CN105038326A - Fly ash doped iron oxide black pigment and preparation method thereof - Google Patents
Fly ash doped iron oxide black pigment and preparation method thereof Download PDFInfo
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- CN105038326A CN105038326A CN201510456105.2A CN201510456105A CN105038326A CN 105038326 A CN105038326 A CN 105038326A CN 201510456105 A CN201510456105 A CN 201510456105A CN 105038326 A CN105038326 A CN 105038326A
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Abstract
The invention discloses fly ash doped iron oxide black pigment which is prepared from the following raw materials by weight: 80 to 100 parts of modified iron oxide black, 10 to 15 parts of fly ash, 3 to 5 parts of sodium tripolyphosphate, 1 to 2 parts of hydroxypropyl methyl cellulose, 6 to 8 parts of sodium silicate, 0.1 to 0.2 part of azodiisobutyronitrile, 10 to 15 parts of phenethylene, 2 to 4 parts of liquid petrolatum, and 1 to 2 parts of erucamide. The iron oxide black pigment is high in tinting strength, favorable in temperature resistance and weatherability, easy to disperse, and high in processability, strength, shock resistance, durability, service performance, and can realize energy conservation and environmental protection.
Description
Technical field
The present invention relates to iron oxide pigment field, be specifically related to black iron oxide pigment of a kind of adulterated flour coal ash and preparation method thereof.
Background technology
Iron oxide black is the one of iron pigment, and its moiety is Z 250, has saturated indigo plant ink light blue.Black iron oxide pigment has good weathering resistance, to light and atmospheric stability, opacifying power and tinting strength high, form and aspect are pure, with low cost, can be widely used in the industries such as building, plastics, pottery, coating.Along with the development of economy, the requirement of market to black iron oxide pigment also improves constantly, and its Application Areas and purposes are just constantly widened.But in actual applications, because the heat resistance of iron oxide black is poor, can fade at relatively high temperatures, the phenomenon such as variable color, easily reunite in addition, be difficult to problems such as being uniformly dispersed, limit the use range of iron oxide black.Therefore, need to carry out surface treatment to black iron oxide pigment, to reach lifting use properties, enrich product function, the object of meeting the market requirement.
Summary of the invention
The object of this invention is to provide a kind of black iron oxide pigment of adulterated flour coal ash, there is good temperature tolerance and erosion resistance, be easy to dispersion, intensity and weather resistance high, use properties is good.
The present invention is achieved by the following technical solutions:
A black iron oxide pigment for adulterated flour coal ash, it is obtained by the raw material of following weight parts:
Modified oxidized iron black 80-100, flyash 10-15, tripoly phosphate sodium STPP 3-5, Vltra tears 1-2, water glass 6-8, Diisopropyl azodicarboxylate 0.1-0.2, vinylbenzene 10-15, whiteruss 2-4, erucicamide 1-2;
Wherein modified oxidized iron oxide black is obtained by the raw material of following weight parts: ferrous sulfate 40-50, imidazoline quaternary ammonium salt 0.3-0.5, citric acid 0.3-0.5, dimethyl silicone oil 0.2-0.4; Citric acid is added to the water by solid-liquid weight ratio 1:100-1:150 to dissolve completely by the preparation method of described modified oxidized iron oxide black, and all the other raw materials 800-1000r/min added outside sulfuric acid ferrous iron stirs 5-10min, obtains modification liquid; Ferrous sulfate is added to the water the solution being mixed with 150-200g/L, in solution, adds described modification liquid, pH regulator is stirred to 7-8, pass into oxygen to be oxidized under 80-90 DEG C of condition, react the iron oxide black of terminating in rear separating slurry, through washing, oven dry, pulverize, to obtain final product.
A preparation method for the black iron oxide pigment of adulterated flour coal ash, comprises the following steps:
(1) grinding after modified oxidized iron oxide black, flyash, tripoly phosphate sodium STPP and Vltra tears mixing evenly, is then added the water of 2-3 times of weight, obtains iron oxide black slurries after dispersed with stirring;
(2) water glass is added to the water the solution being mixed with 20-30g/L, then be added dropwise in the iron oxide black slurries in (1) and stir, by pH regulator to 8-8.5, then ageing 2-3h, filters, washs and obtain coated with silica iron oxide black after drying;
(3) Diisopropyl azodicarboxylate is dissolved in a small amount of toluene obtains initiation solution; Coated with silica iron oxide black in (2) and vinylbenzene to be added jointly in appropriate dehydrated alcohol and to be uniformly dispersed; pass into nitrogen protection and temperature is adjusted to 70-80 DEG C; drip initiation solution reaction 2-4h; mix with all the other raw materials after filtration, washing and grind evenly, after drying, namely obtaining the black iron oxide pigment of adulterated flour coal ash.
Advantage of the present invention is:
The present invention utilizes the properties-correcting agent such as imidazoline quaternary ammonium salt and citric acid to carry out modification to iron oxide black, plays good dissemination in particle formation, effectively improves the tinting strength of iron oxide black, has corrosion inhibition simultaneously; Then carry out silicon-dioxide and vinylbenzene double-coated, both improved the temperature tolerance of black iron oxide pigment, make it have again good erosion resistance, improve its dispersing property in the base simultaneously; Flyash, as industrial waste, has good mechanical property and workability.Composite by with the raw material such as flyash, not only tinting strength is high to make the black iron oxide pigment that obtains, temperature tolerance and weathering resistance good, be easy to dispersion, good processability, intensity is high, strong shock resistance, good endurance, and use properties is good, and energy-conserving and environment-protective.
Embodiment
Non-limiting examples of the present invention is as follows:
A black iron oxide pigment for adulterated flour coal ash, is prepared from by the component raw material of following weight (kg):
Modified oxidized iron black 90, flyash 12, tripoly phosphate sodium STPP 4, Vltra tears 1.5, water glass 7, Diisopropyl azodicarboxylate 0.15, vinylbenzene 12, whiteruss 3, erucicamide 1.5;
Wherein modified oxidized iron oxide black is obtained by the raw material of following weight parts: ferrous sulfate 45, imidazoline quaternary ammonium salt 0.4, citric acid 0.4, dimethyl silicone oil 0.3; Citric acid is added to the water by solid-liquid weight ratio 1:100 to dissolve completely by the preparation method of described modified oxidized iron oxide black, and all the other raw materials 1000r/min added outside sulfuric acid ferrous iron stirs 5min, obtains modification liquid; Ferrous sulfate is added to the water the solution being mixed with 150g/L, in solution, adds described modification liquid, pH regulator is stirred to 7-8, pass into oxygen to be oxidized under 80 DEG C of conditions, react the iron oxide black of terminating in rear separating slurry, through washing, oven dry, pulverize, to obtain final product.
The preparation method of the black iron oxide pigment of adulterated flour coal ash comprises the following steps:
(1) grinding after modified oxidized iron oxide black, flyash, tripoly phosphate sodium STPP and Vltra tears mixing evenly, is then added the water of 3 times of weight, obtains iron oxide black slurries after dispersed with stirring;
(2) water glass is added to the water the solution being mixed with 25g/L, then be added dropwise in the iron oxide black slurries in (1) and stir, by pH regulator to 8-8.5, then ageing 2h, filters, washs and obtain coated with silica iron oxide black after drying;
(3) Diisopropyl azodicarboxylate is dissolved in a small amount of toluene obtains initiation solution; Coated with silica iron oxide black in (2) and vinylbenzene to be added jointly in appropriate dehydrated alcohol and to be uniformly dispersed; pass into nitrogen protection and temperature is adjusted to 80 DEG C; drip initiation solution reaction 2h; mix with all the other raw materials after filtration, washing and grind evenly, after drying, namely obtaining the black iron oxide pigment of adulterated flour coal ash.
Above-mentioned obtained black iron oxide pigment performance is as following table:
| Project | Analytical results |
| 105 DEG C of volatile matter/% | 1.1 |
| Screenings (320 mesh sieve) | 0.4 |
| Tinctorial strength/% | 97.5 |
| Coloured light (with standard specimen ratio) | Slightly |
| Resistance to 260 DEG C/30min △ E | 0.40 |
Claims (2)
1. a black iron oxide pigment for adulterated flour coal ash, is characterized in that, it is obtained by the raw material of following weight parts:
Modified oxidized iron black 80-100, flyash 10-15, tripoly phosphate sodium STPP 3-5, Vltra tears 1-2, water glass 6-8, Diisopropyl azodicarboxylate 0.1-0.2, vinylbenzene 10-15, whiteruss 2-4, erucicamide 1-2;
Described modified oxidized iron oxide black is obtained by the raw material of following weight parts: ferrous sulfate 40-50, imidazoline quaternary ammonium salt 0.3-0.5, citric acid 0.3-0.5, dimethyl silicone oil 0.2-0.4; Citric acid is added to the water by solid-liquid weight ratio 1:100-1:150 to dissolve completely by the preparation method of described modified oxidized iron oxide black, and all the other raw materials 800-1000r/min added outside sulfuric acid ferrous iron stirs 5-10min, obtains modification liquid; Ferrous sulfate is added to the water the solution being mixed with 150-200g/L, in solution, adds described modification liquid, pH regulator is stirred to 7-8, pass into oxygen to be oxidized under 80-90 DEG C of condition, react the iron oxide black of terminating in rear separating slurry, through washing, oven dry, pulverize, to obtain final product.
2. the preparation method of the black iron oxide pigment of a kind of adulterated flour coal ash according to claim 1, is characterized in that, comprise the following steps:
(1) grinding after modified oxidized iron oxide black, flyash, tripoly phosphate sodium STPP and Vltra tears mixing evenly, is then added the water of 2-3 times of weight, obtains iron oxide black slurries after dispersed with stirring;
(2) water glass is added to the water the solution being mixed with 20-30g/L, is then added dropwise in the iron oxide black slurries in (1) and stirs, by pH regulator to 8-8.5, then ageing 2-3h, filters, washs and obtain coated with silica iron oxide black after drying;
(3) Diisopropyl azodicarboxylate is dissolved in a small amount of toluene obtains initiation solution; Coated with silica iron oxide black in (2) and vinylbenzene to be added jointly in appropriate dehydrated alcohol and to be uniformly dispersed; pass into nitrogen protection and temperature is adjusted to 70-80 DEG C; initiation solution reaction 2-4h described in dropping; mix with all the other raw materials after filtration, washing and grind evenly, after drying, namely obtaining the black iron oxide pigment of adulterated flour coal ash.
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| CN201510456105.2A CN105038326A (en) | 2015-07-27 | 2015-07-27 | Fly ash doped iron oxide black pigment and preparation method thereof |
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| CN201510456105.2A CN105038326A (en) | 2015-07-27 | 2015-07-27 | Fly ash doped iron oxide black pigment and preparation method thereof |
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| CN1473883A (en) * | 2003-07-01 | 2004-02-11 | 上海华明高技术（集团）有限公司 | Method for increasing dispersiveness of inorganic oxide powder in organic medium |
| CN1517412A (en) * | 2003-01-24 | 2004-08-04 | 罗姆和哈斯公司 | Organic-inorganic compound particle and its preparation method |
| CN101082752A (en) * | 2006-06-01 | 2007-12-05 | 陈宇 | Electrophoresis displaying particle and synthetic method thereof |
| CN101205421A (en) * | 2007-12-10 | 2008-06-25 | 南京工业大学 | Nano magnetron pigment and preparation method thereof |
| CN102344632A (en) * | 2011-06-13 | 2012-02-08 | 天津大学 | Three-layer core-shell-structure inorganic nanoparticle/silicon dioxide/high polymer composite microspheres and preparation method thereof |
| CN102485806A (en) * | 2010-12-06 | 2012-06-06 | 上海暄洋化工材料科技有限公司 | Water-based inorganic zinc shop primer, its preparation method and its application |
-
2015
- 2015-07-27 CN CN201510456105.2A patent/CN105038326A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1517412A (en) * | 2003-01-24 | 2004-08-04 | 罗姆和哈斯公司 | Organic-inorganic compound particle and its preparation method |
| CN1473883A (en) * | 2003-07-01 | 2004-02-11 | 上海华明高技术（集团）有限公司 | Method for increasing dispersiveness of inorganic oxide powder in organic medium |
| CN101082752A (en) * | 2006-06-01 | 2007-12-05 | 陈宇 | Electrophoresis displaying particle and synthetic method thereof |
| CN101205421A (en) * | 2007-12-10 | 2008-06-25 | 南京工业大学 | Nano magnetron pigment and preparation method thereof |
| CN102485806A (en) * | 2010-12-06 | 2012-06-06 | 上海暄洋化工材料科技有限公司 | Water-based inorganic zinc shop primer, its preparation method and its application |
| CN102344632A (en) * | 2011-06-13 | 2012-02-08 | 天津大学 | Three-layer core-shell-structure inorganic nanoparticle/silicon dioxide/high polymer composite microspheres and preparation method thereof |
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Application publication date: 20151111 |