CN102604434A - Preparation method of coated iron oxide black with medium temperature resistance - Google Patents
Preparation method of coated iron oxide black with medium temperature resistance Download PDFInfo
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- CN102604434A CN102604434A CN2012100382242A CN201210038224A CN102604434A CN 102604434 A CN102604434 A CN 102604434A CN 2012100382242 A CN2012100382242 A CN 2012100382242A CN 201210038224 A CN201210038224 A CN 201210038224A CN 102604434 A CN102604434 A CN 102604434A
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Abstract
The invention relates to a preparation method of temperature resistant iron oxide black, and discloses coated iron oxide black with medium temperature resistance. According to the preparation method, a plurality of layers of compact films are coated on the surfaces of iron oxide molecules, so that the heat resistance of iron oxide black is improved. The method mainly comprises the steps of firstly stirring iron oxide black filter cake into pulpous state, then adding aluminum ions and silicon ions, ensuring that ion precipitate is gradually coated on the surface of the iron oxide black molecules by adjusting pH value, so as to form a plurality of protecting films to ensure that the heated temperature of coated iron oxide black reaches 200 DEG C. According to the method, coating treatment process is performed on the surface of iron oxide pigment to passivate the surface, the treatment method is advanced, and coated pigment ions are uniform, and have high strength and superior dispersion property. Accessory ingredients such as aluminum sulfate and sodium silicate for coating are easily accessible, and have low costs. The oxide black filter cake is provided by oxide black plants, the coating treatment is performed in middle stage test workshop, the treatment process is short, the energy consumption is low, the technology of the project is mature, samples are approved by customers, and performance indexes of products meet the demands of the customers.
Description
Technical field
The present invention relates to a kind of preparation method of heatproof iron oxide black.
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 the preparation method of warm cladded type iron oxide black; The iron oxide black resistance to elevated temperatures of this method preparation is good, and the pigment ion after the coating is even, intensity is high, and dispersing property is more superior.
In order to realize above-mentioned purpose, the technical scheme below the present invention has adopted:
The preparation method of warm cladded type iron oxide black in anti-, 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, the add-on of sour aluminium or sodium aluminate is 10%~30% of a dry powder amount; 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, the add-on of water glass is 15% ~ 30% of a dry powder amount; Drop into to have shifted in the empty dissolving bucket and dissolve 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.
As most preferably, the add-on of described Tai-Ace S 150 or sodium aluminate is 18%~25% of a dry powder amount
As most preferably, the add-on of described water glass is 20% ~ 25% of a dry powder amount.
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 (3)
1. the preparation method of warm cladded type iron oxide black in anti-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, the add-on of sour aluminium or sodium aluminate is 10%~30% of a dry powder amount; 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, the add-on of water glass is 15% ~ 30% of a dry powder amount; Drop into to have shifted in the empty dissolving bucket and dissolve 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.
2. according to claim 1 anti-in the preparation method of 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.
3. according to claim 1 anti-in the preparation method of 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.
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Cited By (16)
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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 |
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 |
CN103318968A (en) * | 2013-06-25 | 2013-09-25 | 升华集团德清华源颜料有限公司 | Method for preparing medium-temperature-resistant iron oxide yellow pigment |
CN103318970A (en) * | 2013-06-25 | 2013-09-25 | 升华集团德清华源颜料有限公司 | Medium-temperature-resistant iron oxide yellow pigment |
CN103333541A (en) * | 2013-06-08 | 2013-10-02 | 安徽天泰环保科技有限公司 | Method for producing rust-proof uvioresistant black iron oxide |
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 |
CN103450709A (en) * | 2013-08-19 | 2013-12-18 | 铜陵瑞莱科技有限公司 | Surface-coated high-temperature-resistant iron oxide green |
CN103665947A (en) * | 2013-11-04 | 2014-03-26 | 铜陵市镜铁粉厂 | High-hardness black iron oxide |
CN104031423A (en) * | 2014-04-24 | 2014-09-10 | 铜陵市陵阳化工有限责任公司 | Preparation method for high temperature-resistant coated iron oxide black |
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 |
CN105293991A (en) * | 2015-10-16 | 2016-02-03 | 卓达新材料科技集团威海股份有限公司 | Modifying agent for filler and preparation method of filler |
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CN105504882A (en) * | 2015-12-15 | 2016-04-20 | 江苏省常熟环通实业有限公司 | Preparation method for surface-coated modified iron oxide yellow |
CN107090195A (en) * | 2017-05-02 | 2017-08-25 | 湖州师范学院 | A kind of easy dispersing iron oxide yellow pigment of heat resistant type and preparation method thereof |
CN111269588A (en) * | 2020-03-26 | 2020-06-12 | 正太新材料科技有限责任公司 | Heat-resistant iron oxide yellow with high tinting strength and preparation method and application thereof |
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 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. |