CN101412623A - Method for producing manganese-zinc ferrite particle from manganese-zinc ferrite waste material - Google Patents
Method for producing manganese-zinc ferrite particle from manganese-zinc ferrite waste material Download PDFInfo
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- CN101412623A CN101412623A CNA2008101435804A CN200810143580A CN101412623A CN 101412623 A CN101412623 A CN 101412623A CN A2008101435804 A CNA2008101435804 A CN A2008101435804A CN 200810143580 A CN200810143580 A CN 200810143580A CN 101412623 A CN101412623 A CN 101412623A
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Abstract
The invention provides a method for producing manganese-zinc ferrite granule materials by manganese-zinc ferrite waste materials, which comprises the following steps: making use of various waste materials, including waste devices and polishing waste materials, which are produced in the process of magnetic material processing as raw materials; performing reinforced leaching and reduction purification to obtain a qualified mixed solution containing major metallic ions; and performing the processes of coprecipitation, calcination, spraying granulation and the like to obtain high performance ferrite granule materials. The method is suitable for preparing high grade ferrite products. The method achieves a closed cycle of 'raw materials, products, wastes, and raw materials' in the magnetic material industry so that the utilization efficiency of resources are greatly improved; and at the same time, the production cost of the ferrite materials is reduced, and the market competitiveness of the products is improved.
Description
Technical field
The invention belongs to field of magnetic material, relate to a kind of method of utilizing Mn-Zn ferrite waste material production high-quality manganese-zinc ferrite particle material.
Background technology
Present technique comes from " coprecipitation method and direct method " technology, and its maximum characteristics are: 1. utilize the soft magnetism waste material to substitute " coprecipitation method " most raw metal, greatly reduce material cost; 2. utilize the raw mineral materials of soft magnetism waste material alternative " direct method ", improved the purity of raw material, shortened technical process.Therefore, this project both came from " coprecipitation method and direct method ", was higher than " coprecipitation method and direct method " again." coprecipitation method and direct method " all has plant-scale precedent at home, but because cost height, all operation suspension (as the super think of of Yibin, Sichuan Red River electronics and Chongqing).Raw material of the present invention adopts MnZn soft magnetism waste material, and coprecipitation method is adopted in the powder preparation, so the advantage on the existing above-mentioned two kinds of methods of project product, can avoid the high deficiency of its cost again.
Summary of the invention
The invention provides a kind of method of utilizing Mn-Zn ferrite waste material production high-quality manganese-zinc ferrite particle material.Comprise processes such as leaching, reduction, purification, co-precipitation, pre-burning, refining, batch mixing, mist projection granulating.The invention is characterized in: the magnetic core that will give up obtains leach liquor through powder or the polished waste material that crushing grinding obtains after vitriol intensified leaching, leach liquor obtains reduced liquid after the metal powder reduction, reduced liquid obtains qualified scavenging solution after a kind of scavenging agent purifies, in scavenging solution, add agricultural carbon ammonium and obtain coprecipitated starch, coprecipitated starch obtains the pre-burning powder after pre-burning, after the pre-burning powder is refining, obtain the fine ferrite particle material through batch mixing, mist projection granulating again.
Detailed process and parameter are:
During vitriol intensified leaching, vitriol oil consumption be theoretical amount 1.05-1.25 doubly, extraction temperature 80-120 ℃, extraction time 1.5-4.0h, the leaching yield of three kinds of principal constituents all reaches more than 95%.
Add a certain amount of iron powder, zinc powder and manganese powder successively according to the leach liquor composition during reduction, make the Fe in the leach liquor on the one hand
3+Restore All becomes Fe
2+, help follow-up scavenging process; Make principal constituent content meet theoretical prescription (the mole proportioning of iron, manganese, zinc is 68.29:16.57:15.14) on the other hand.In leach liquor, add iron powder reaction 1.0-2.0h earlier, add zinc powder reaction 0.5-1.0h again, add manganese powder reaction 0.5-1.0h at last, reduction temperature 60-90 ℃, Fe in the reduced liquid
3+Concentration is less than 1.0g/L, and the mole prescription of three kinds of principal constituents meets: Fe 67.5-70.5%, Mn 15.5-17.5%, Zn 14.5-16.5%.
Adding concentration during purification is the ammoniacal liquor of 1:1-1:3, and temperature is controlled to be 30-60 ℃, clarification time 2.0-5.0h, and pH is controlled to be 4.5-5.5, and purification can be removed impurity such as Si, Al more than 90%, Cr.
During co-precipitation, the bicarbonate of ammonia add-on is 1.1-1.5 a times of theoretical amount, and the pH value is controlled at 6.5-8.0, and the deposition rate of principal constituent ferrimanganic zinc is all more than 95%.
During coprecipitated starch pre-burning, because the wet method powder is active high, calcined temperature is lower than the calcined temperature of existing china-clay method, helps saving energy consumption, and concrete calcining system is:
Room temperature is to 400-450 ℃, temperature rise rate 10-12 ℃/min;
400-450 ℃ to 820-870 ℃, temperature rise rate 8-10 ℃/min;
820-870 ℃, soaking time 2.5-3.5h;
Keep equilibrium oxygen partial pres-sure to lower the temperature naturally.
The refining back of pre-burning powder Ca＜200ppm, Si＜60ppm, clearance Ca〉70%, Si〉50%, the content of other impurity elements is all extremely low, can obtain the fine ferrite particle material again behind batch mixing, mist projection granulating.
The advantage and the positively effect of invention:
1) because the raw material sources of present technique in industrial waste, will reduce the preparation cost of Ferrite Material greatly, promotes the competitiveness of product in market.
2) fully utilized the main body composition of magneticsubstance, eliminated useless magnetic core or polished waste material and stored up the problem of environmental pollution that causes, remarkable social benefit and environmental benefit have been arranged.
3) this technology can prepare the extremely low manganese-zinc ferrite particle material of foreign matter content by MnZn soft magnetism waste material, provides the foundation for preparing high performance Mn-Zn ferrite.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Embodiment 1
Of the present inventionly prepare the method for ferrite particle material, comprise processes such as leaching, reduction, purification, co-precipitation, pre-burning, refining, batch mixing, mist projection granulating with MnZn soft magnetism waste material.Specific embodiment is:
With the vitriol intensified leaching of MnZn soft magnetism waste material, vitriol oil consumption is 1.05 times of theoretical amount, extraction temperature 80-90 ℃, obtains leach liquor behind the leaching 4.0h.
Add iron powder, zinc powder and manganese powder successively and reduce in leach liquor, the iron powder add-on is about 20% of waste material quality, and zinc powder is about 10%, and manganese powder is about 2%.Reduction temperature 60-70 ℃, add iron powder reaction 2.0h earlier, add zinc powder reaction 1.0h again, add manganese powder reaction 1.0h at last.Fe in the reduced liquid
3+Concentration is 0.8g/L, and the mole formula rate of three kinds of principal constituents is: Fe 67.9%, and Mn 16.7%, and Zn 15.4%.
Add 1:1 ammoniacal liquor in reduced liquid, temperature is controlled to be 30-40 ℃, clarification time 5.0h, and pH is controlled to be 4.5-5.0.
During co-precipitation, the bicarbonate of ammonia add-on is 1.1 times of theoretical amount, and the pH value is controlled at 6.5-6.8, and the deposition rate of principal constituent is Fe 96.2%, and Mn 95.3%, and Zn 95.7%.。
With coprecipitated starch pre-burning, more on the low side relatively than traditional ceramics method, calcining system is:
Room temperature to 400 ℃, 10 ℃/min of temperature rise rate;
400 ℃ to 820 ℃, 8 ℃/min of temperature rise rate;
820 ℃, soaking time 3.5h;
Keep equilibrium oxygen partial pres-sure to lower the temperature naturally.
Principal constituent and foreign matter content after the pre-burning powder is refining the results are shown in Table 1.The high-purity Fe of impurity component and JFE
2O
3Quite, the element that has (as Cr) even lower.
Refined powder obtains ferrite particle material behind batch mixing, mist projection granulating, its physical performance index is: the pine dress compares 1.31g/cm
3, water ratio 0.3%, 28.6 ° of angles of repose, size distribution 60-180 order accounts for 87%, and the 60-100 order accounts for 42%.
Composition analysis result/the % of table 1 refined powder
| Fe 2O 3 | Mn 3O 4 | ZnO | Si | Al | Ca | Cr | Ni | SO 2 | P | |
| Sample 1 | 68.7 | 15.6 | 15. 5 | 0.00 65 | 0.00 61 | 0.02 | 0.00 04 | 0.0 1 | 0.02 4 | 0.01 1 |
| Sample 2 | 68.4 | 15.8 | 15. 6 | 0.00 51 | 0.00 55 | 0.01 7 | 0.00 04 | 0.0 1 | 0.02 5 | 0.01 |
| Sample 3 | 68.9 | 15.6 | 15. 3 | 0.00 53 | 0.00 57 | 0.01 8 | 0.00 04 | 0.0 1 | 0.02 6 | 0.01 |
| JFEFe 2O 3 | 99.5 8 | - | - | 0.00 59 | 0.00 58 | 0.00 9 | 0.00 1 | 0.0 1 | 0.03 | 0.00 1 |
Embodiment 2
Of the present inventionly prepare the method for ferrite particle material, comprise processes such as leaching, reduction, purification, co-precipitation, pre-burning, refining, batch mixing, mist projection granulating with MnZn soft magnetism waste material.Specific embodiment is:
With the vitriol intensified leaching of MnZn soft magnetism waste material, vitriol oil consumption is 1.15 times of theoretical amount, extraction temperature 95-105 ℃, obtains leach liquor behind the leaching 3.0h.
Add iron powder, zinc powder and manganese powder successively and reduce in leach liquor, the iron powder add-on is about 20% of waste material quality, and zinc powder is about 10%, and manganese powder is about 2%.Reduction temperature 70-80 ℃, add iron powder reaction 1.5h earlier, add zinc powder reaction 0.75h again, add manganese powder reaction 0.75h at last.Fe in the reduced liquid
3+Concentration is 0.6g/L, and the mole formula rate of three kinds of principal constituents is: Fe 68.3%, and Mn 16.6%, and Zn 15.1%.
Add 1:2 ammoniacal liquor in reduced liquid, temperature is controlled to be 40-50 ℃, clarification time 4.0h, and pH is controlled to be 4.7-5.2.
During co-precipitation, the bicarbonate of ammonia add-on is 1.2 times of theoretical amount, and the pH value is controlled at 6.9-7.2, and the deposition rate of principal constituent is Fe 97.6%, and Mn 96.7%, and Zn 96.9%.。
With coprecipitated starch pre-burning, calcining system is:
Room temperature to 420 ℃, 11 ℃/min of temperature rise rate;
420 ℃ to 850 ℃, 9 ℃/min of temperature rise rate;
850 ℃, soaking time 3.0h;
Keep equilibrium oxygen partial pres-sure to lower the temperature naturally.
Principal constituent and foreign matter content after the pre-burning powder is refining the results are shown in Table 1.The high-purity Fe of impurity component and JFE
2O
3Quite, the element that has (as Cr) even lower.
Refined powder obtains ferrite particle material behind batch mixing, mist projection granulating, its physical performance index is: the pine dress compares 1.33g/cm
3, water ratio 0.2%, 29.4 ° of angles of repose, size distribution 60-180 order accounts for 89%, and the 60-100 order accounts for 45%.
Embodiment 3
Of the present inventionly prepare the method for ferrite particle material, comprise processes such as leaching, reduction, purification, co-precipitation, pre-burning, refining, batch mixing, mist projection granulating with MnZn soft magnetism waste material.Specific embodiment is:
With the vitriol intensified leaching of MnZn soft magnetism waste material, vitriol oil consumption is 1.20 times of theoretical amount, extraction temperature 100-110 ℃, obtains leach liquor behind the leaching 2.0h.
Add iron powder, zinc powder and manganese powder successively and reduce in leach liquor, the iron powder add-on is about 20% of waste material quality, and zinc powder is about 10%, and manganese powder is about 2%.Reduction temperature 80-90 ℃, add iron powder reaction 1.0h earlier, add zinc powder reaction 0.5h again, add manganese powder reaction 0.5h at last., Fe in the reduced liquid
3+Concentration is 0.5g/L, and the mole formula rate of three kinds of principal constituents is: Fe 68.4%, and Mn 16.3%, and Zn 15.3%.
Add 1:3 ammoniacal liquor in reduced liquid, temperature is controlled to be 50-60 ℃, clarification time 3.0h, and pH is controlled to be 5.0-5.5.
During co-precipitation, the bicarbonate of ammonia add-on is 1.3 times of theoretical amount, and the pH value is controlled at 7.2-7.6, and the deposition rate of principal constituent is Fe 96.7%, and Mn 96.0%, and Zn 95.2%.。
With coprecipitated starch pre-burning, calcining system is:
Room temperature to 450 ℃, 12 ℃/min of temperature rise rate;
450 ℃ to 870 ℃, 10 ℃/min of temperature rise rate;
870 ℃, soaking time 2.5h;
Keep equilibrium oxygen partial pres-sure to lower the temperature naturally.
Principal constituent and foreign matter content after the pre-burning powder is refining the results are shown in Table 1.The high-purity Fe of impurity component and JFE
2O
3Quite, the element that has (as Cr) even lower.
Refined powder obtains ferrite particle material behind batch mixing, mist projection granulating, its physical performance index is: the pine dress compares 1.34g/cm
3, water ratio 0.4%, 28.9 ° of angles of repose, size distribution 60-180 order accounts for 86%, and the 60-100 order accounts for 40%.
Claims (7)
1, a kind of method with producing manganese-zinc ferrite particle from manganese-zinc ferrite waste material, it is characterized in that: the magnetic core that will give up obtains leach liquor through powder or the polished waste material that crushing grinding obtains after vitriol intensified leaching, leach liquor obtains reduced liquid after the metal powder reduction, reduced liquid is removed Si, Al, Cr impurity after ammoniacal liquor purifies, in scavenging solution, add agricultural carbon ammonium again and obtain coprecipitated starch, coprecipitated starch obtains the pre-burning powder after pre-burning, after the pre-burning powder is refining, obtain ferrite particle material through batch mixing, mist projection granulating again.
2, method of producing manganese-zinc ferrite particle material with waste material according to claim 1 is characterized in that: described Mn-Zn ferrite waste material is useless magnetic core and polished waste material.
3, method of producing manganese-zinc ferrite particle material with waste material according to claim 1, it is characterized in that: during vitriol intensified leaching, vitriol oil consumption be theoretical amount 1.05-1.25 doubly, extraction temperature 80-120 ℃, extraction time 1.5-4.0h, the leaching yield of three kinds of principal constituents is more than 95%.
4, method of producing manganese-zinc ferrite particle material with waste material according to claim 1 is characterized in that: add iron powder, zinc powder and manganese powder during reduction successively, and reduction temperature 60-90 ℃, recovery time 2.0-4.0h, Fe in the reduced liquid
3+Concentration is less than 1.0g/L, and the mole prescription of three kinds of principal constituents meets: Fe67.5-70.5%, Mn15.5-17.5%, Zn14.5-16.5%.
5, method of producing manganese-zinc ferrite particle material with waste material according to claim 1, temperature is controlled to be 30-60 ℃ when it is characterized in that purifying, clarification time 2.0-5.0h, pH is controlled to be 4.5-5.5, and purification can be removed Si, Al, the Cr impurity more than 90%.
6, method of producing manganese-zinc ferrite particle material with waste material according to claim 1, it is characterized in that: during co-precipitation, the bicarbonate of ammonia add-on is 1.1-1.5 a times of theoretical amount, and the pH value is controlled at 6.5-8.0, and the deposition rate of principal constituent ferrimanganic zinc is all more than 95%.
7, method of producing manganese-zinc ferrite particle material with waste material according to claim 1 is characterized in that the concrete pre-burning system of coprecipitated powder calcined temperature is:
Room temperature is to 400-450 ℃, temperature rise rate 10-12 ℃/min;
400-450 ℃ to 820-870 ℃, temperature rise rate 8-10 ℃/min;
820-870 ℃, soaking time 2.5-3.5h;
Keep equilibrium oxygen partial pres-sure to lower the temperature naturally.
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Cited By (9)
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| CN101912963A (en) * | 2010-08-26 | 2010-12-15 | 江苏省晶石磁性材料与器件工程技术研究有限公司 | Recovery method of magnetic material grinding scraps |
| CN102376442A (en) * | 2010-08-10 | 2012-03-14 | 张志明 | Method for producing current-resisting inductor by using waste materials |
| CN101921116B (en) * | 2009-06-11 | 2013-02-13 | 中山科成化纤有限公司 | Method for preparing high-conductivity granular material by using waste manganese-zinc ferrite |
| CN105060875A (en) * | 2015-08-19 | 2015-11-18 | 无锡斯贝尔磁性材料有限公司 | Thin film type MnZn ferrite magnetic material special powder |
| CN108484155A (en) * | 2018-04-11 | 2018-09-04 | 中南大学 | It is a kind of magnetic to inhale wave brick and preparation method thereof |
| CN109400144A (en) * | 2018-11-08 | 2019-03-01 | 安徽龙磁科技股份有限公司 | A method of high performance magnet is prepared with wet pressing permanent-magnet ferrite reclaimed materials |
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| CN109896849A (en) * | 2019-04-22 | 2019-06-18 | 南通冠优达磁业有限公司 | A kind of method that manganese-zinc ferrite grinding waste material prepares manganese-zinc ferrite |
| CN116875827A (en) * | 2023-07-12 | 2023-10-13 | 重庆上甲电子股份有限公司 | Method for preparing soft magnetic manganese zinc ferrite composite material by utilizing manganese-containing waste residues and zinc-containing waste residues generated in production of perillaldehyde |
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Cited By (12)
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| CN101921116B (en) * | 2009-06-11 | 2013-02-13 | 中山科成化纤有限公司 | Method for preparing high-conductivity granular material by using waste manganese-zinc ferrite |
| CN102376442A (en) * | 2010-08-10 | 2012-03-14 | 张志明 | Method for producing current-resisting inductor by using waste materials |
| CN102376442B (en) * | 2010-08-10 | 2016-02-03 | 张志明 | The method of the inductance of resistance to stream is manufactured with waste material |
| CN101912963A (en) * | 2010-08-26 | 2010-12-15 | 江苏省晶石磁性材料与器件工程技术研究有限公司 | Recovery method of magnetic material grinding scraps |
| CN105060875A (en) * | 2015-08-19 | 2015-11-18 | 无锡斯贝尔磁性材料有限公司 | Thin film type MnZn ferrite magnetic material special powder |
| CN108484155A (en) * | 2018-04-11 | 2018-09-04 | 中南大学 | It is a kind of magnetic to inhale wave brick and preparation method thereof |
| CN108484155B (en) * | 2018-04-11 | 2021-08-27 | 中南大学 | Magnetic wave-absorbing brick and preparation method thereof |
| CN109400144A (en) * | 2018-11-08 | 2019-03-01 | 安徽龙磁科技股份有限公司 | A method of high performance magnet is prepared with wet pressing permanent-magnet ferrite reclaimed materials |
| CN109835954A (en) * | 2019-03-21 | 2019-06-04 | 辽宁大学 | ZnMnO 3 Preparation method and application of nanoparticles |
| CN109896849A (en) * | 2019-04-22 | 2019-06-18 | 南通冠优达磁业有限公司 | A kind of method that manganese-zinc ferrite grinding waste material prepares manganese-zinc ferrite |
| CN116875827A (en) * | 2023-07-12 | 2023-10-13 | 重庆上甲电子股份有限公司 | Method for preparing soft magnetic manganese zinc ferrite composite material by utilizing manganese-containing waste residues and zinc-containing waste residues generated in production of perillaldehyde |
| CN116875827B (en) * | 2023-07-12 | 2024-03-15 | 重庆上甲电子股份有限公司 | Method for preparing soft magnetic manganese zinc ferrite composite material by utilizing manganese-containing waste residues and zinc-containing waste residues generated in production of perillaldehyde |
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Open date: 20090422 |