CN103421355A - Preparation method for organosilicone high temperature resisting black iron oxide - Google Patents

Preparation method for organosilicone high temperature resisting black iron oxide Download PDF

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Publication number
CN103421355A
CN103421355A CN2013103183298A CN201310318329A CN103421355A CN 103421355 A CN103421355 A CN 103421355A CN 2013103183298 A CN2013103183298 A CN 2013103183298A CN 201310318329 A CN201310318329 A CN 201310318329A CN 103421355 A CN103421355 A CN 103421355A
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China
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iron oxide
weight
black iron
seriflux
high temperature
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CN2013103183298A
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CN103421355B (en
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吴墨可
朱盛
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ANHUI QILIN CHEMICAL TECHNOLOGY Co Ltd
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ANHUI QILIN CHEMICAL TECHNOLOGY Co Ltd
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Abstract

The invention discloses a preparation method for organosilicone high temperature resisting black iron oxide, wherein the black iron oxide is prepared by adopting the sodium hydroxide oxidation method, and the preparation method comprises the following steps: a black iron oxide filter cake, which is not kiln dried, is directly used; ethanol solution, the weight of which is 2-3% of that of the black iron oxide filter cake, and silica sand, the weight of which is 1-2% of that of the black iron oxide filter cake, are added; the mixture is ground for 15-20 minutes at the speed of 1500-2500 rpm; the powder is taken out and dried, appropriate water is added, pulping is performed for 20-25 minutes, and seriflux with the concentration of 55-60% is prepared; methyl triethoxy silane, the weight of which is 4-6% of that of the seriflux, dimethyl dioxethyl silane, the weight of which is 2-3% of that of the seriflux, phenyl triethoxy silane, the weight of which is 5-8% of that of the seriflux, and hollow floating beads, the weight of which is 0.3-0.4% of that of the seriflux, are added, and the mixture is heated in water bath to 60-70 DEG C and stirred for 2-3 hours; a colloid mill is utilized to grind the seriflux until the grain size is less than 40 Mum; filtering, drying and powdering are performed, and the finished product is generated. The black iron oxide, disclosed by the invention, has superior high temperature resisting property and can bear the high temperature of 500-600 DEG C.

Description

A kind of preparation method of organosilicon fire-resistant iron oxide black
Technical field
The present invention relates to a kind of preparation method of organosilicon fire-resistant iron oxide black, belong to the chemical color field.
Background technology
Iron pigment is as important inorganic color(ed)pigment, and its annual production occupies first of inorganic color(ed)pigment.Due to the reinforcement of world's environmental consciousness, the inorganic iron series pigments constantly replaces the plumbous series such as pigment dyestuff and red lead, lead-chrome yellow, the serial poisonous mineral dye of chromium with characteristics such as it are nontoxic, odorless, pollution-free.Iron oxide black is because chemical composition is simple, nontoxic pollution-free, and chemical stability is strong, is widely used in the building trade paint.But iron oxide black will dewater when temperature reaches 100 ℃ of left and right, oxidation becomes iron oxide red.Use iron oxide black in some temperature under higher occasion, will fade, the phenomenon such as variable color, thereby limited the use range of iron oxide black.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of preparation method of organosilicon fire-resistant iron oxide black is provided.The iron oxide black high thermal resistance that this preparation method produces is good, and water-tolerant is dispersed superior.
The technical solution used in the present invention is as follows:
A kind of preparation method of organosilicon fire-resistant iron oxide black, the iron oxide black that adopts the sodium hydroxide oxidation style to make, directly use the oxidation filter cake of not drying, add the ethanolic soln that is equivalent to iron oxide black filter cake weight 2-3% and the quartz sand of 1-2%, 1500-2500rpm speed lapping 15-20 minute, take out after drying and add appropriate water making beating 20-25 minute, make the slurries that concentration is 55-60%, and add the Union carbide A-162 of slurry weight 4-6%, the dimethyldiethoxysilane of 2-3%, the phenyl triethoxysilane of 5-8% and the hollow float bead of 0.3-0.4%, heating in water bath is to 60-70 ℃, stir 2-3h, be less than 40 μ m by colloidal mill defibrination to particle diameter again, filter, oven dry is beaten powder and is finished product.
Beneficial effect of the present invention:
The present invention reacts by between oxygen Union carbide A-162, dimethyldiethoxysilane and phenyl triethoxysilane three and hollow float bead, form the resin-coated film of one deck organosilicon-hollow float bead on the iron oxide black surface, can significantly improve the high-temperature stability of iron oxide black, high temperature that can anti-500-600 ℃, nondiscoloration is colour-fast, the iron oxide black that the present invention produces has superior resistance to elevated temperatures, well resistance to acids and bases, water tolerance and the characteristics such as light absorptive is strong, tinting strength is high, consistency is good, good dispersity.
Embodiment
A kind of preparation method of organosilicon fire-resistant iron oxide black, the iron oxide black that adopts the sodium hydroxide oxidation style to make, directly use the oxidation filter cake of not drying, add the ethanolic soln that is equivalent to iron oxide black filter cake weight 2% and 1.5% quartz sand, 2000rpm speed lapping 15 minutes, take out after drying and add appropriate water making beating 20 minutes, make the slurries that concentration is 55%, and add the Union carbide A-162 of slurry weight 5%, 2% dimethyldiethoxysilane, 7% phenyl triethoxysilane and 0.3% hollow float bead, heating in water bath to 65 ℃, stir 3h, be less than 40 μ m by colloidal mill defibrination to particle diameter again, filter, oven dry is beaten powder and is finished product.
The present invention reacts by between oxygen Union carbide A-162, dimethyldiethoxysilane and phenyl triethoxysilane three and hollow float bead, form the resin-coated film of one deck organosilicon-hollow float bead on the iron oxide black surface, can significantly improve the high-temperature stability of iron oxide black, high temperature that can anti-500-600 ℃, nondiscoloration is colour-fast
The iron oxide black product performance analysis data that the present embodiment is produced is as following table:
Project Index Detected result
Fe 2O 3Content (%) ≥85 ?90.6
105 ℃ of volatile matters (%) ≤1.0 0.68
Oil number (%) 15-25 21.5
Tinctorial strength (%) 95-105 98.2
Anti-200 ℃/30min (△ E) ≤1.0 0.77

Claims (1)

1. the preparation method of an organosilicon fire-resistant iron oxide black, it is characterized in that: the iron oxide black that adopts the sodium hydroxide oxidation style to make, directly use the oxidation filter cake of not drying, add the ethanolic soln that is equivalent to iron oxide black filter cake weight 2-3% and the quartz sand of 1-2%, 1500-2500rpm speed lapping 15-20 minute, take out after drying and add appropriate water making beating 20-25 minute, make the slurries that concentration is 55-60%, and add the Union carbide A-162 of slurry weight 4-6%, the dimethyldiethoxysilane of 2-3%, the phenyl triethoxysilane of 5-8% and the hollow float bead of 0.3-0.4%, heating in water bath is to 60-70 ℃, stir 2-3h, be less than 40 μ m by colloidal mill defibrination to particle diameter again, filter, oven dry is beaten powder and is finished product.
CN201310318329.8A 2013-07-26 2013-07-26 Preparation method for organosilicone high temperature resisting black iron oxide Active CN103421355B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104031422A (en) * 2014-04-24 2014-09-10 铜陵市陵阳化工有限责任公司 Preparation method for kaolin/iron oxide black composite pigment
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
CN104312221A (en) * 2014-10-27 2015-01-28 合肥旭阳铝颜料有限公司 Heat-resisting magnetic aluminum 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

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JP4253157B2 (en) * 2002-03-27 2009-04-08 三井金属鉱業株式会社 Mg-containing black iron oxide particles and method for producing the same
CN101824236A (en) * 2010-04-29 2010-09-08 南通宝聚颜料有限公司 Preparation process of medium temperature resistant iron oxide black
CN102807775A (en) * 2012-06-21 2012-12-05 浙江理工大学 Water-proof and oil-repellent magnetic SiO2/Fe3O4 composite particles and preparation method and application thereof
CN102942842A (en) * 2012-11-09 2013-02-27 上海元方涂料有限公司 Nanoscale high temperature resisting environment-friendly paint
CN102993781A (en) * 2012-11-22 2013-03-27 嘉兴学院 Preparation method of magnetic nano ferroferric oxide modified hollow glass microsphere
CN103214907A (en) * 2013-03-14 2013-07-24 湖北大学 Aqueous microwave absorbing anticorrosion protection paint and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1538995A (en) * 2001-08-02 2004-10-20 Ĭ��ר���ɷ����޹�˾ Highly anti-corrosive metal pigments
JP4253157B2 (en) * 2002-03-27 2009-04-08 三井金属鉱業株式会社 Mg-containing black iron oxide particles and method for producing the same
CN1805086A (en) * 2006-01-23 2006-07-19 浙江大学宁波理工学院 Preparation method of silane coupled nanometer magnetic composite ferroferric oxide material
US20070277703A1 (en) * 2006-06-02 2007-12-06 Iop Specialists Sdn. Bhd. Iron oxide pigments from mill scale
CN101314678A (en) * 2008-06-20 2008-12-03 升华集团德清华源颜料有限公司 Fire resistant black iron oxide pigment and preparation method thereof
CN101824236A (en) * 2010-04-29 2010-09-08 南通宝聚颜料有限公司 Preparation process of medium temperature resistant iron oxide black
CN102807775A (en) * 2012-06-21 2012-12-05 浙江理工大学 Water-proof and oil-repellent magnetic SiO2/Fe3O4 composite particles and preparation method and application thereof
CN102942842A (en) * 2012-11-09 2013-02-27 上海元方涂料有限公司 Nanoscale high temperature resisting environment-friendly paint
CN102993781A (en) * 2012-11-22 2013-03-27 嘉兴学院 Preparation method of magnetic nano ferroferric oxide modified hollow glass microsphere
CN103214907A (en) * 2013-03-14 2013-07-24 湖北大学 Aqueous microwave absorbing anticorrosion protection paint and preparation method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104031422A (en) * 2014-04-24 2014-09-10 铜陵市陵阳化工有限责任公司 Preparation method for kaolin/iron oxide black composite pigment
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
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
CN104031422B (en) * 2014-04-24 2015-12-30 安徽陵阳新材料有限公司 The preparation method of a kind of kaolin/iron oxide black composite pigment
CN104312221A (en) * 2014-10-27 2015-01-28 合肥旭阳铝颜料有限公司 Heat-resisting magnetic aluminum 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
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

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