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Method of preparing high purity iron oxide for soft magnet using titanium white by product ferrous sulphate

A technology of ferrous sulfate and iron oxide, applied in the directions of iron oxide, iron oxide/iron hydroxide, etc., can solve the problems of inability to reduce production cost, low yield, and lack of high-magnesium raw materials, so as to solve the problems of pollution and utilization , The effect of reducing production costs and retaining product activity

Inactive Publication Date: 2006-09-13
广西冶金研究院有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the method provided by the Chinese patent application "Refinement process of ferrous sulfate by-product of titanium dioxide" (application number 94105891), although the purification effect of titanium impurities is good, manganese and magnesium can hardly be removed
Chinese patent "preparation method of iron oxide red for soft ferrite" (patent No. 00139210) is to add inhibitors in the synthesis stage, so that metal ions such as magnesium remain in the mother liquor and filter out magnesium, but the used raw material magnesium content of this patent is only It is 0.20%, and there is no example of preparation with high-magnesium raw materials, and there is no indication that it has an effect on the removal of manganese, and the index of manganese content is not provided
Chinese patent application "a preparation method of iron oxide red powder" (application number 03150766) has done special research on manganese removal, by adding manganese removal agent to achieve the purpose of manganese removal, but this method is relatively difficult in precipitation washing, SO 4 2- It is difficult to clean, and the product after spray burning needs to go through a series of processes to remove SO 4 2- , and the production rate of the pilot test is low, only 15 kg of product is produced per cubic meter, and the production cost cannot be reduced
So far, there is no method report with significant effect on the removal of manganese and magnesium

Method used

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  • Method of preparing high purity iron oxide for soft magnet using titanium white by product ferrous sulphate
  • Method of preparing high purity iron oxide for soft magnet using titanium white by product ferrous sulphate
  • Method of preparing high purity iron oxide for soft magnet using titanium white by product ferrous sulphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Add 2.2 liters of deionized water into a 3-liter beaker, add green vitriol 1200g while stirring, and use a small amount of chemically pure concentrated H 2 SO 4 Adjust the pH value of the solution to 2.0, add 12g of iron filings, heat to about 80°C, and keep stirring for 4 hours. Then add 350ml of deionized water to dilute and lower the temperature, then add 200ml of 0.05% polyacrylamide, stir for 2-5 minutes and then let stand for 2-3 hours. After filtration, 3L of clear and transparent green ferrous sulfate solution was obtained, and the filtrate contained Fe 73g / L. The impurity content before and after purification is shown in Table 1:

[0042] Main impurities (%)

Embodiment 2

[0044] Add 1200ml of the ferrous sulfate solution after the purification of Example 1 into a 3-liter beaker, stir at room temperature at 25°C and slowly add dropwise the neutralizing solution 500ml containing ammonium bicarbonate 23g and strong ammonia water 23ml, then heat to 60°C, Air was oxidized for 3.5 hours, and the final pH value was controlled to be 4.5. Then add dropwise the neutralizing solution 800ml containing 100g ammonium bicarbonate and 100ml strong ammonia water while oxidizing, the oxidation time is 6 hours, the terminal pH value is 6.8, stop oxidation and heating, continue to stir for 30 minutes and leave standstill for 2 hours. Then filter, wash with deionized water to wash with 1% BaCl 2 Solution detects no SO 4 2- The precipitate was baked in an oven at 100°C for 2 to 3 hours, and then moved to a muffle furnace for calcination at 680°C for 2 hours to obtain 115g of iron oxide. The Fe yield was 91.9%. The sample analysis results are shown in Table 2 [Mi...

Embodiment 3

[0046] Add 1200ml of the ferrous sulfate solution purified in Example 1 into a 3-liter beaker, heat to 60°C, stir and slowly add 550ml of neutralizing solution containing 30g of ammonium bicarbonate and 30ml of concentrated ammonia water dropwise, heat up to 70°C, and pass Air oxidation was carried out for 3.5 hours, and the final pH value was controlled at 4.0. Add dropwise 750ml of neutralizing solution containing 98g of ammonium bicarbonate and 98ml of strong ammonia water while oxidizing, the oxidation time is 7 hours, and the terminal pH value is 7.5. Stop oxidation and heating, stir for 30min and let stand for 2 hours. Then filter and wash with deionized water until SO-free 4 2- The precipitate was dried in an oven at 100°C for 2-3 hours, and then moved to a muffle furnace for calcination at 720°C for 2 hours to obtain 114g of iron oxide product with a Fe yield of 91.1%. See Table 2 for sample analysis.

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Abstract

A process for preparing the high-purity iron oxide used as soft-magnetic material from the copperas, which is the by-product of Ti white powder, and ferrous sulfate includes such steps as removing impurities, two-step neutralizing, two-step oxidizing to obtain Fe3O4, filtering, baking and calcining. The technological parameters for said neutralizing and oxidizing steps are also disclosed.

Description

technical field [0001] The invention belongs to the technical field of soft magnetic material production, in particular to a method for preparing high-purity iron oxide for soft magnetic use by using ferrous sulfate as a by-product of titanium white. Background technique [0002] Soft ferrite is an important basic material in the electronics industry, and iron oxide accounts for about 70% of its composition. my country's soft ferrite production has maintained rapid growth since 1990. At present, the main method of producing iron oxide for soft magnetic is the Ruthner method, which is the spray roasting method. This method is suitable for the hydrochloric acid system, and the raw material is the pickling waste liquid of the rolling mill. The advantages of this method are large output and relatively low cost, but it is difficult to produce high-grade Therefore, most of the iron oxide produced by this method is used for medium and low-grade ferri...

Claims

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Application Information

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IPC IPC(8): C01G49/06
Inventor 侬健桃黄瀚韦世强
Owner 广西冶金研究院有限公司
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