CN1837065A - Process for preparing quasi-spherical black ferroferric oxide magnetic powder - Google Patents
Process for preparing quasi-spherical black ferroferric oxide magnetic powder Download PDFInfo
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- CN1837065A CN1837065A CN 200610013524 CN200610013524A CN1837065A CN 1837065 A CN1837065 A CN 1837065A CN 200610013524 CN200610013524 CN 200610013524 CN 200610013524 A CN200610013524 A CN 200610013524A CN 1837065 A CN1837065 A CN 1837065A
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Abstract
The invention discloses a Method for preparation of quasi sphericity black ferriferrous oxide magnetic powder, belonging to the compositing technique of magnetic powder. This method containing steps as follows: mixing the ferrisulphas and ferric persulfate according to mol ratio as 1:0-0.8 and adding water mill to dissolve, and then heating-up adding sodium carbonate solution, or blowing air and adjusting Ph value as 7-9 by caustic lye of soda, in order to forming bubble chamber microenvironment and making precipitate slurry in this environment, making the precipitate slurry in bubble chamber microenvironment, 70-95 Deg C, pH value 9-12 doing reaction to crystallization, after water filtration, drying,comminuting, getting quasi sphericity black ferriferrous oxide magnetic powder. The advantage of this invention is lies in: forming given bubble chamber microenvironment by controlling condition in synthesize course, in order to reach the purpose of controlling the appearance of magnetic powder as quasi sphericity. The method is simple, the cost is low, the products' appearance is quasi sphericity, the granularity is quite equal, the mean particle diameter is 50-200nm.
Description
Technical field
The present invention relates to a kind of preparation method of quasi-spherical black ferroferric oxide magnetic powder, belong to the synthetic technology of magnetic.
Background technology
Black ferroferric oxide magnetic powder is important and uses very wide magneticsubstance, it is one of main raw material (utilizing its black and magnetic) of producing photocopy toner, producing high-grade ink powder requirement is raw material with comparatively high-grade magnetic, and the particle morphology of magnetic, size-grade distribution, magnetic property etc. are all had higher requirement.
According to different requirements, the ferroferric oxide magnetic powder of using in the photocopy toner has two kinds: cube particle and class spheroidal particle magnetic.The ferroferric oxide magnetic powder of domestic production mostly is the product of cube particle, and the quasi-spherical black ferroferric oxide magnetic powder that the also producer of the spherical ferroferric oxide magnetic powder of not production class, so China uses is by import.
The traditional preparation method of ferroferric oxide magnetic powder mostly is direct synthesis technique greatly, be ferric oxide and ferrous hydroxide (ferrous sulfate and sodium hydroxide solution reaction form), under certain temperature and pH value, directly carry out the method for addition reaction, starting raw material ferric oxide, ferrous sulfate and sodium hydroxide.The method of also useful ferrous hydroxide oxidation is carried out synthetic, starting raw material ferrous sulfate and sodium hydroxide.The particle of traditional prepared ferroferric oxide magnetic powder of preparation method is cuboidal, and granularity is even inadequately, does not therefore have preferably and stable magnetic particle capability.Class spheroidal particle magnetic has high-performances such as good fluidity, but the spherical ferroferric oxide magnetic powder of class only minority developed country (as Germany, the U.S. etc.) production is arranged, and because synthetic method is comparatively complicated, price is more expensive, so can't be commonly used.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of quasi-spherical black ferroferric oxide magnetic powder, it is simpler that this method has production technique, and be class spheric characteristics by bubble-chamber microenvironment control magnetic particle.
The present invention is realized by following technical proposals.A kind of preparation method of quasi-spherical black ferroferric oxide magnetic powder is characterized in that may further comprise the steps:
1. be 1 with ferrous sulfate and ferric sulfate by the ratio of amount of substance: (0～0.8) mixing and water adding stirring and dissolving obtains mixing solutions;
2. step 1 gained mixing solutions is warming up to 40～70 ℃, add sodium carbonate solution generation bubble precipitin reaction takes place simultaneously, this moment, the pH value of solution value was 7～9, or evenly blast air reaction and be 7～9 with the sodium hydroxide solution adjust pH, with formation bubble-chamber microenvironment and in this environment, make the throw out slurry;
3. in the prepared throw out slurry of step 2, continue to blast air, and make it in the bubble-chamber microenvironment that forms, to react crystallization, crystallization temperature is controlled to be 70～95 ℃, and is 9～12 with sodium hydroxide solution control pH value, is incubated still aging 2 hours, slurry and clear liquid are separated, and the washing slurry, filtration under diminished pressure, 50～60 ℃ of oven dry, put into the mortar porphyrize, obtain quasi-spherical black ferroferric oxide magnetic powder.
The invention has the advantages that: only by the CONTROL PROCESS condition, forming specific bubble-chamber microenvironment in the building-up process, is class spheric purpose to reach control magnetic particle morphology.This method is simpler, and raw materials cost is lower, and the product pellet pattern is the class sphere, and granularity is more even, and median size is 50～200nm.
Description of drawings
Fig. 1 is the TEM photo of the embodiment of the invention 1 products made thereby.
Embodiment
Embodiment 1:
Take by weighing 216 gram ferrous sulfate and 156 gram ferric sulfate, add the water stirring and dissolving and obtain mixing solutions; Adding sodium carbonate solution when being warming up to 40 ℃ in mixed molysite solution, to make pH value be 8, produces bubble precipitin reaction takes place simultaneously, must the throw out slurry; Blast air this moment, continues to be warming up to 80 ℃, adds 3molL
-1Sodium hydroxide solution to pH value be 11, react crystallization process, be incubated still aging 2 hours, with slurry and clear liquid separately, and the washing slurry, filtration under diminished pressure, the mortar porphyrize is put in 55 ℃ of oven dry, obtains product, productive rate 92%; The product median size is 100nm, and specific saturation magnetization is 90emu/g, and coercive force is 80Oe, and remanent magnetism is 6emu/g.
Embodiment 2:
Take by weighing 216 gram ferrous sulfate and 22 gram ferric sulfate, add the water stirring and dissolving and obtain mixing solutions; Adding sodium carbonate solution when being warming up to 40 ℃ in mixed molysite solution, to make pH value be 8, produces bubble precipitin reaction takes place simultaneously, must the throw out slurry; Blast air this moment, continues to be warming up to 80 ℃, adds 3molL
-1Sodium hydroxide solution to pH value be 11, react crystallization process, be incubated still aging 2 hours, with slurry and clear liquid separately, and the washing slurry, filtration under diminished pressure, the mortar porphyrize is put in 55 ℃ of oven dry, obtains product, productive rate 92%; The product median size is 120nm, and specific saturation magnetization is 95emu/g, and coercive force is 900e, and remanent magnetism is 10emu/g.
Embodiment 3:
Take by weighing 216 gram ferrous sulfate, add the water stirring and dissolving and obtain solution; Blast air when being warming up to 70 ℃, and use 3molL
-1The pH value of sodium hydroxide solution regulator solution be 9, precipitin reaction takes place in bubbling simultaneously, the throw out slurry; Continue to blast air, and be warming up to 80 ℃, add 3molL
-1NaOH solution to pH value be 11, react crystallization process, be incubated still aging 2 hours, with slurry and clear liquid separately, and the washing slurry, filtration under diminished pressure, the mortar porphyrize is put in 55 ℃ of oven dry, obtains product, productive rate 92%; The product median size is 150nm, and specific saturation magnetization is 95emu/g, and coercive force is 100Oe, and remanent magnetism is 12emu/g.
Claims (1)
1. the preparation method of a quasi-spherical black ferroferric oxide magnetic powder is characterized in that may further comprise the steps:
1). is 1 with ferrous sulfate and ferric sulfate by the ratio of amount of substance: (0～0.8) mixing and water adding stirring and dissolving obtains mixing solutions;
2). step 1) gained mixing solutions is warming up to 40～70 ℃, add sodium carbonate solution generation bubble precipitin reaction takes place simultaneously, this moment, the pH value of solution value was 7～9, or evenly blast air reaction and be 7～9 with the sodium hydroxide solution adjust pH, with formation bubble-chamber microenvironment and in this environment, make the throw out slurry;
3). with step 2) the throw out slurry that makes continues to blast air, and make it in the bubble-chamber microenvironment that forms, to react crystallization, crystallization temperature is controlled at 70～95 ℃, and is 9～12 with sodium hydroxide solution control pH value, is incubated still aging 2 hours, slurry and clear liquid are separated, and the washing slurry, filtration under diminished pressure, 50～60 ℃ of oven dry, put into the mortar porphyrize, obtain quasi-spherical black ferroferric oxide magnetic powder.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB200610013524XA CN100453470C (en) | 2006-04-24 | 2006-04-24 | Process for preparing quasi-spherical black ferroferric oxide magnetic powder |
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| CNB200610013524XA CN100453470C (en) | 2006-04-24 | 2006-04-24 | Process for preparing quasi-spherical black ferroferric oxide magnetic powder |
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| CN1837065A true CN1837065A (en) | 2006-09-27 |
| CN100453470C CN100453470C (en) | 2009-01-21 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633308A (en) * | 2012-05-19 | 2012-08-15 | 河南佰利联化学股份有限公司 | Method for producing iron oxide black by ferrous sulfate mother liquor |
| CN104140127A (en) * | 2013-05-09 | 2014-11-12 | 中国科学院过程工程研究所 | Method for producing ferriferrous oxide by using ferric oxide as raw material |
| CN104261486A (en) * | 2014-09-19 | 2015-01-07 | 上海一品颜料有限公司 | Method for controlling content of iron of black iron oxide |
| CN107673410A (en) * | 2017-10-19 | 2018-02-09 | 兰州城市学院 | The method that nano ferriferrous oxide is prepared using industrial ferrous contained waste liquid |
| CN109133450A (en) * | 2018-08-10 | 2019-01-04 | 天津城建大学 | A method of iron oxide black pigment is prepared using steel pickling waste liquor |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62128926A (en) * | 1985-11-30 | 1987-06-11 | Toda Kogyo Corp | Production of magnetic iron oxide grain powder having spindle type |
| CN1014511B (en) * | 1988-07-30 | 1991-10-30 | 北京理工大学 | Preparation for submicron particle of ferriferous oxide |
-
2006
- 2006-04-24 CN CNB200610013524XA patent/CN100453470C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633308A (en) * | 2012-05-19 | 2012-08-15 | 河南佰利联化学股份有限公司 | Method for producing iron oxide black by ferrous sulfate mother liquor |
| CN104140127A (en) * | 2013-05-09 | 2014-11-12 | 中国科学院过程工程研究所 | Method for producing ferriferrous oxide by using ferric oxide as raw material |
| CN104140127B (en) * | 2013-05-09 | 2015-09-30 | 中国科学院过程工程研究所 | A kind of take ferric oxide as the method for raw material production Z 250 |
| CN104261486A (en) * | 2014-09-19 | 2015-01-07 | 上海一品颜料有限公司 | Method for controlling content of iron of black iron oxide |
| CN107673410A (en) * | 2017-10-19 | 2018-02-09 | 兰州城市学院 | The method that nano ferriferrous oxide is prepared using industrial ferrous contained waste liquid |
| CN109133450A (en) * | 2018-08-10 | 2019-01-04 | 天津城建大学 | A method of iron oxide black pigment is prepared using steel pickling waste liquor |
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| CN100453470C (en) | 2009-01-21 |
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Granted publication date: 20090121 Termination date: 20110424 |