferrous chloride aqueous solution with a mass ratio of 5-35%, clean iron flakes and iron yellow Put the crystal seeds into the reactor, control the reaction temperature at 10-40 degrees, and add the precipitant to the reactor; the stirring time is 0.5-5 hours, the stirring rate is 30-120 rpm, and the air flow rate is 2000-10000 into the reactor cubic meters per hour; wait for the reactant to turn into a khaki suspension, and stop the reaction when the pH value of the reaction system is between 4-5; through pressure filtration, drying, crushing and drum-type temperature-programmed calcination, nano-oxidized Iron oxide red.

Description

technical field [0001] The invention relates to the field of iron oxide red production methods, in particular to a method for producing nanometer iron oxide red from ferrous chloride recovered from waste pickling liquid. Background technique [0002] Ferrous chloride solution or ferrous chloride crystals can be obtained after concentrated treatment of hydrochloric acid pickling waste liquid in iron and steel plants. On the one hand, ferrous chloride is extremely easy to be oxidized under normal conditions, which makes it difficult to preserve a large amount of ferrous chloride; on the other hand, nano-iron oxide red has a stable structure and is widely used in pigments, paints, cosmetics, and catalytic materials And biomedicine and other fields, products with higher added value than ferrous chloride. The traditional production process of iron oxide red is usually prepared by adding acid to dissolve iron powder, and then oxidizing and adding alkali to precipitate. This proce...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09C1/24C01G49/06
Inventor 王育乔孙岳明施晓秋钱乐刘阳谭佃龙
Owner SOUTHEAST UNIV