CN104495952A - Preparation method of high-coercivity iron black for photocopy toner - Google Patents
Preparation method of high-coercivity iron black for photocopy toner Download PDFInfo
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- CN104495952A CN104495952A CN201510012216.4A CN201510012216A CN104495952A CN 104495952 A CN104495952 A CN 104495952A CN 201510012216 A CN201510012216 A CN 201510012216A CN 104495952 A CN104495952 A CN 104495952A
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- iron oxide
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Abstract
The invention discloses a preparation method of a high-coercivity iron black for a photocopy toner. The innovation point is that the preparation method comprises the following steps: adding ferrite yellow or iron red serving as a raw material into a ferrous sulfate solution; adjusting the pH value to be alkaline by using an alkali; and then performing high-temperature dehydration to synthesize the high-coercivity iron black. By virtue of prospect analysis and benefit forecast of the product prepared by the method disclosed by the invention, the performance of octahedron-shaped black ferroferric oxide magnetic powder is superior to that of cubical black ferroferric oxide magnetic powder (mainly in the aspect of high coercivity), the price of the octahedron-shaped black ferroferric oxide magnetic powder is also dominant, and if the octahedron-shaped black ferroferric oxide magnetic powder is put into production, the monopolization of ink iron black by foreign markets can be broken through, the economic and social benefits are huge, and the octahedron-shaped black ferroferric oxide magnetic powder produced by original factories of the cubical black ferroferric oxide magnetic powder by virtue of technical innovation can be put into production more quickly, so that the octahedron-shaped black ferroferric oxide magnetic powder has greater economic benefits and has the advantages reasonable process, simple method, environment-friendliness, energy conservation, low cost, good product quality, high utilization ratio of valuable components and the like.
Description
Technical field
The present invention relates to a kind of preparation method of photocopy toner high-coercive force iron oxide black, belong to mineral dye technical field.
Background technology
Black ferroferric oxide magnetic powder is important and application magneticsubstance very widely, and having the pigment performance of black and superior magnetic property, is indispensable main ingredient in photocopy toner (generally proportion is 25%-30% in ink powder).Ferroferric oxide magnetic powder possesses the performance of magneticsubstance and tinting material, mainly for the preparation of single component magnetic ink powder and the magnetic ink of duplicating machine, laser printer.For the application in this field, in granularity, form and aspect, size-grade distribution, magnetic property etc., higher requirement is proposed to ferroferric oxide magnetic powder.
The ferroferric oxide magnetic powder applied in photocopy toner has two kinds: octahedral bodily form particle (duplicating ink) and class spheroidal particle magnetic (Laser Printing ink).At home, the ferroferric oxide magnetic powder particle of production is cuboidal, rarely has the producer of octahedral bodily form ferroferric oxide magnetic powder, and (as Germany, the U.S.) existing production abroad, the black ferroferric oxide (Fe of therefore China's ink application
3o
4) magnetic is mainly by import.In China, the research iron black about wet-layer preparation high-coercive force ink powder is fewer.Zhang Xiaobo etc. have studied the iron black preparation technology of ink powder: mainly in the basic conditions, by treated technical grade ferrous sulfate and the sodium hydroxide method by oxidation precipitation, prepare suitable high-grade Z 250 (coercive force is 75Oe), mainly have studied feed way, system pH, air-blowing amount, blasting time and dispersion agent to the impact of product performance, to the synthesis of high-coercive force iron oxide black from now on, there is directive significance.But along with client requires more and more higher (requiring at more than 100Oe) to the coercive force of iron oxide black, this method requires too high to working condition, now can not meet the high-coercive force requirement of client in addition.So prepare under existing working condition, high-coercive force is iron black has important economic benefit and social effect to China's magneticsubstance production domesticization.
Summary of the invention
The object of the invention is to for deficiency of the prior art, a kind of preparation method of photocopy toner high-coercive force iron oxide black be provided, break abroad to the monopolization of ink iron oxide black, economic benefit and social benefit huge.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of photocopy toner high-coercive force iron oxide black, its innovative point is: with iron oxide yellow or iron oxide red for raw material, add copperas solution, regulate pH to alkalescence with bases, then high temperature dehydration, synthesis high-coercive force is iron black.
Further, described method concrete steps are as follows:
(1) material making beating: iron oxide red or iron oxide yellow are put into reaction container and thin up, stirs, and form suspension, be warming up to 60 ~ 90 DEG C, material enters next step;
(2) add copperas solution: in material obtained in the previous step, add copperas solution, stir, and keep material constant temperature to 60 ~ 90 DEG C, enter next step;
(3) neutralization is ferrous: in liquid phase material obtained in the previous step, add liquid base regulate pH to alkalescence, keep temperature to 60 ~ 90 DEG C, stir, form grey black precipitation, material enters next step;
(4) iron black synthesis: material, under high temperature, agitation condition, reacts 2 ~ 4 hours;
(5) aftertreatment: reaction terminates, by the iron oxide black for preparing through press filtration rinsing, two blade-tray drier series connection drying mode, 90 ~ 120 DEG C of oven dry, beats powder and fills and wrap.
Further, the suspended substance solid content formed in described step (1) is 8 ~ 15wt%.
Further, 1.6 ~ 2.0 times that ferrous sulfate amount is the middle iron oxide yellow of step (1) or iron oxide red quality are added in described step (2).
Further, described copperas solution concentration is 15 ~ 20wt%.
Further, in described step (1), (2), (3), (4), the mixing speed of stirring operation is set to 60 ~ 200r/min.
Further, in described step (3), liquid base is Na
2cO
3or NaOH solution or both are arbitrarily than mixture.
Further, in described step (3), liquid base regulates PH scope to be 9 ~ 13.
Further, the hot conditions in described step (4) is control temperature scope is 95 ~ 105 DEG C.
Reaction principle of the present invention is as follows:
Fe
2O
3+ FeSO
4+ 2NaOH → Fe
3O
4+ Na
2SO
4+ H
2O
Fe
2O
3+ FeSO
4+ Na
2CO
3→ Fe
3O
4 + Na
2SO
4+ CO
2↑
Beneficial effect of the present invention is as follows:
(1) product of the present invention analyzed by application prospect and effectiveness forecasting known, octahedral bodily form black ferroferric oxide magnetic powder is cube black ferroferric oxide magnetic powder excellent performance (mainly in high-coercive force) comparatively, price is also preponderated, if go into operation, iron black to ink monopolization can be broken abroad, economic benefit and social benefit huge, undergo technological transformation the producer of former cube shaped black ferroferric oxide magnetic powder the octahedral bodily form black ferroferric oxide magnetic powder produced, can put into production sooner, there is larger economic benefit.
(2) preparation method of the present invention adopts liquid phase method, with iron oxide red or the thick product of iron oxide yellow for raw material by Reactive Synthesis crystal formation again for regular octahedron and to have the photocopy toner of high-coercive force iron black, have rational technology, method simply, environmental protection and energy saving, cost low, good product quality, valuable constituent utilization ratio advantages of higher.
(3) the present invention is by traditional two blades-tray drier series connection drying mode applies in preparation method of the present invention, control 90 ~ 120 DEG C of appropriate bake out temperatures, product moisture content can be strict controlled within 2%, and the energy consumption consumed is 1/3 of oven drying, energy-conserving and environment-protective, meet modern production requirement.
(4) in preparation method of the present invention, by suitable control suspended substance solid content, add ferrous sulfate amount, copperas solution concentration, mixing speed, adjustment PH scope, the selection of Heating temperature and liquid base even, make octahedral bodily form black ferroferric oxide magnetic powder of the present invention have more excellent performance, economic worth is higher.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Fig. 2 is the SEM figure of product in embodiments of the invention 1.
Fig. 3 is the magnetic hysteresis loop figure of product in embodiments of the invention 1.
Fig. 4 is the SEM figure of product in embodiments of the invention 2.
Fig. 5 is the magnetic hysteresis loop figure of product in embodiments of the invention 2.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is elaborated.
Embodiment 1
The major equipment used is with the reaction container of whipping appts, steaming plant, liquid caustic soda bunkerage and drying plant.
A preparation method for high-coercive force iron oxide black, method steps is as follows:
(1) material making beating: iron oxide red is put into reaction container and thin up, stir, mixing speed is set to 60r/min, and form suspension, suspension vol is 40m
3, suspension solid content is 10wt%, and be then warming up to 60 DEG C, material enters next step; ;
(2) copperas solution is added: in material obtained in the previous step, add concentration is 20wt% copperas solution 36m
3, stir, mixing speed is set to 60r/min, and keeps temperature of charge to be 60 DEG C, enters next step;
(3) neutralization is ferrous: in liquid phase material obtained in the previous step, add 32wt%NaOH solution regulate pH to 12, stir, mixing speed is set to 60r/min, and form grey black precipitation, material enters next step;
(4) iron black synthesis: material is high temperature 100 DEG C and under agitation, mixing speed is set to 60r/min, reacts 4 hours;
(5) aftertreatment: reaction terminates, by the iron oxide black for preparing through press filtration rinsing, is then dried to 90 DEG C through two blade-tray drier, beats powder and fills and wrap.
The product of the present embodiment shows according to Fig. 2 scanning electron microscope: the crystal formation of sintetics is regular octahedron; The magnetic hysteresis loop figure of Fig. 3 tests: the coercive force of sample is 110Oe, meets the iron black standard of toner material.
Embodiment 2
Major equipment is with the reaction container of whipping appts, steaming plant, liquid caustic soda bunkerage and drying plant etc.
(1) material making beating: iron oxide yellow is put into reaction container and thin up, stir, mixing speed is set to 200r/min, and form suspension, volume is 30m
3, solid content is 15wt%, and be warming up to 60 DEG C, material enters next step;
(2) copperas solution is added: in material obtained in the previous step, add concentration is 20wt% copperas solution 45m
3, stir, mixing speed is set to 200r/min, and keeps temperature of charge to be 60 DEG C, enters next step;
(3) neutralization is ferrous: in liquid phase material obtained in the previous step, add 20wt%Na
2cO
3solution regulates pH to 10, and stir, mixing speed is set to 200r/min, and form grey black precipitation, material enters next step;
(4) iron black synthesis: material is high temperature 100 DEG C and under agitation condition, mixing speed is set to 200r/min, reacts 2 hours;
(5) aftertreatment: reaction terminates, by the iron oxide black for preparing through press filtration rinsing, is then dried to 120 DEG C through two blade-tray drier, beats powder and fills and wrap.
The product of the present embodiment shows according to Fig. 4 scanning electron microscope: the crystal formation of sintetics is regular octahedron; The magnetic hysteresis loop figure of Fig. 5 tests: the coercive force of sample is 99Oe, meets the iron black standard of toner material.
Embodiment 3
Major equipment is with the reaction container of whipping appts, steaming plant, liquid caustic soda bunkerage and drying plant etc.
(1) material making beating: iron oxide red is put into reaction container and thin up, stirs, and form suspension, volume is 30m
3, solid content is 10wt%, and be then warming up to 80 DEG C, material enters next step;
(2) copperas solution is added: in material obtained in the previous step, add concentration is 20wt% copperas solution 30m
3, stir and keep temperature of charge to be 60 DEG C, entering next step;
(3) neutralization is ferrous: in liquid phase material obtained in the previous step, add 20wt%NaOH solution regulate pH to 11, stir, and form grey black precipitation, material enters next step;
(4) iron black synthesis: material is high temperature 98 DEG C and under agitation condition, react 3 hours;
(5) aftertreatment: reaction terminates, by the iron oxide black for preparing through press filtration rinsing, is then dried to 105 DEG C through two blade-tray drier, beats powder and fills and wrap.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (9)
1. a photocopy toner preparation method for high-coercive force iron oxide black, is characterized in that: with iron oxide yellow or iron oxide red for raw material, add copperas solution, regulates pH to alkalescence, then high temperature dehydration with bases, and synthesis high-coercive force is iron black.
2. the preparation method of photocopy toner high-coercive force iron oxide black according to claim 1, is characterized in that: described method concrete steps are as follows:
(1) material making beating: iron oxide red or iron oxide yellow are put into reaction container and thin up, stirs, and form suspension, be warming up to 60 ~ 90 DEG C, material enters next step;
(2) add copperas solution: in material obtained in the previous step, add copperas solution, stir, and keep material constant temperature to 60 ~ 90 DEG C, enter next step;
(3) neutralization is ferrous: in liquid phase material obtained in the previous step, add liquid base regulate pH to alkalescence, keep temperature to 60 ~ 90 DEG C, stir, form grey black precipitation, material enters next step;
(4) iron black synthesis: material, under high temperature, agitation condition, reacts 2 ~ 4 hours;
(5) aftertreatment: reaction terminates, by the iron oxide black for preparing through press filtration rinsing, adopts two blade-tray drier series connection drying mode, 90 ~ 120 DEG C of oven dry, beats powder and fills and wrap.
3. the preparation method of photocopy toner high-coercive force iron oxide black according to claim 2, is characterized in that: the suspended substance solid content formed in described step (1) is 8 ~ 15wt%.
4. the preparation method of photocopy toner high-coercive force iron oxide black according to claim 2, is characterized in that: add 1.6 ~ 2.0 times that ferrous sulfate amount is the middle iron oxide yellow of step (1) or iron oxide red quality in described step (2).
5. the photocopy toner preparation method of high-coercive force iron oxide black according to claim 1,2 or 4, is characterized in that: described copperas solution concentration is 15 ~ 20wt%.
6. the preparation method of photocopy toner high-coercive force iron oxide black according to claim 2, is characterized in that: in described step (1), (2), (3), (4), the mixing speed of stirring operation is set to 60 ~ 200r/min.
7. the preparation method of photocopy toner high-coercive force iron oxide black according to claim 2, is characterized in that: in described step (3), liquid base is Na
2cO
3or NaOH solution or both are arbitrarily than mixture.
8. the preparation method of photocopy toner high-coercive force iron oxide black according to claim 2, is characterized in that: in described step (3), liquid base regulates PH scope to be 9 ~ 13.
9. the preparation method of photocopy toner high-coercive force iron oxide black according to claim 2, is characterized in that: the hot conditions in described step (4) is control temperature scope is 95 ~ 105 DEG C.
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| CN201510012216.4A CN104495952B (en) | 2015-01-09 | 2015-01-09 | A kind of preparation method of photocopy toner high-coercive force iron oxide black |
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| CN104495952B CN104495952B (en) | 2016-02-17 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4173624A (en) * | 1976-03-25 | 1979-11-06 | Bayer Aktiengesellschaft | Recovery of sodium sulphate in production of iron oxide black pigments |
| JPS5527813A (en) * | 1978-08-10 | 1980-02-28 | Jgc Corp | Manufacture of tri-iron tetroxide from iron polysulfate |
| CN86103643A (en) * | 1986-05-31 | 1987-12-09 | 天津市建新化工厂 | With steel melting furnace flue dust is the method for raw material production iron oxide black |
| CN1807263A (en) * | 2006-02-21 | 2006-07-26 | 上海宝齐氧化铁有限公司 | Method for producing iron oxide black using desilicified mud cake |
-
2015
- 2015-01-09 CN CN201510012216.4A patent/CN104495952B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4173624A (en) * | 1976-03-25 | 1979-11-06 | Bayer Aktiengesellschaft | Recovery of sodium sulphate in production of iron oxide black pigments |
| JPS5527813A (en) * | 1978-08-10 | 1980-02-28 | Jgc Corp | Manufacture of tri-iron tetroxide from iron polysulfate |
| CN86103643A (en) * | 1986-05-31 | 1987-12-09 | 天津市建新化工厂 | With steel melting furnace flue dust is the method for raw material production iron oxide black |
| CN1807263A (en) * | 2006-02-21 | 2006-07-26 | 上海宝齐氧化铁有限公司 | Method for producing iron oxide black using desilicified mud cake |
Non-Patent Citations (1)
| Title |
|---|
| 张伟: "低温水热法制备八面体四氧化三铁亚微米晶", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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