CN102604434B - 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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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 relative density is 4.73.Its opacifying power and tinting strength are all very high, and be very stable to the effect of light and atmosphere.Relatively poor because of the heat resistance of common iron oxide black, heating temperature is in 100 about degree, uses under some have the occasion of temperature, the phenomenon such as variable color will occur, fade.
Common iron oxide black production method such as Chinese invention patent application (application number: 200510075112.4 applyings date: 2005-06-08) disclose a kind of production 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 namely 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, the black reaction through the high temperature lattice by Z 250 and Mn oxide of described ferromanganese generates, 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: the manufacturing process that 2010-04-29) discloses a kind of anti-middle temperature iron oxide black, the iron oxide black that the method adopts oxidation style production to obtain, directly use the not filter cake of oven dry, iron oxide black filter cake and water are dropped into, control hollander and make certain density slurries, add water-soluble additive in pulping process, add neutralizing agent, regulate the pH value; Continue to stir, produce the iron oxide black by normal step after insulation is completed, powder is beaten in oven dry, obtains anti-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 under 270 ℃ 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 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 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) with step b) particle that makes screens with vibratory screening apparatus, and gained particle diameter material is dried and is got product.The method adopts individual layer to coat, 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 preparation method of anti-middle temperature cladded type iron oxide black, the iron oxide black resistance to elevated temperatures of the method preparation is good, and the pigment ion after coating is even, intensity is high, and dispersing property is more superior.
In order to realize above-mentioned purpose, the present invention has adopted following technical scheme:
The preparation method of anti-middle temperature cladded type iron oxide black, the method comprises the following steps:
1) the iron oxide black filter cake is poured in oxidation barrel, amount is done to get in the sampling that stirs, and opens simultaneously steam valve punching temperature, and opens 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 dry powder amount; Drop in the dissolving bucket, add a certain amount of water to dissolve;
3) after in reaction container temperature reaches the 70-80 degree, add dissolving good Tai-Ace S 150 or sodium aluminate, 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, the add-on of water glass is 15% ~ 30% of dry powder amount; Drop into to have shifted in empty dissolving bucket and dissolve with a certain amount of water;
5) after etc. the reaction times finished, adding concentration was 10% ~ 15% water glass that has dissolved, and will regulate pH with dilute sulphuric acid in adition process, made it pH in the situation that 6 ~ 7 reacted 8 ~ 12 minutes;
6) last, then with the anti-pH that transfers of dilute sulphuric acid, be transferred to neutrality, stirring reaction 20 ~ 40 minutes, the steam off valve stops stirring, and reaction finishes;
7) processing of later process is carried out in press filtration, rinsing etc.;
8) carry out at last blending, 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 dry powder amount
As most preferably, the add-on of described water glass is 20% ~ 25% of dry powder amount.
What the present invention mainly adopted is at the film of the molecular surface coating multilayer densification of ferric oxide, improves the resistance toheat of iron oxide black with this.Technique is mainly first iron black filter cake to be broken into pulpous state, then adds to contain aluminium and silicon ion, by regulating the 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 the coating treatment process on the iron oxide pigment surface, passivation its surface, and treatment process is comparatively advanced, and the pigment ion after coating is evenly, intensity is high, and dispersing property is more superior.Coating adjuvant used Tai-Ace S 150 and water glass is easier to obtain, and the auxiliary agent cost is lighter, iron black filter cake has iron black workshop to provide, coat to process and carry 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 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 |
Technique of the present invention be except can produce anti-middle temperature black iron oxide pigment, and the most important thing is not add any organic chemicals in making processes, and the equipment that inventive method adopts is extensive, and is simple, easy to operate.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
The present invention is further illustrated below by concrete experiment:
The iron oxide black filter cake that this process using wet method oxide sulfate method obtains, making beating, heating up adds auxiliary agent to carry out the oxidation 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 the 85-95 degree, add auxiliary agent Tai-Ace S 150 to be 18% of conversion dry powder amount, actual add-on is 108 kilograms, continue making beating reaction 30 minutes, regulate PH with the liquid caustic soda of 20-40% and 9.5 allow 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, continue making beating reaction 30 minutes, regulating PH with the dilute sulphuric acid of 10-20% is neutrality, allows its stirring reaction 90 minutes.Rinsing, oven dry.Anti-middle temperature iron oxide black and the contrast of common iron oxide black test result with this explained hereafter are as follows:
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 to be 25% of conversion dry powder amount, actual add-on is 150 kilograms, continue making beating reaction 30 minutes, regulate PH with the liquid caustic soda of 20-40% and 9.5 allow its stirring reaction 90 minutes. 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, regulating PH with the dilute sulphuric acid of 10-20% is neutrality, allows its stirring reaction 90 minutes.Rinsing, oven dry.Anti-middle temperature iron oxide black and the contrast of common iron oxide black test result with this explained hereafter are as follows:
Show from above comparative result, the temperature tolerance of the black iron oxide pigment that the process coating is processed is spent the left and right 200 and is changed △ E below 1.0, and has become iron oxide red △ E in 10.0 left and right without the black iron oxide pigment temperature tolerance of coating processing about 200 degree.
Claims (2)
1. the preparation method of anti-middle temperature cladded type iron oxide black, it is characterized in that: the iron oxide black filter cake that the method adopts wet method oxide sulfate method to obtain, get 1 ton of iron oxide black filter cake, solid content is that 60% making beating is warming up to the 85-95 degree, adding auxiliary agent Tai-Ace S 150 is 108 kilograms, continuing making beating reaction 30 minutes, is 9.5 to allow its stirring reaction 90 minutes with the liquid caustic soda adjusting pH of 20-40%; To calculate water glass and add, add-on is 150 kilograms, continues making beating reaction 30 minutes, and regulating pH with the dilute sulphuric acid of 10-20% is neutrality, allows its stirring reaction 90 minutes; Rinsing, oven dry.
2. the preparation method of anti-middle temperature cladded type iron oxide black, it is characterized in that: the iron oxide black filter cake that the method adopts wet method oxide sulfate method to obtain, get 1 ton of iron oxide black filter cake, solid content is that 60% making beating is warming up to the 85-95 degree, adding auxiliary agent Tai-Ace S 150 is 150 kilograms, continuing making beating reaction 30 minutes, is 9.5 to allow its stirring reaction 90 minutes with the liquid caustic soda adjusting pH of 20-40%; To calculate water glass and add, add-on is 120 kg, continues making beating reaction 30 minutes, and regulating pH with the dilute sulphuric acid of 10-20% is neutrality, allows its stirring reaction 90 minutes; Rinsing, oven dry.
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| 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 |
| 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 |
| CN103333541B (en) * | 2013-06-08 | 2014-12-17 | 安徽天泰环保科技有限公司 | Method for producing rust-proof uvioresistant black iron oxide |
| CN103318970B (en) * | 2013-06-25 | 2015-04-15 | 升华集团德清华源颜料有限公司 | Medium-temperature-resistant iron oxide yellow pigment |
| CN103318968B (en) * | 2013-06-25 | 2015-02-04 | 升华集团德清华源颜料有限公司 | Method for preparing medium-temperature-resistant iron oxide yellow pigment |
| 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 |
| CN103450709B (en) * | 2013-08-19 | 2016-01-13 | 铜陵瑞莱科技有限公司 | The resistant to elevated temperatures iron oxide green of a kind of surface-coating |
| CN103665947A (en) * | 2013-11-04 | 2014-03-26 | 铜陵市镜铁粉厂 | High-hardness black iron oxide |
| CN104031423B (en) * | 2014-04-24 | 2015-12-02 | 安徽陵阳新材料有限公司 | A kind of preparation method of high temperature resistant cladded type 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 |
| 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 |
| 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 |
| CN107090195B (en) * | 2017-05-02 | 2018-11-13 | 湖州师范学院 | A kind of easy dispersing iron oxide yellow pigment of heat resistant type and preparation method thereof |
| CN111269588B (en) * | 2020-03-26 | 2021-09-03 | 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. |