CN1554712A - Preparation method of zinc ferrite pigment powder - Google Patents
Preparation method of zinc ferrite pigment powder Download PDFInfo
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- CN1554712A CN1554712A CNA2003101106950A CN200310110695A CN1554712A CN 1554712 A CN1554712 A CN 1554712A CN A2003101106950 A CNA2003101106950 A CN A2003101106950A CN 200310110695 A CN200310110695 A CN 200310110695A CN 1554712 A CN1554712 A CN 1554712A
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- zinc ferrite
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Abstract
The invention relates to a preparation method of zinc ferrite pigment powder. The present invention features that metal iron powder and zinc powder are used as raw material and are directly rusted and oxidized in low temperature (less than 100 deg.c) water medium system to prepare yellowish brown zinc ferrite color powder. The process flow is simple, the pigment powder has good uniformity and dispersibility, and the content of harmful impurities such as chlorine is low, so the pigment is an environment-friendly pigment.
Description
Technical field: the present invention relates to the inorganic pigment powder preparation field, especially the preparation method of pigment of zinc ferrite powder.
Technical background: zinc ferrite is spinel structure, is a kind of important magneticsubstance and catalyzer, also is a kind of good sweetening agent and rust-stabilising pigment simultaneously.As mineral dye, it has advantages such as heat-resisting, fast light, nontoxic, that rustless property is strong, is the ideal substitute of poisonous rust-stabilising pigments such as zinc-chrome yellow.
The traditional synthetic method of zinc ferrite is the elevated temperature heat chemosynthesis, after soon high-purity zinc oxide and brown iron oxide will mix in proportion, roasting under 900～1100 ℃ of high temperature, make it that solid phase thermal chemical reaction take place, cool off fragmentation then and obtain the zinc ferrite powder, this method technology is simple, but long reaction time, the energy consumption height, product granularity is big.For shortening the reaction times, people's villaumite commonly used is made catalyzer, and with fast reaction speed, but the chloride zinc ferrite powder corrosion resistance that makes reduces, thereby is not suitable for use in anti-corrosion paint.At this problem, U.S. Pat 2904395 reports are used in oxidation divalent iron salt in zinc oxide or the zinc subcarbonate suspension, and the ZnO-FeOOH that obtains is promptly as the roasting raw material, and high-temperature roasting obtains fine ferrous acid zinc powder then.This method can significantly improve the raw material activity, and reduces product granularity, but its precipitation temperature requires strict (49～52 ℃) especially, and is low slightly or high slightly all not all right.According to US4681637, adopt the alpha-feooh that newly obtains to mix with ZnO, and add compounds such as 0.1%～1% boric acid, borophosphoric acid and react at 700～1000 ℃ of roasting temperatures, cool off ore grinding then fast, the ultra-fine zinc ferrite powder that can not contained Cl-, but it is high that this technology requires the raw material alpha-feooh, and long flow path, the energy consumption height.
The liquid phase chemical coprecipitation method is the another kind of zinc ferrite synthetic method that people use always, it comprises that chemical coprecipitation is produced precursor and two big steps are decomposed in the presoma roasting, specifically be to be raw material with soluble Zn, molysite, add up to precipitation agent with carbonate, oxalic acid, at first make the tiny basic carbonate of crystal grain, oxalate precursor, precursor is decomposed in roasting under comparatively high temps then, finally obtains the zinc ferrite powder.It is thin, active high that this method obtains product granularity, but technical process is long, the production cost height, and the acid-base neutralisation environmental issue is serious in the process.In addition, the zinc ferrite synthetic method of people's research and development also has the synthetic and sol-gel method of mechanochemistry, and all because of the technology more complicated, the cost height is difficult to carry out industrialization.
Summary of the invention: the objective of the invention is to propose a kind of acid dissolving that need not add, also needn't add precipitation agent, technical process is simply with the synthetic preparation method who produces the pigment of zinc ferrite powder of the direct liquid phase corrosion of metal powder oxidation.
Technical solution of the present invention is with metal iron powder, zinc powder is a raw material, with granularity less than 50 purpose metal iron powders and zinc powder be by weight percentage 60～67%: 33～40% prepare burden mixed after, compound is joined ball milling in the ball mill, 0.5～3 hour ball milling time, material thin up behind the ball milling, solid-to-liquid ratio 1: 8～20, add salt 5～100 grams per liters, the pH value of solution value is 4.0～9.0, bubbling air or pure oxygen, flow of oxygen is 0.2～2.0 liter/minute, temperature of reaction is room temperature～100 ℃, 700～2000 rev/mins of stirring velocitys, 24～48 hours reaction times, form zinc ferrite suspension, through clarification, washing, drying makes the pigment of zinc ferrite powder.
The salt of above-mentioned interpolation can be one or more in the non-villaumite of iron, zinc, ammonium.
The present invention compared with prior art, it is long to have broken through traditional elevated temperature heat chemosynthesis reaction time, powder size is thick, simultaneously overcomes the chemical coprecipitation long flow path again, and problems such as a large amount of by-product abraum salt solution generation are arranged.The present invention is a raw material with the metal, the synthetic pigment of zinc ferrite powder of direct reaction in the aqueous solution.Its product component is even, fine size, and not chloride, antirust ability is strong, and technical process is simple, and the reaction times is short, and cost is low, reduced investment, operational condition is good.
The pigment of zinc ferrite powder physical and chemical performance such as the table 1 of the present invention's preparation:
Table 1 ZnFe
2O
4The typical physical chemical property
Zn％ 31.0～35.0％
Fe
2O
3％ 65.0～69.0％
Cl
-％ 0.0005％
Particle diameter μ m＞325 orders＜0.05%
Color: tawny
Specific embodiment: embodiment 1 is with metal iron powder, zinc powder (%) batch mixes of 64: 36 by weight percentage, ball milling 120 minutes, and corrosion oxidation in the 2L reactive tank, the corrosion oxidizing condition is solid-to-liquid ratio 1: 10, (NH
4)
2SO
420 grams per liters, 10 liters/min of bubbling air amount, 80 ℃ of temperature of reaction, stirring velocity are 1000 rev/mins, in 36 hours reaction times, the after scouring drying is finished in reaction, promptly gets the tawny ZnFe of homogeneous grain diameter
2O
4The pigment powder.
Embodiment 2 is with (%) proportion ingredient of 60: 40 mixing by weight percentage of metal iron powder, zinc powder, and ball milling 40 minutes carries out the corrosion oxidation then in the 2L reactive tank, and the corrosion oxidizing condition is solid-to-liquid ratio 1: 12, ZnSO
410 grams per liters, feeding the pure oxygen amount is 1 liter/min, and 80 ℃ of temperature of reaction, stirring velocity are 1200 rev/mins, and in 30 hours reaction times, after reaction was finished, washing was drying to obtain the tawny ZnFe of homogeneous grain diameter
2O
4The pigment powder.
Claims (5)
1. the preparation method of a pigment of zinc ferrite powder, it is characterized in that: with granularity less than 50 purpose metal iron powders and zinc powder be respectively by weight percentage 60～67% and 33～40% prepare burden mixed, after the ball milling activation, thin up, the corrosion oxidation, form zinc ferrite suspension, make the pigment of zinc ferrite powder through clarification, washing, drying.
2. the preparation method of pigment of zinc ferrite powder according to claim 1 is characterized in that: ball milling activation is that the compound with iron powder and zinc powder joins ball milling in the ball mill, 0.5～3 hour ball milling time.
3. the preparation method of pigment of zinc ferrite powder according to claim 1, it is characterized in that: the condition of corrosion oxidation is: solid-to-liquid ratio 1: 8～20, add salt 5～100 grams per liters, the pH value of solution value is 4.0～9.0, the flow of oxygen of oxygenant is 0.2～2.0 liter/minute, temperature of reaction is room temperature～100 ℃, 700～2000 rev/mins of stirring velocitys, 24～48 hours reaction times.
4. according to the preparation method of claim 1 or 3 described pigment of zinc ferrite powders, it is characterized in that: add salt and can be in the non-villaumite of iron, zinc, ammonium one or more.
5. according to the preparation method of claim 1 or 3 described pigment of zinc ferrite powders, it is characterized in that: what the oxygenant of corrosion oxidizing reaction can be in air, the pure oxygen is any.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200310110695 CN1220734C (en) | 2003-12-23 | 2003-12-23 | Preparation method of zinc ferrite pigment powder |
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| CN 200310110695 CN1220734C (en) | 2003-12-23 | 2003-12-23 | Preparation method of zinc ferrite pigment powder |
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| CN1554712A true CN1554712A (en) | 2004-12-15 |
| CN1220734C CN1220734C (en) | 2005-09-28 |
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| CN 200310110695 Expired - Fee Related CN1220734C (en) | 2003-12-23 | 2003-12-23 | Preparation method of zinc ferrite pigment powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100389154C (en) * | 2006-03-24 | 2008-05-21 | 昆明理工大学 | Method for preparing pigment of zinc ferrite |
| CN101020792B (en) * | 2006-11-24 | 2012-01-11 | 中国石油化工股份有限公司中原油田分公司采油工程技术研究院 | Process of preparing rubber filler with oil-bearing sludge |
| CN1821313B (en) * | 2005-01-25 | 2012-11-14 | 朗盛德国有限责任公司 | Zinc-ferrit pigments stable against reduction, method for making and use of said pigments |
| CN108358604A (en) * | 2018-03-29 | 2018-08-03 | 广西钦州市品艺堂坭兴陶有限公司 | The production method of colored Nixing pottery |
| CN115572494A (en) * | 2022-09-27 | 2023-01-06 | 佛山市三水区康立泰无机合成材料有限公司 | Red-brown ceramic pigment, preparation method thereof and application of red-brown ceramic pigment in ceramic ink-jet printing ink |
-
2003
- 2003-12-23 CN CN 200310110695 patent/CN1220734C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1821313B (en) * | 2005-01-25 | 2012-11-14 | 朗盛德国有限责任公司 | Zinc-ferrit pigments stable against reduction, method for making and use of said pigments |
| CN100389154C (en) * | 2006-03-24 | 2008-05-21 | 昆明理工大学 | Method for preparing pigment of zinc ferrite |
| CN101020792B (en) * | 2006-11-24 | 2012-01-11 | 中国石油化工股份有限公司中原油田分公司采油工程技术研究院 | Process of preparing rubber filler with oil-bearing sludge |
| CN108358604A (en) * | 2018-03-29 | 2018-08-03 | 广西钦州市品艺堂坭兴陶有限公司 | The production method of colored Nixing pottery |
| CN108358604B (en) * | 2018-03-29 | 2021-04-20 | 广西钦州市品艺堂坭兴陶有限公司 | Manufacturing method of colored nixing pottery |
| CN115572494A (en) * | 2022-09-27 | 2023-01-06 | 佛山市三水区康立泰无机合成材料有限公司 | Red-brown ceramic pigment, preparation method thereof and application of red-brown ceramic pigment in ceramic ink-jet printing ink |
| CN115572494B (en) * | 2022-09-27 | 2024-02-02 | 佛山市三水区康立泰无机合成材料有限公司 | Red brown ceramic pigment, preparation method thereof and application thereof in ceramic inkjet printing ink |
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| CN1220734C (en) | 2005-09-28 |
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Granted publication date: 20050928 Termination date: 20100125 |