CN102604437A - 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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- CN102604437A CN102604437A CN2012100382524A CN201210038252A CN102604437A CN 102604437 A CN102604437 A CN 102604437A CN 2012100382524 A CN2012100382524 A CN 2012100382524A CN 201210038252 A CN201210038252 A CN 201210038252A CN 102604437 A CN102604437 A CN 102604437A
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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, the chemical name Z 250 belongs to spinel type, and it has saturated blue black light black, and specific density is 4.73.Its opacifying power and tinting strength are all very high, and be very stable to light and atmospheric effect.Relatively poor because of the heat resistance of common iron oxide black, heating temperature uses under some have the occasion of temperature about 100 degree, phenomenon such as variable color will take place, fade.
Common iron oxide black working method such as Chinese invention patent application (application number: 200510075112.4 applyings date: 2005-06-08) disclose a kind of working method of iron oxide black, comprised following content: (1), make perferrite solution; (2), make neutralizing agent and perferrite solution reaction generation ferrous hydroxide with caustic soda; (3), make oxygenant with oxygen-containing gas, with above-mentioned hydroxide iron oxidation reaction generation iron oxide black; Sieve in the iron oxide black that (4), will generate, press filtration, rinsing, oven dry, pulverizing promptly get blue phase oxidation iron oxide black pigment product.
For the bad technological deficiency of the high thermal resistance that solves existing iron oxide black; The 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 black by Z 250 and Mn oxide through high temperature lattice reaction generation, the ferro element in the 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 being produced can reach 700 ℃ or more than.
The Chinese invention patent application (application number: the 201010158966.X applying date: 2010-04-29) disclose a kind of anti-in the ME of warm iron oxide black; The iron oxide black that this method adopts oxidation style production to obtain directly uses not dried filter cake, with iron oxide black filter cake and water input; The control hollander is processed certain density slurries; In pulping process, add water-soluble additive, add neutralizing agent, regulate the pH value; Continue to stir, insulation is accomplished the back and is produced iron blackly by normal step, dries and beats powder, obtain anti-in warm iron oxide black.The iron oxide black that this technology 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 under 270 ℃, can use simultaneously.
Chinese invention patent application (application number: the 200910153578.X applying date: 2009-10-20) disclose a kind of iron oxide black granular pigment and method of manufacture thereof; This method comprises that the combination of a) getting in Xylo-Mucine, Z 150PH, water glass, gelatin, sodium lignosulfonate, ferrous sulfate, calcium lignin sulphonate, Sodium hexametaphosphate 99, ROHM, the StNa any one or more than one component is as additive; Additive is mixed with 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 on the powder, form small-particle gradually; C) particle that step b) is made screens with vibratory screening apparatus, and gained particle diameter material is dried and got product.This method adopts individual layer to coat, and the mobile and dispersed 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 anti-in warm cladded type iron oxide black, this iron oxide black resistance to elevated temperatures is good, the pigment ion after the coating evenly, intensity is high, dispersing property is more superior.Another object of the present invention provide above-mentioned anti-in the preparation method of warm cladded type iron oxide black.
In order to realize above-mentioned first purpose, the technical scheme below the present invention has adopted:
A kind of anti-in warm 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 the additive-package coating, and main body composition iron oxide black and multilayer coating layer combine and constitute the pigment of band film, and described multilayer coating layer passes through to regulate the pH value by the compound that contains aluminum ion and silicon ion; Make aluminum ion and silicon ion precipitate the surface that is coated on the iron oxide black molecule gradually successively, form multilayer resist.
As preferably, the described aluminum ion compound that contains adopts Tai-Ace S 150 or sodium aluminate.
Preferred as again, the add-on of described Tai-Ace S 150 or sodium aluminate is 10%～30% of a dry powder amount.
As most preferably, the add-on of described Tai-Ace S 150 or sodium aluminate is 18%～25% of a dry powder amount
As preferably, described siliceous ionic compound adopts water glass.
Preferred as again, the add-on of described water glass is 15% ~ 30% of a dry powder amount.
As most preferably, the add-on of described water glass is 20% ~ 25% of a dry powder amount.
In order to realize above-mentioned second purpose, the technical scheme below the present invention has adopted:
A kind of prepare above-mentioned anti-in the preparation method of warm cladded type iron oxide black, this method comprises the steps:
1) the iron oxide black filter cake is poured in the oxidation bucket, the sampling that stirs is done to such an extent that measure, and opens steam valve simultaneously and dashes temperature, and open and stir, and mixing speed is 200 ~ 300rpm;
2) calculate Tai-Ace S 150 or sodium aluminate add-on according to measuring, drop in the dissolving bucket, add a certain amount of water and dissolve;
3) when ground in the reaction container after temperature reaches the 70-80 degree, add dissolving good Tai-Ace S 150 or sodium aluminate, stirring reaction 8 ~ 12 minutes is used liquid adjusting PH with base to 5 ~ 7 again, lets its stirring reaction 20 ~ 40 minutes;
4) will calculate the add-on of water glass, and drop into to have shifted in the empty dissolving bucket and dissolves with a certain amount of water;
5) after etc. the reaction times finishes, add concentration and be 10% ~ 15% dissolved water glass, in adition process, will regulate pH with dilute sulphuric acid, making it pH reacted under 6 ~ 7 situation 8 ~ 12 minutes;
6) last, with the anti-pH that transfers of dilute sulphuric acid, be transferred to neutrality again, stirring reaction 20 ~ 40 minutes, the steam off valve stops to stir, and reaction finishes;
7) processing of later process is carried out in press filtration, rinsing etc.;
8) piece together mixedly at last, make solid colour, conformance with standard.
What the present invention mainly adopted is at the fine and close film of the molecular surface coating multilayer of red stone, improves the resistance toheat of iron oxide black with this.Technology mainly is earlier iron black filter cake to be broken into pulpous state, adds then and contains aluminium and silicon ion, through regulating the pH value, makes its deposition be coated on the surface of iron oxide black molecule gradually, forms multilayer resist, makes its heating temperature reach 200 degree.
The present invention does the coating treatment process on the iron oxide pigment surface, its surface of passivation, and treatment process is comparatively advanced, and the pigment ion after the coating is even, intensity is high, and dispersing property is more superior.Coat adjuvant used Tai-Ace S 150 and water glass and be easier to obtain, and the auxiliary agent cost is lighter, iron black filter cake has iron black workshop to provide; Coat to handle and carry out at pilot plant; Treating processes is shorter, and energy consumption is lower, and this project technology is ripe; And sample has obtained customer approval, and the product performance index aspect all satisfies 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 | The aqeous suspension pH value | 5.5～9.5 |
| 9 | Coloured light (with the standard specimen ratio) | Approximate～slightly seemingly |
| 10 | Anti-200 ℃/30min △ E | ≤1.0 |
Technology of the present invention except can produce anti-in warm black iron oxide pigment, and in making processes, the most important thing is not add any organic chemicals, and the equipment that inventive method adopted is extensive, simple, easy to operate.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Through concrete experiment the present invention is further described below:
The iron oxide black filter cake that this process using wet method oxide sulfate method obtains, making beating, the adding auxiliary agent that heats up carries out the oxidation coating and obtains 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 the 85-95 degree; Add auxiliary agent Tai-Ace S 150 and be 18% of conversion dry powder amount, actual add-on is 108 kilograms, continues making beating reaction 30 minutes; Use the liquid caustic soda of 20-40% to regulate PH and 9.5 let its stirring reaction 90 minutes. will calculate the add-on of water glass; 25% of conversion dry powder amount, actual add-on is 150 kilograms, continues making beating reaction 30 minutes; Use the dilute sulphuric acid of 10-20% to regulate PH and be neutrality, let its stirring reaction 90 minutes.Rinsing, oven dry.Contrast as follows with warm iron oxide black in this explained hereafter anti-and common iron oxide black test result:
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 the 85-95 degree; Add auxiliary agent Tai-Ace S 150 and be 25% of conversion dry powder amount, actual add-on is 150 kilograms, continues making beating reaction 30 minutes; Use the liquid caustic soda of 20-40% to regulate PH and 9.5 let its stirring reaction 90 minutes. will calculate the add-on of water glass; 20% of conversion dry powder amount, actual add-on is a 120 kg, continues making beating reaction 30 minutes; Use the dilute sulphuric acid of 10-20% to regulate PH and be neutrality, let its stirring reaction 90 minutes.Rinsing, oven dry.Contrast as follows with warm iron oxide black in this explained hereafter anti-and common iron oxide black test result:
Show that from above comparative result the temperature tolerance of the black iron oxide pigment of handling through coating changes △ E below 1.0 about 200 degree, and about 200 degree, has become iron oxide red △ E without the black iron oxide pigment temperature tolerance that coating is handled about 10.0.
Claims (8)
- One kind anti-in warm 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 the additive-package coating, and main body composition iron oxide black and multilayer coating layer combine and constitute the pigment of band film, and described multilayer coating layer passes through to regulate the pH value by the compound that contains aluminum ion and silicon ion; Make aluminum ion and silicon ion precipitate the surface that is coated on the iron oxide black molecule gradually successively, form multilayer resist.
- 2. according to claim 1 a kind of anti-in warm cladded type iron oxide black, it is characterized in that: contain the aluminum ion compound and adopt Tai-Ace S 150 or sodium aluminate.
- 3. according to claim 2 a kind of anti-in warm cladded type iron oxide black, it is characterized in that: the add-on of Tai-Ace S 150 or sodium aluminate is 10%～30% of a dry powder amount.
- 4. according to claim 3 a kind of anti-in warm cladded type iron oxide black, it is characterized in that: the add-on of Tai-Ace S 150 or sodium aluminate is 18%～25% of a dry powder amount.
- 5. according to claim 1 a kind of anti-in warm cladded type iron oxide black, it is characterized in that: siliceous ionic compound adopts water glass.
- 6. according to claim 5 a kind of anti-in warm cladded type iron oxide black, it is characterized in that: the add-on of water glass is 15% ~ 30% of a dry powder amount.
- 7. according to claim 6 a kind of anti-in warm cladded type iron oxide black, it is characterized in that: the add-on of water glass is 20% ~ 25% of a dry powder amount.
- One kind prepare any claim of claim 1 ~ 7 described anti-in the preparation method of warm cladded type iron oxide black, it is characterized in that this method comprises the steps:1) the iron oxide black filter cake is poured in the oxidation bucket, the sampling that stirs is done to such an extent that measure, and opens steam valve simultaneously and dashes temperature, and open and stir, and mixing speed is 200 ~ 300rpm;2) calculate Tai-Ace S 150 or sodium aluminate add-on according to measuring, drop in the dissolving bucket, add a certain amount of water and dissolve;3) when ground in the reaction container after temperature reaches the 70-80 degree, add dissolving good Tai-Ace S 150 or sodium aluminate, stirring reaction 8 ~ 12 minutes is used liquid adjusting PH with base to 5 ~ 7 again, lets its stirring reaction 20 ~ 40 minutes;4) will calculate the add-on of water glass, and drop into to have shifted in the empty dissolving bucket and dissolves with a certain amount of water;5) after etc. the reaction times finishes, add concentration and be 10% ~ 15% dissolved water glass, in adition process, will regulate pH with dilute sulphuric acid, making it pH reacted under 6 ~ 7 situation 8 ~ 12 minutes;6) last, with the anti-pH that transfers of dilute sulphuric acid, be transferred to neutrality again, stirring reaction 20 ~ 40 minutes, the steam off valve stops to stir, and reaction finishes;7) processing of later process is carried out in press filtration, rinsing etc.;8) piece together mixedly at last, make solid colour, conformance with standard.
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| CN103289439A (en) * | 2013-05-23 | 2013-09-11 | 铜陵瑞莱科技有限公司 | Method for preparing enveloped iron oxide black granules |
| CN103289437A (en) * | 2013-05-23 | 2013-09-11 | 铜陵瑞莱科技有限公司 | Method for preparing high-dispersion black iron oxide particles |
| CN103289440A (en) * | 2013-05-23 | 2013-09-11 | 铜陵瑞莱科技有限公司 | Preparation method of water glass coated iron oxide black particles |
| CN103289443A (en) * | 2013-05-23 | 2013-09-11 | 铜陵瑞莱科技有限公司 | Method for preparing medium-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 |
| CN103289445A (en) * | 2013-05-23 | 2013-09-11 | 铜陵瑞莱科技有限公司 | Method for preparing high-temperature-resistant iron oxide black granules |
| CN103305031A (en) * | 2013-05-23 | 2013-09-18 | 铜陵瑞莱科技有限公司 | Preparation method of precipitated white graphite/graphite iron oxide black granule |
| CN103333524A (en) * | 2013-06-08 | 2013-10-02 | 安徽天泰环保科技有限公司 | Preparation method of heat-resistant iron oxide black |
| CN103333522A (en) * | 2013-06-08 | 2013-10-02 | 安徽天泰环保科技有限公司 | Preparation method of oxidation-resistant corrosion-resistant iron oxide black |
| CN103421356A (en) * | 2013-07-26 | 2013-12-04 | 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 |
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| 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 |
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| 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 |
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| 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. |