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CN1709985A - Method for producing iron oxide black - Google Patents

Method for producing iron oxide black Download PDF

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Publication number
CN1709985A
CN1709985A CN 200510075112 CN200510075112A CN1709985A CN 1709985 A CN1709985 A CN 1709985A CN 200510075112 CN200510075112 CN 200510075112 CN 200510075112 A CN200510075112 A CN 200510075112A CN 1709985 A CN1709985 A CN 1709985A
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Prior art keywords
iron oxide
black
ferrous
oxide black
salt water
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CN 200510075112
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CN100352866C (en
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刘世琦
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Hubei Wanrun New Energy Technology Co Ltd
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  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

This is the producing method of a kind of oxidized iron oxide black including following contents: prepare ferrite watery solution; use sodium hydroxide as neutralizaing agent and react with ferrite watery solution to produce hydroxide ferrous; use oxygenous gas as oxidant, and react with said hydroxide ferrous to produce iron oxide black; make the prepared iron oxide black water washed, sieved, dried and comminuted orderly to get blue oxidized iron oxide black pigment product. The oxidized iron oxide black produced by this method has high purity and thin crystal grain, the grain size of produced pigment is thin and even, and has saturated blue ink light black and stable effect to light and atmosphere. It also has strong pigmentation strength and hiding power, and can be used in such fine chemical industry products as printing ink and carbon powder. The farther project is using waste residue containing ferrous sulfate and vented in titanium oxide powder production, to produce ferrous sulfate watery solution and produce oxidized iron oxide black, which can adequately use industry waste material to produce oxidized iron oxide black products of high quality, and reduce environmental pollution.

Description

Production method of iron oxide black
Technical Field
The invention belongs to a production method of a pigment, and particularly relates to a production method of iron oxide black.
Background
Iron oxide black, abbreviated as iron black, has a molecular formula of Fe3O4Or Fe2O3FeO, known under the chemical name ferriferrous oxide, is of the spinel type and can also be called ferrous ferrite and used in combinationThe structural formula is shown.
Iron oxide black is widely used in the fields of paint, building material, cement industry coloring and the like due to strong covering power, tinting strength and good light resistance, and is also widely used in the fields of printing ink, printing, plastic coloring, polishing, metal flaw detection and the like. The prior art generally uses a direct addition method, namely, leftover bits and pieces for producing iron oxide red or iron oxide yellow are used as raw materials, and iron oxide black is generated by addition and dehydration under certain process conditions. In addition, in the existing titanium dioxide production, 3-4 tons of waste residues containing ferrous sulfate can be generated when one ton of titanium dioxide is produced, and serious environmental pollution is caused.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for producing iron oxide black with high purity, fine and uniform particle size, high tinting strength and blue phase characteristic.
The technical problem to be further solved by the invention is
The technical scheme for solving the problems is as follows:
1. preparing a ferrous salt aqueous solution;
2. using caustic soda as a neutralizing agent to react with a ferrous salt aqueous solution to generate ferrous hydroxide;
3. using oxygen-containing gas as oxidant, making it and the above-mentioned ferrous hydroxide undergo the oxidation reaction to produce iron black;
4. and sieving, filter pressing, rinsing, drying and crushing the generated iron oxide black to obtain a blue-phase iron oxide black pigment product.
The ferrous salt aqueous solution can be ferrous sulfate aqueous solution prepared by refining and removing impurities from ferrous sulfate-containing waste slag discharged from titanium dioxide production, or pure ferrous aqueous solution obtained by treating pickling waste liquid in the steel industry;
the concentration of the ferrous salt aqueous solution is preferably 5-50%, and the preferable scheme is that the content of the ferrous salt is 40-50%;
the neutralizing agent caustic soda comprises liquid alkali, solid alkali, flake alkali and the like, and the pH value of the neutralized gel is 7.5-9;
the oxygen-containing gas may be air or other oxygen-containing gas.
The oxidation reaction condition of item 3 is that the oxidation reaction is carried out at a temperature of 90-102 ℃ and a pH value of 7.5-9.
The further scheme of the invention is a method for producing iron oxide black by using waste residues produced in titanium dioxide production as raw materials:
the method is characterized in that: the preparation method of the ferrous salt water solution comprises the following steps:
waste slag particles containing ferrous sulfate discharged from titanium dioxide production are put into water to be heated and fully dissolved, wherein, the impurity titanyl sulfate is hydrolyzed into metatitanic acid precipitate, and after sedimentation separation, clear liquid is taken as ferrous salt water solution for producing iron oxide black.
The method of the invention is a liquid phase production method, the produced iron oxide black has high purity and fine crystal grains, and the prepared pigment has fine and uniform grain diameter, has the blue phase characteristic of saturated blue ink light black, has stable light and atmosphere action, strong tinting strength and strong covering power, and can be used for fine chemical products such as printing ink, carbon powder and the like.
The further scheme of the invention is a method for producing the iron oxide black by using the waste residues generated in the production of the titanium dioxide as the raw materials, can fully utilize industrial waste materials to produce high-quality iron oxide black products, and reduces the environmental pollution.
Detailed Description
Example 1
The method for producing the blue-phase black iron oxide pigment comprises the following steps:
1. putting waste residue containing ferrous sulfate discharged in titanium dioxide production into a dissolving tank, heating by steam, fully dissolving, standing for settling, taking supernatant liquid on the upper part of the dissolving tank to prepare 2000Kg of ferrous sulfate aqueous solution with the concentration of 45%, and putting the ferrous sulfate aqueous solution into a reaction container;
2. adding about 865Kg of liquid caustic soda with 30% of neutralizing agent into ferrous sulfate aqueous solution while stirring to generate ferrous hydroxide, wherein the pH value of the system is 8.5;
3. pumping the prepared ferrous hydroxide into a 5000L reaction tank, controlling the temperature at 95 deg.C and pH at about 8.5 with steam, and introducing water at a flow rate of 0.3m while stirring3Performing oxidation reaction in air for/min to generate iron oxide black;
the reaction formulas of the steps 2 and 3 are as follows:
4. sieving a wet material: sieving the slurry obtained in the step 3, wherein the mesh number of the sieve is 320 meshes;
5. filter pressing and water washing: putting the sieved substance into a washing tank for washing and then filtering;
6. drying the filtrate obtained in the step 5;
7. and crushing the dried substance to obtain the blue-phase iron oxide black pigment.
The product of this example was tested to contain Fe3O496.5 percent; the tinting strength was 160% compared to industry-specified standards.
The following are the main technical data of the production process of examples 2 to 4:
example 2 example 3 example 4
30 percent of ferrous salt aqueous solution (concentration), 40 percent of ferrous salt aqueous solution and 50 percent of ferrous salt aqueous solution
Neutralizer solid caustic soda 42% liquid caustic soda 30% liquid caustic soda
pH 7.589 after neutralization
Oxidation reaction temperature 9095100
Oxidation pH 7.589
The products produced in examples 2 to 4 all had substantially the same effects as in example 1.

Claims (9)

1. The production method of the iron oxide black is characterized by comprising the following steps:
(1) to prepare ferrous salt water solution;
(2) reacting with ferrous salt water solution by using caustic soda as a neutralizing agent to generate ferrous hydroxide;
(3) using oxygen-containing gas as oxidant to make oxidation reaction with the above-mentioned ferrous hydroxide to produce iron black;
(4) and sieving, filter-pressing, rinsing, drying and crushing the generated iron oxide black to obtain the blue-phase iron oxide black pigment product.
2. The method for producing black iron oxide according to claim 1, characterized in that: the preparation method of the ferrous salt water solution comprises the following steps: waste slag particles containing ferrous sulfate discharged from titanium dioxide production are put into water to be heated and fully dissolved, wherein, the impurity titanyl sulfate is hydrolyzed into metatitanic acid precipitate, and after sedimentation separation, clear liquid is taken as ferrous salt water solution for producing iron oxide black.
3. The method for producing iron oxide black according to claim 1 or 2, characterized in that: the oxidation reaction condition is that the oxidation reaction is carried out at the temperature of 90-102 ℃ and the PH value of 7.5-9.
4. The method for producing iron oxide black according to claim 1 or 2, characterized in that: the concentration of the ferrous salt water solution is 5-50%.
5. The method for producing black iron oxide according to claim 3, characterized in that: the concentration of the ferrous salt water solution is 5-50%.
6. The method for producing iron oxide black according to claim 1 or 2, characterized in that: the pH value of ferrous hydroxide gel generated by neutralizing the ferrous salt water solution and caustic soda is 7.5-9.
7. The method for producing black iron oxide according to claim 3, characterized in that: the pH value of ferrous hydroxide gel generated by neutralizing the ferrous salt water solution and caustic soda is 7.5-9.
8. The method for producing black iron oxide according to claim 4, wherein: the pH value of ferrous hydroxide gel generated by neutralizing the ferrous salt water solution and caustic soda is 7.5-9.
9. The method for producing black iron oxide according to claim 5, wherein: the pH value of ferrous hydroxide gel generated by neutralizing the ferrous salt water solution and caustic soda is 7.5-9.
CNB2005100751124A 2005-06-08 2005-06-08 Method for producing iron oxide black Active CN100352866C (en)

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101538420B (en) * 2008-03-21 2012-02-22 北京康之维科技有限公司 Method and equipment for shearing-cycling stirring type iron oxide orange production
CN102502878A (en) * 2011-10-18 2012-06-20 山西大同大学 Method for preparing nano iron oxide black pigment from dust
CN102502875A (en) * 2011-10-11 2012-06-20 安徽明珠颜料科技有限公司 Method for synthersizing iron oxide black by taking lime as raw material
CN102604434A (en) * 2012-02-21 2012-07-25 升华集团德清华源颜料有限公司 Preparation method of coated iron oxide black with medium temperature resistance
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
CN104071852A (en) * 2013-03-25 2014-10-01 北京三聚环保新材料股份有限公司 Preparation process for iron oxide black
CN104108814A (en) * 2014-07-22 2014-10-22 四川龙蟒钛业股份有限公司 Method for treating rutile titanium dioxide waste water
CN104386761A (en) * 2014-11-13 2015-03-04 常熟铁红厂有限公司 Preparation method of high-tinting-strength iron oxide black paint
CN105086517A (en) * 2015-07-27 2015-11-25 安徽明珠颜料科技有限公司 Ferric oxide black pigment with refreshing and consciousness-restoring functions and preparation method thereof
CN104016418B (en) * 2014-06-27 2016-01-20 四川金沙纳米技术有限公司 Titanium dioxide waste residue ferrous sulfate is utilized to prepare the method for iron oxide black fast
CN107200359A (en) * 2016-03-17 2017-09-26 北京中金瑞丰环保科技有限公司 A kind of iron oxide pigment and its production method
CN113772741A (en) * 2021-09-06 2021-12-10 江苏宇星科技有限公司 Method for producing iron oxide black by liquid phase synthesis
CN116425207A (en) * 2022-01-04 2023-07-14 宜兴华谊一品着色科技有限公司 Preparation method of high blue phase iron oxide black

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5202043A (en) * 1985-01-09 1993-04-13 Bayer Aktiengesellschaft Process for the preparation of isometric magnetic iron oxide
CN1590304A (en) * 2003-09-05 2005-03-09 李景钞 Comprehensive utilization method of ferrous sulfate waste water and waste iron scraps
CN1218882C (en) * 2003-12-03 2005-09-14 南京工业大学 High-hysteresis heat generating capacity iron oxide magnetic powder for tumor magnetic thermotherapy and preparation method thereof

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101538420B (en) * 2008-03-21 2012-02-22 北京康之维科技有限公司 Method and equipment for shearing-cycling stirring type iron oxide orange production
CN102502875A (en) * 2011-10-11 2012-06-20 安徽明珠颜料科技有限公司 Method for synthersizing iron oxide black by taking lime as raw material
CN102502878A (en) * 2011-10-18 2012-06-20 山西大同大学 Method for preparing nano iron oxide black pigment from dust
CN102604434A (en) * 2012-02-21 2012-07-25 升华集团德清华源颜料有限公司 Preparation method of coated iron oxide black with medium temperature resistance
CN102604434B (en) * 2012-02-21 2013-11-06 升华集团德清华源颜料有限公司 Preparation method of coated iron oxide black with medium temperature resistance
CN104071852B (en) * 2013-03-25 2016-03-30 北京三聚环保新材料股份有限公司 A kind of preparation technology of iron oxide black
CN104071852A (en) * 2013-03-25 2014-10-01 北京三聚环保新材料股份有限公司 Preparation process for iron oxide black
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
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
CN104016418B (en) * 2014-06-27 2016-01-20 四川金沙纳米技术有限公司 Titanium dioxide waste residue ferrous sulfate is utilized to prepare the method for iron oxide black fast
CN104108814A (en) * 2014-07-22 2014-10-22 四川龙蟒钛业股份有限公司 Method for treating rutile titanium dioxide waste water
CN104108814B (en) * 2014-07-22 2016-03-30 四川龙蟒钛业股份有限公司 A kind of method processing Rutile type Titanium Dioxide waste water
CN104386761A (en) * 2014-11-13 2015-03-04 常熟铁红厂有限公司 Preparation method of high-tinting-strength iron oxide black paint
CN105086517A (en) * 2015-07-27 2015-11-25 安徽明珠颜料科技有限公司 Ferric oxide black pigment with refreshing and consciousness-restoring functions and preparation method thereof
CN107200359A (en) * 2016-03-17 2017-09-26 北京中金瑞丰环保科技有限公司 A kind of iron oxide pigment and its production method
CN113772741A (en) * 2021-09-06 2021-12-10 江苏宇星科技有限公司 Method for producing iron oxide black by liquid phase synthesis
CN116425207A (en) * 2022-01-04 2023-07-14 宜兴华谊一品着色科技有限公司 Preparation method of high blue phase iron oxide black

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Assignee: Hubei Wan run industry and Trade Development Co., Ltd.

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