CN103421355B - 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
CN103421355B
CN103421355B CN201310318329.8A CN201310318329A CN103421355B CN 103421355 B CN103421355 B CN 103421355B CN 201310318329 A CN201310318329 A CN 201310318329A CN 103421355 B CN103421355 B CN 103421355B
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iron oxide
weight
black iron
seriflux
high temperature
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CN103421355A (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 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 features such as inorganic iron series pigments is nontoxic with it, odorless, pollution-free constantly replace pigment dyestuff and the plumbous series such as red lead, lead-chrome yellow, the serial poisonous mineral dye of chromium.Iron oxide black due to chemical composition simple, nontoxic pollution-free, chemical stability is strong, is widely used in building trade paint.But iron oxide black will dewater when temperature reaches about 100 DEG C, oxidation becomes iron oxide red.Under the occasion that some temperature are higher, use iron oxide black, will fade, the phenomenon such as variable color, thus limit 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, water-tolerant, 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, adopt the iron oxide black that sodium hydroxide oxidation style is obtained, the oxidation filter cake that direct use is not dried, add and be equivalent to the ethanolic soln of 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 DEG C, stir 2-3h, 40 μm are less than again by colloidal mill defibrination to particle diameter, filter, oven dry is beaten powder and is finished product.
Beneficial effect of the present invention:
The present invention is by oxygen Union carbide A-162, dimethyldiethoxysilane and react between phenyl triethoxysilane three and hollow float bead, the resin-coated film of one deck organosilicon-hollow float bead is formed on iron oxide black surface, the high-temperature stability of iron oxide black can be significantly improved, can the high temperature of resistance to 500-600 DEG C, nondiscoloration is colour-fast, the iron oxide black that the present invention produces has superior resistance to elevated temperatures, the features such as good resistance to acids and bases, water tolerance and light absorptive are strong, tinting strength is high, consistency is good, good dispersity.
Embodiment
A kind of preparation method of organosilicon fire-resistant iron oxide black, adopt the iron oxide black that sodium hydroxide oxidation style is obtained, the oxidation filter cake that direct use is not dried, add and be equivalent to the ethanolic soln of iron oxide black filter cake weight 2% and the quartz sand of 1.5%, 2000rpm speed lapping 15 minutes, add appropriate water after taking out oven dry to pull an oar 20 minutes, make the slurries that concentration is 55%, and add the Union carbide A-162 of slurry weight 5%, the dimethyldiethoxysilane of 2%, the phenyl triethoxysilane of 7% and the hollow float bead of 0.3%, heating in water bath to 65 DEG C, stir 3h, 40 μm are less than again by colloidal mill defibrination to particle diameter, filter, oven dry is beaten powder and is finished product.
The present invention is by oxygen Union carbide A-162, dimethyldiethoxysilane and react between phenyl triethoxysilane three and hollow float bead, the resin-coated film of one deck organosilicon-hollow float bead is formed on iron oxide black surface, the high-temperature stability of iron oxide black can be significantly improved, can the high temperature of resistance to 500-600 DEG C, 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 DEG C of volatile matters (%) ≤1.0 0.68
Oil number (%) 15-25 21.5
Tinctorial strength (%) 95-105 98.2
Resistance to 200 DEG C/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: adopt the iron oxide black that sodium hydroxide oxidation style is obtained, the oxidation filter cake that direct use is not dried, add and be equivalent to the ethanolic soln of 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 DEG C, stir 2-3h, 40 μm are less than again by colloidal mill defibrination to particle diameter, 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 examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
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
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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JP3581339B2 (en) * 2001-08-02 2004-10-27 メルク株式会社 High corrosion-resistant flaky metal pigment, method for producing the same, and metallic luster interference coloring pigment based on the same
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
CN1805086B (en) * 2006-01-23 2010-07-28 浙江大学宁波理工学院 Preparation method of silane coupled nanometer magnetic composite ferroferric oxide material
US7347893B2 (en) * 2006-06-02 2008-03-25 Iop Specialists Sdn. Bhd. Iron oxide pigments from mill scale
CN101314678B (en) * 2008-06-20 2011-08-03 升华集团德清华源颜料有限公司 Fire resistant black iron oxide pigment and preparation method thereof
CN101824236B (en) * 2010-04-29 2012-10-31 南通宝聚颜料有限公司 Preparation process of medium temperature resistant iron oxide black
CN102807775B (en) * 2012-06-21 2014-03-12 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
CN102993781B (en) * 2012-11-22 2014-05-21 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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