CN102604437B - Intermediate temperature-resistant coated iron oxide black and preparation method thereof - Google Patents
Intermediate temperature-resistant coated iron oxide black and preparation method thereof Download PDFInfo
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- CN102604437B CN102604437B CN201210038252.4A CN201210038252A CN102604437B CN 102604437 B CN102604437 B CN 102604437B CN 201210038252 A CN201210038252 A CN 201210038252A CN 102604437 B CN102604437 B CN 102604437B
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Abstract
The invention relates to a temperature resistant iron oxide black and a preparation method thereof, in particular to an intermediate temperature-resistant coated iron oxide black which comprises iron oxide black as a main component, wherein iron oxide black is coated with multiple additive coating layers and iron oxide black and the multiple additive coating layers are combined to form a pigment with films. The multiple coating layers are formed in the way that pH value of compounds containing aluminum ions and silicon ions is regulated so that aluminum ions and silicon ions precipitate in sequence and gradually coat the surface of iron oxide black molecules to form multiple protective films. The iron oxide black prepared by the method disclosed by the invention has good high temperature resistance; and the coated pigment contains uniform ions and has high strength and excellent dispersibility. The invention also discloses a preparation method of the intermediate temperature-resistant coated iron oxide black.
Description
Technical field
The present invention relates to a kind of heatproof iron oxide black and preparation method thereof.
Background technology
Iron oxide black is called for short iron black molecular formula, Fe
2o
3.FeO, chemical name Z 250, belongs to spinel type, and it has saturated indigo plant China ink light black, and relative density is 4.73.Its opacifying power and tinting strength are all very high, very stable to the effect of light and atmosphere.Poor because of the heat resistance of common iron oxide black, heating temperature is in 100 about degree, under some have the occasion of temperature, uses, the phenomenon such as variable color will occur, fade.
Common iron oxide black production method, as Chinese invention patent application (application number: 200510075112.4 applyings date: 2005-06-08) discloses a kind of production method of iron oxide black, comprises following content: (1), make perferrite solution; (2), with caustic soda, make neutralizing agent and react generation ferrous hydroxide with perferrite solution; (3), make oxygenant with oxygen-containing gas, generate iron black with above-mentioned hydroxide iron oxidation reaction; (4), sieved in the iron oxide black of generation, press filtration, rinsing, oven dry, pulverizing obtain blue phase oxidation iron oxide black pigment product.
In order to solve the bad technological deficiency of high thermal resistance of existing iron oxide black, applicant has applied for fire resistant black iron oxide pigment and preparation method thereof (200810063587.5 applyings date: 2008-06-20), the fire resistant black iron oxide pigment of this patent, comprise that ferromanganese is black, described ferromanganese is black to be reacted and generates through high temperature lattice by Z 250 and Mn oxide, ferro element in described pigment and the mol ratio of manganese element are 1.5: 1～5: 1, its heatproof effect of the fire resistant black iron oxide pigment of producing can reach 700 ℃ or more than.
Chinese invention patent application (application number: the 201010158966.X applying date: 2010-04-29) discloses a kind of manufacturing process of resistance to middle temperature iron oxide black; the method adopts oxidation style to produce the iron oxide black obtaining; directly use the filter cake of not drying; iron oxide black filter cake and water are dropped into; control hollander and make certain density slurries; in pulping process, add water-soluble additive, add neutralizing agent, regulate pH value; Continue to stir, after being incubated, by normal step, produce iron oxide black, dry and beat powder, obtain resistance to middle temperature iron oxide black.The iron oxide black that this technique makes can bear 260～270 ℃ and nondiscoloration or change very little; Iron black resistance toheat of the present invention is good, nonflammable and variable color when transportation and preservation, and the colour-change of guaranteeing to be heated is little, guarantees transportation and the security of preserving, and can use at 270 ℃ simultaneously.
Chinese invention patent application (application number: the 200910153578.X applying date: 2009-10-20) discloses a kind of iron oxide black granular pigment and manufacture method thereof, the method comprises that the combination of a) getting in Xylo-Mucine, polyvinyl alcohol, water glass, gelatin, sodium lignosulfonate, ferrous sulfate, calcium lignin sulphonate, Sodium hexametaphosphate 99, polyacrylic acid, sodium stearate any one or more than one component is as additive, additive is mixed with to the aqueous solution of 0.1～30% (weight ratio), heats 30～100 ℃; B) by weight, get 100 parts～200 parts of iron oxide blacks, send into tablets press, 15 parts～60 parts additive aqueous solution are evenly sprayed to powder, form gradually small-particle; C) particle step b) being made screens with vibratory screening apparatus, and gained particle diameter material is dried and got product.The method adopts individual layer coated, and mobility and the dispersiveness of product is provided.
Summary of the invention
In order to solve the resistance toheat problem of iron oxide black, an object of the present invention is to provide a kind of resistance to middle temperature cladded type iron oxide black, this iron oxide black resistance to elevated temperatures is good, and the pigment ion after being coated is even, intensity is high, and dispersing property is more superior.Another object of the present invention is to provide the preparation method of above-mentioned resistance to middle temperature cladded type iron oxide black.
In order to realize above-mentioned first object, the present invention has adopted following technical scheme:
A kind of resistance to middle temperature cladded type iron oxide black; this iron oxide black comprises main body composition iron oxide black; main body composition iron oxide black is wrapped with additive-package coating; main body composition iron oxide black and multilayer coating structure layer combine and form the pigment with film; described multilayer coating structure layer by the compound containing aluminum ion and silicon ion by regulating pH value; make aluminum ion and silicon ion precipitate successively the surface that is coated on gradually iron oxide black molecule, form multilayer resist.
As preferably, described adopts Tai-Ace S 150 or sodium aluminate containing aluminum ion compound.
As the add-on of preferred again, described Tai-Ace S 150 or sodium aluminate, it is 10%～30% of dry powder amount.
As most preferably, described Tai-Ace S 150 or the add-on of sodium aluminate are 18%～25% of dry powder amount
As preferably, described siliceous ionic compound adopts water glass.
As the add-on of preferred again, described water glass, it is 15% ~ 30% of dry powder amount.
As most preferably, the add-on of described water glass is 20% ~ 25% of dry powder amount.
In order to realize above-mentioned second object, the present invention has adopted following technical scheme:
A preparation method who prepares above-mentioned resistance to middle temperature cladded type iron oxide black, the method comprises the following steps:
1) iron oxide black filter cake is poured in oxidation barrel, amount is done to obtain in the sampling that stirs, and opens steam valve punching temperature simultaneously, and opens and stir, and mixing speed is 200 ~ 300rpm;
2) according to measuring, calculate Tai-Ace S 150 or sodium aluminate add-on, drop into and dissolve in bucket, add a certain amount of water to dissolve;
3) when in reaction container temperature reach after 70-80 degree, add the Tai-Ace S 150 or the sodium aluminate that have dissolved, stirring reaction 8 ~ 12 minutes, then use liquid adjusting PH with base to 5 ~ 7, allows its stirring reaction 20 ~ 40 minutes;
4) will calculate the add-on of water glass, drop into have shifted in empty dissolving bucket and dissolve with a certain amount of water;
5) after etc. the reaction times finishes, adding concentration is 10% ~ 15% water glass having dissolved, and in adition process, with dilute sulphuric acid, regulates pH, makes it pH and reacts 8 ~ 12 minutes 6 ~ 7 in the situation that;
6) last, then with the anti-pH that adjusts of dilute sulphuric acid, be transferred to neutrality, stirring reaction 20 ~ 40 minutes, steam off valve, stops stirring, and reaction finishes;
7) processing of later process is carried out in press filtration, rinsing etc.;
8) finally carry out blending, make solid colour, conformance with standard.
What the present invention mainly adopted is the film in the molecular surface coating multilayer densification of ferric oxide, with this, improves the resistance toheat of iron oxide black.Technique is mainly first iron black filter cake to be broken into pulpous state, then adds containing aluminium and silicon ion, by regulating pH value, makes its precipitation be coated on gradually the surface of iron oxide black molecule, forms multilayer resist, makes its heating temperature reach 200 degree.
The present invention does coating treatment process on iron oxide pigment surface, its surface of passivation, and treatment process is comparatively advanced, and the pigment ion after being coated is even, intensity is high, and dispersing property is more superior.Coated adjuvant used Tai-Ace S 150 and water glass are easier to obtain, and auxiliary agent cost is lighter, iron black filter cake has iron black workshop to provide, coated processing carried out at pilot plant, treating processes is shorter, and energy consumption is lower, and this project technique is more ripe, and sample has obtained client's approval, and product performance index aspect all meets client's demand.
the key technical indexes of product of the present invention:
| Sequence number | Project | Index |
| 1 | Proterties | Black powder |
| 2 | Fe 2O 3Content % | ≥88 |
| 3 | 105 ℃ of volatile matter % | ≤1.5 |
| 4 | Water solubles % | ≤0.5 |
| 5 | Oil number % | 15～35 |
| 6 | 320 screen residue % | ≤0.3 |
| 7 | Tinctorial strength % | 95～105 |
| 8 | Aqeous suspension pH value | 5.5～9.5 |
| 9 | Coloured light (with standard specimen ratio) | Approximate～slightly seemingly |
| 10 | Resistance to 200 ℃/30min △ E | ≤1.0 |
Technique of the present invention is except producing resistance to middle temperature black iron oxide pigment, and in making processes, the most important thing is not add any organic chemicals, and the equipment that inventive method adopts is extensive, simple, easy to operate.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below by concrete experiment, the present invention is further illustrated:
The iron oxide black filter cake that this process using wet method oxide sulfate method obtains, making beating, heats up and adds auxiliary agent to be oxidized coating to obtain this product.
embodiment 1
As shown in Figure 1, get 1 ton of iron oxide black filter cake, solid content is that 60% making beating is warming up to 85-95 degree, adding auxiliary agent Tai-Ace S 150 is 18% of conversion dry powder amount, actual add-on is 108 kilograms, continue making beating reaction 30 minutes, regulate PH 9.5 allow its stirring reaction 90 minutes with the liquid caustic soda of 20-40%. will calculate the add-on of water glass, 25% of conversion dry powder amount, actual add-on is 150 kilograms, continue making beating reaction 30 minutes, with the dilute sulphuric acid of 10-20%, regulating PH is neutrality, allows its stirring reaction 90 minutes.Rinsing, dries.As follows with resistance to middle temperature iron oxide black and the contrast of common iron oxide black test result of this explained hereafter:
embodiment 2
As shown in Figure 1, get 1 ton of iron oxide black filter cake, solid content is that 60% making beating is warming up to 85-95 degree, adding auxiliary agent Tai-Ace S 150 is 25% of conversion dry powder amount, actual add-on is 150 kilograms, continue making beating reaction 30 minutes, regulate PH 9.5 allow its stirring reaction 90 minutes with the liquid caustic soda of 20-40%. will calculate the add-on of water glass, 20% of conversion dry powder amount, actual add-on is 120 kg, continue making beating reaction 30 minutes, with the dilute sulphuric acid of 10-20%, regulating PH is neutrality, allows its stirring reaction 90 minutes.Rinsing, dries.As follows with resistance to middle temperature iron oxide black and the contrast of common iron oxide black test result of this explained hereafter:
From above comparative result, show, the temperature tolerance of the black iron oxide pigment of process coating processing changes △ E below 1.0 in 200 degree left and right, and in 200 degree left and right, has become iron oxide red △ E in 10.0 left and right without the black iron oxide pigment temperature tolerance of coating processing.
Claims (3)
1. a resistance to middle temperature cladded type iron oxide black, this iron oxide black comprises main body composition iron oxide black, it is characterized in that: main body composition iron oxide black is wrapped with additive-package coating, main body composition iron oxide black and multilayer coating structure layer combine and form the pigment with film, described multilayer coating structure layer by the compound containing aluminum ion and silicon ion by regulating pH value, make aluminum ion and silicon ion precipitate successively the surface that is coated on gradually iron oxide black molecule, form multilayer resist; Described adopts Tai-Ace S 150 or sodium aluminate containing aluminum ion compound, and the add-on of Tai-Ace S 150 or sodium aluminate is 10%～30% of dry powder amount; Siliceous ionic compound adopts water glass, and the add-on of water glass is 15% ~ 30% of dry powder amount.
2. the resistance to middle temperature cladded type iron oxide black of one according to claim 1, is characterized in that: the add-on of Tai-Ace S 150 or sodium aluminate is 18%～25% of dry powder amount.
3. the resistance to middle temperature cladded type iron oxide black of one according to claim 1, is characterized in that: the add-on of water glass is 20% ~ 25% of dry powder amount.
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| CN103289445B (en) * | 2013-05-23 | 2014-11-19 | 铜陵瑞莱科技有限公司 | Method for preparing high-temperature-resistant iron oxide black granules |
| CN103289442A (en) * | 2013-05-23 | 2013-09-11 | 铜陵瑞莱科技有限公司 | Preparation method of black iron oxide particles with corrosion inhibition performance |
| CN103305031B (en) * | 2013-05-23 | 2014-07-16 | 铜陵瑞莱科技有限公司 | Preparation method of precipitated white graphite/graphite iron oxide black granule |
| CN103289443B (en) * | 2013-05-23 | 2014-12-31 | 铜陵瑞莱科技有限公司 | Method for preparing medium-temperature-resistant iron oxide black granules |
| CN103289437B (en) * | 2013-05-23 | 2014-07-16 | 铜陵瑞莱科技有限公司 | Method for preparing high-dispersion black iron oxide particles |
| CN103289440B (en) * | 2013-05-23 | 2014-07-16 | 铜陵瑞莱科技有限公司 | Preparation method of water glass coated iron oxide black particles |
| CN103289439B (en) * | 2013-05-23 | 2015-01-21 | 铜陵瑞莱科技有限公司 | Method for preparing enveloped iron oxide black granules |
| CN103333524B (en) * | 2013-06-08 | 2014-07-16 | 安徽天泰环保科技有限公司 | Preparation method of heat-resistant iron oxide black |
| CN103333522B (en) * | 2013-06-08 | 2014-07-16 | 安徽天泰环保科技有限公司 | Preparation method of oxidation-resistant corrosion-resistant iron oxide black |
| CN103421356B (en) * | 2013-07-26 | 2015-07-08 | 安徽麒麟化工科技有限公司 | Preparation method of rare earth modified iron oxide black |
| CN103788714A (en) * | 2014-02-12 | 2014-05-14 | 铜陵瑞莱科技有限公司 | Heat-resisting iron oxide black pigment |
| CN104087022B (en) * | 2014-06-30 | 2016-06-29 | 肇庆金三江硅材料有限公司 | A kind of silicon dioxide of hud typed cladding pigment and preparation method thereof |
| CN104312221B (en) * | 2014-10-27 | 2016-03-02 | 合肥旭阳铝颜料有限公司 | A kind of fire resistant magnetic aluminium pigment and preparation method thereof |
| CN104312222A (en) * | 2014-10-27 | 2015-01-28 | 合肥旭阳铝颜料有限公司 | Anti-rusting magnetic aluminium pigment and preparation method thereof |
| CN105131653A (en) * | 2015-07-25 | 2015-12-09 | 铜陵瑞莱科技有限公司 | Iron oxide black pigment used for printing ink and preparation method thereof |
| CN105086519A (en) * | 2015-07-27 | 2015-11-25 | 安徽明珠颜料科技有限公司 | Antibacterial and bacteriostatic ferric oxide black pigment and preparation method thereof |
| CN105504883B (en) * | 2015-12-29 | 2018-01-02 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of high temperature tolerance ferric oxide yellow pigment |
| CN110317474A (en) * | 2019-06-28 | 2019-10-11 | 广西新晶科技有限公司 | A kind of ferric oxide powder and preparation method thereof that nano inorganic-is organic coated |
| CN112300605A (en) * | 2020-11-26 | 2021-02-02 | 江苏宇星工贸有限公司 | Coated iron oxide black pigment and preparation method thereof |
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Address after: 313220, Zhejiang, Huzhou province Deqing County bell town landscape crossing sublimation group Deqing Huayuan Pigment Co., Ltd. Patentee after: Zhejiang Huayuan pigment Limited by Share Ltd Address before: 313220, Zhejiang, Huzhou province Deqing County bell town landscape crossing sublimation group Deqing Huayuan Pigment Co., Ltd. Patentee before: Shenghua Group Deqing Huayuan Pigment Co., Ltd. |