CN1807263A - Method for producing iron oxide black using desilicified mud cake - Google Patents
Method for producing iron oxide black using desilicified mud cake Download PDFInfo
- Publication number
- CN1807263A CN1807263A CN 200610024039 CN200610024039A CN1807263A CN 1807263 A CN1807263 A CN 1807263A CN 200610024039 CN200610024039 CN 200610024039 CN 200610024039 A CN200610024039 A CN 200610024039A CN 1807263 A CN1807263 A CN 1807263A
- Authority
- CN
- China
- Prior art keywords
- iron oxide
- iron
- desiliconized
- mud
- mud cake
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The disclosed preparation method for Fe2O3 black with desilicated mud cake as material comprises: (1) preparing Fe2+ solution; (2) preparing ferrite-yellow crystal seed; (3) pre-treating the desilicated mud cake; (4) oxidating and slurrying; (5) composing; (6) screening; (7) pressure filtering; (8) drying; (9) checking and packing. This invention is simple, and has low request to the device and little side reaction.
Description
Technical Field
The invention relates to a production method of an inorganic pigment, in particular to a method for producing iron oxide black by using a byproduct desilicated mud cake obtained after utilizing pickling waste liquor of a steel mill as a raw material.
Background
The desiliconized mud cake produced in cold rolling mill is the filtering waste material produced by desiliconizing apparatus when the waste acid produced after pickling steel plate is used to produce magnetic iron oxide red. The dry desiliconized mud cake is in the shape of block, yellowish red and mud block, the total iron content is 50-65% after drying at 100 ℃, the screen residue is less than or equal to 0.2%, and the particle fineness of the mud cakeGood results are obtained. The main component is Fe (OH)3、Fe(OH)2And water, and about 1% SiO2And FeO.
A large cold rolling steel mill can produce nearly ten thousand tons of desiliconized mud cakes every year, and becomes an important subject of comprehensive treatment of the steel mill.
On the other hand, the existing production of iron oxide black Fe3O4The method mostly adopts a solution precipitation method of precipitating iron oxide black by reacting a ferrous sulfate solution with soda ash. The method is divided into a synthetic method and an oxidation method. The synthesis method comprises the steps of performing addition reaction on ferric oxide and ferrous oxide, wherein ferric oxide is used for ferric oxide or ferric oxide, ferrous hydroxide is used for ferrous oxide, the ferric oxide and the ferrous oxide are mixed by a wet method and then are subjected to addition reaction directly, and the mixture is dehydrated to generate iron oxide black. The oxidation method comprises the steps of putting a ferrous sulfate solution and a sodium hydroxide solution into a reaction kettle to generate ferrous hydroxidesol, introducing steam for heating, controlling the pH value for reaction, and putting ammonium nitrate when the color light is close to the end point to prepare the iron oxide black. The traditional solution precipitation method has high requirements on raw materials, single product variety and high raw material cost.
Disclosure of Invention
The invention aims to provide a method for producing iron oxide black by adopting desiliconized mud cakes, which utilizes the desiliconized mud cakes made from the pickling waste liquid of a steel mill as a raw material, integrates two processes in the traditional solution precipitation method, and adopts an oxidation synthesis method to produce the iron oxide black, thereby not only solving the problem of treatment of the desiliconized mud cakes made from the pickling waste liquid of the steel mill, but also reducing the cost for producing the iron oxide black.
The invention relates to a method for producing iron oxide black by taking desiliconized mud cakes as raw materials, which comprises the following steps:
(1) preparing a ferrous solution: putting the pickling waste liquid containing ferrous sulfate and residual sulfuric acid into a reaction kettle, adding sufficient thin iron materials, introducing steam, heating to 60-70 ℃, fully reacting the residual sulfuric acid in the waste liquid with iron, and controlling the pH value of the solution to be 4-5 to prepare a ferrous sulfate solution; the chemical reaction formula is as follows: ；
(2) preparing iron oxide yellow seed crystal: pumping the ferrous solution prepared in the step (1) into a reaction kettle, and adding the ferrous solution with the concentration of25 to 35 percent of liquid alkali, introducing air, adjusting the pH value to 4.5 to 5.5, and preparing the iron yellow seed crystal Fe2O3·H2O; the chemical reaction formula is as follows:
(3) pretreating desiliconized mud cakes: adding water into the desiliconized mud cake, heating and pulping, heating and rinsing, filtering to remove impurities, and pulping to prepare desiliconized mud material;
(4) oxidizing and pulping: pumping the pretreated desiliconized sludge into a reaction kettle, adding the iron yellow seed crystal prepared in the step (2) and sufficient thin iron material, introducing steam and air, and reacting to obtain the product with the main component of Fe2O3·H2Desilicated iron oxide yellow slurry of O;
(5) synthesizing: pumping the iron oxide yellow slurry prepared in the step (4) into a reaction kettle, adding the ferrous solution obtained in the step (1), adding liquid alkali with the concentration of 25-35%, introducing steam and air, controlling the reaction temperature at 90-100 ℃, controlling the pH value to 8-9, and preparing iron oxide black Fe after reaction3O4A slurry having the chemical reaction formula:
(6) sieving: sieving the prepared iron oxide black slurry by a 300-mesh sieving machine;
(7) and (3) filter pressing: pumping the sieved slurry into a plate-and-frame filter press for filter pressing and rinsing to obtain an iron oxide black solid phase substance;
(8) drying: putting the iron oxide black solid phase substance obtained in the step (7) into an oven for drying to obtain an iron oxide black finished product with the water content of less than 1%;
(9) and (6) inspecting and packaging.
The invention has the following effects: the iron oxide black is produced by taking the desiliconized mud cake of the pickling waste liquid of the steel mill as a raw material, the oxidation synthesis method is adopted, the oxidation and synthesis process in the traditional solution precipitation method is integrated, and the process has the characteristics of simplicity, low requirement on equipment, less side reaction, effective comprehensive utilization of the desiliconized mud cake of the pickling waste liquid of the steel mill and the like. The iron oxide black prepared by the method has excellent performance and low production cost.
Detailed description of the preferred embodiments
Examples
Preparing ferrous solution and ferrite yellow seed crystal.
Desiliconizing mud cake treatment: 1000kg of desilicated mud cakes containing 30 percent of water are taken and added into a mud cake pulping kettle, water is added and dispersed while adding, the stirring speed of the pulping kettle is 45 r/min, when the capacity of the pulping kettle reaches 50 percent, steam is introduced, the temperature of liquid is ensured to reach 80 ℃, and the mud cakes are stirred for 2 hours to be fully dispersed into slurry. Then pumping the slurry into a filter press for rinsing by hot water, and then putting the filter press into another pulping kettle for pulping.
Oxidizing and pulping: pumping the treated slurry of the two-kettle mud cake into a pump with the diameter of 50m3The iron oxide yellow reaction kettle is filled with 9m3Adding a proper amount of water into the iron oxide yellow seed crystal slurry, adding enough thin iron materials in time, controlling the reaction temperature, ensuring the final heat preservation temperature of 85 ℃, and preparing the iron oxide yellow seed crystal slurry into 40m after oxidation reaction for 40 hours35.6t of mud cake iron yellow and 2.4t of ferrous iron are calculated by dry basis.
Synthesizing: take 20m3The iron oxide yellow slurry is pumped into an iron oxide black reaction kettle, the dry content is 2.8 tons, and according to the weight of the yellow iron oxide dry of the mud cake, 7m of ferrous iron is added in batches according to the proportion of 1: 1.56 to 100g/100ml of ferrous iron330% ofIntroducing steam into the iron solution to raise the temperature, adding liquid alkali to neutralize, introducing air, controlling the reaction temperature to be higher than 95 ℃, reacting and preserving the temperature for a period of time, and dehydrating the solution to generate iron oxide black slurry.
Sieving, filter pressing, rinsing and drying: discharging, sieving by a 300-mesh sieve, performing filter pressing and rinsing, and controlling the screen residue and the conductivity of the slurry. Iron black filter cake (main component Fe) after filter pressing3O4) Sending the mixture to an oven for drying to obtain 3636Kg iron oxide black finished product.
The product quality evaluation adopts the chemical industry standard: HG/T2250-91. And the measurement can meet and exceed the standard requirement.
Claims (4)
1. A method for producing iron oxide black by using desiliconized mud cakes comprises the following steps:
(1) preparing a ferrous solution: putting the pickling waste liquid containing ferrous sulfate and residual sulfuric acid into a reaction kettle, adding sufficient thin iron materials, introducing steam, heating to 60-70 ℃, fully reacting the residual sulfuric acid in the waste liquid with iron, and controlling the pH value of the solution to be 4-5 to prepare a ferrous sulfate solution; the chemical reaction formula is as follows: ；
(2) preparing iron oxide yellow seed crystal: pumping the ferrous solution prepared in the step (1) into a reaction kettle, adding liquid alkali with the concentration of 25-35%, introducing air, adjusting the pH value to 4.5-5.5, and preparing the iron oxide yellow seed crystal Fe2O3·H2O; the chemical reaction formula is as follows:
(3) pretreating desiliconized mud cakes: adding water into the desiliconized mud cake, heating and pulping, heating and rinsing, filtering to remove impurities, and pulping to prepare desiliconized mud material;
(4) oxidizing and pulping: pumping the pretreated desiliconized sludge into a reaction kettle, adding the iron yellow seed crystal prepared in the step (2) and sufficient thin iron material, introducing steam and air, and reacting to obtain the product with the main component of Fe2O3·H2Desilicated iron oxide yellow slurry of O;
(5) synthesizing: pumping the iron oxide yellow slurry prepared in the step (4) into a reaction kettle, adding the ferrous solution obtained in the step (1), adding liquid alkali with the concentration of 25-35%, introducing steam and air, controlling the reaction temperature at 90-100 ℃, controlling the pH value to 8-9, and preparing iron oxide black Fe after reaction3O4A slurry having the chemical reaction formula:
(6) sieving: sieving the prepared iron oxide black slurry by a 200-mesh sieving machine;
(7) and (3) filter pressing: pumping the sieved slurry into a plate-and-frame filter press for filter pressing and rinsing to obtain an iron oxide black solid phase substance;
(8) drying: putting the iron oxide black solid phase substance obtained in the step (7) into an oven for drying to obtain an iron oxide black finished product with the water content of less than 1%;
(9) and (6) inspecting and packaging.
2. The method for producing black iron oxide from desilicated mud cake as set forth in claim 1, wherein: the desiliconized mud cake is in a block shape, yellow red and mud block shape, the total iron content after drying at 100 ℃ is 63.2 percent, and the screen residue is 0.2 percent.
3. The method for producing black iron oxide from desilicated mud cake as set forth in claim 1, wherein: wherein the oxidation reaction temperature of the step (4) is 80-90 ℃, and the reaction time is 30-50 h.
4. The method for producing black iron oxide from desilicated mud cake as set forth in claim 1, wherein: wherein the ferrous solution in the step (5) comprises the following components in percentage by weight: the ratio of desilicated ferric yellow (calculated on a dry basis) to ferrous solution (calculated as 100g/100 ml) is 1: 1.5-1.6, and the optimal addition amount is 1: 1.56.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100240392A CN100564267C (en) | 2006-02-21 | 2006-02-21 | Produce the method for iron oxide black with the desiliconization mud cake |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100240392A CN100564267C (en) | 2006-02-21 | 2006-02-21 | Produce the method for iron oxide black with the desiliconization mud cake |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1807263A true CN1807263A (en) | 2006-07-26 |
| CN100564267C CN100564267C (en) | 2009-12-02 |
Family
ID=36839389
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100240392A Expired - Fee Related CN100564267C (en) | 2006-02-21 | 2006-02-21 | Produce the method for iron oxide black with the desiliconization mud cake |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100564267C (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101560336B (en) * | 2008-04-18 | 2012-07-25 | 上海宝齐氧化铁有限公司 | Spherical iron oxide black and preparation technology thereof |
| CN102653437A (en) * | 2011-09-20 | 2012-09-05 | 卢玉柱 | Method for treating yellow sludge obtained in neutralization of steel pickling waste water lime |
| CN102689931A (en) * | 2012-06-11 | 2012-09-26 | 上海宝齐氧化铁有限公司 | Method for producing iron oxide black from desiliconized sludge cake by one-step process |
| CN102826614A (en) * | 2012-08-31 | 2012-12-19 | 长春工程学院 | Method for preparing iron oxide black by recovering iron in sludge water from biological iron and manganese removal water plant |
| CN102863029A (en) * | 2012-09-25 | 2013-01-09 | 上海应用技术学院 | Method of using acid regeneration desiliconized mud cakes to prepare superfine iron oxide red |
| CN102863030A (en) * | 2012-09-25 | 2013-01-09 | 上海应用技术学院 | Method for preparing nanometer ferroferric oxide through acid-regenerating desilicated mud cake |
| CN104495952A (en) * | 2015-01-09 | 2015-04-08 | 南通宝聚颜料有限公司 | Preparation method of high-coercivity iron black for photocopy toner |
| 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 |
| CN105435738A (en) * | 2014-08-27 | 2016-03-30 | 宝山钢铁股份有限公司 | A method of preparing a C/gamma-Fe2O3 composite material from acid-regeneration desilication mud cakes |
| CN105439211A (en) * | 2015-12-17 | 2016-03-30 | 江苏省常熟环通实业有限公司 | Energy-saving environmental-protection production method for iron oxide black pigment |
| CN106475098A (en) * | 2015-08-31 | 2017-03-08 | 宝山钢铁股份有限公司 | A kind of method that magnetic photocatalyst is prepared by acid regeneration desiliconization mud cake |
| CN109987641A (en) * | 2017-12-30 | 2019-07-09 | 天津友发钢管集团股份有限公司 | A kind of method that red soil prepares iron oxide black |
-
2006
- 2006-02-21 CN CNB2006100240392A patent/CN100564267C/en not_active Expired - Fee Related
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101560336B (en) * | 2008-04-18 | 2012-07-25 | 上海宝齐氧化铁有限公司 | Spherical iron oxide black and preparation technology thereof |
| CN102653437A (en) * | 2011-09-20 | 2012-09-05 | 卢玉柱 | Method for treating yellow sludge obtained in neutralization of steel pickling waste water lime |
| CN102653437B (en) * | 2011-09-20 | 2013-07-17 | 卢玉柱 | Method for treating yellow sludge obtained in neutralization of steel pickling waste water lime |
| CN102689931A (en) * | 2012-06-11 | 2012-09-26 | 上海宝齐氧化铁有限公司 | Method for producing iron oxide black from desiliconized sludge cake by one-step process |
| CN102689931B (en) * | 2012-06-11 | 2014-05-14 | 上海宝齐氧化铁有限公司 | Method for producing iron oxide black from desiliconized sludge cake by one-step process |
| CN102826614B (en) * | 2012-08-31 | 2014-03-05 | 长春工程学院 | Method for preparing iron oxide black by recovering iron in sludge water from biological iron and manganese removal water plant |
| CN102826614A (en) * | 2012-08-31 | 2012-12-19 | 长春工程学院 | Method for preparing iron oxide black by recovering iron in sludge water from biological iron and manganese removal water plant |
| CN102863029A (en) * | 2012-09-25 | 2013-01-09 | 上海应用技术学院 | Method of using acid regeneration desiliconized mud cakes to prepare superfine iron oxide red |
| CN102863030A (en) * | 2012-09-25 | 2013-01-09 | 上海应用技术学院 | Method for preparing nanometer ferroferric oxide through acid-regenerating desilicated mud cake |
| CN102863030B (en) * | 2012-09-25 | 2014-07-30 | 上海应用技术学院 | Method for preparing nanometer ferroferric oxide through acid-regenerating desilicated mud cake |
| 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 |
| CN105435738A (en) * | 2014-08-27 | 2016-03-30 | 宝山钢铁股份有限公司 | A method of preparing a C/gamma-Fe2O3 composite material from acid-regeneration desilication mud cakes |
| CN105435738B (en) * | 2014-08-27 | 2018-10-02 | 宝山钢铁股份有限公司 | A kind of acid regeneration desiliconization mud cake preparation C/ γ-Fe2O3The method of composite material |
| CN104495952A (en) * | 2015-01-09 | 2015-04-08 | 南通宝聚颜料有限公司 | Preparation method of high-coercivity iron black for photocopy toner |
| CN104495952B (en) * | 2015-01-09 | 2016-02-17 | 南通宝聚颜料有限公司 | A kind of preparation method of photocopy toner high-coercive force iron oxide black |
| CN106475098A (en) * | 2015-08-31 | 2017-03-08 | 宝山钢铁股份有限公司 | A kind of method that magnetic photocatalyst is prepared by acid regeneration desiliconization mud cake |
| CN106475098B (en) * | 2015-08-31 | 2019-04-23 | 宝山钢铁股份有限公司 | A method of magnetic photocatalyst is prepared by acid regeneration desiliconization mud cake |
| CN105439211A (en) * | 2015-12-17 | 2016-03-30 | 江苏省常熟环通实业有限公司 | Energy-saving environmental-protection production method for iron oxide black pigment |
| CN109987641A (en) * | 2017-12-30 | 2019-07-09 | 天津友发钢管集团股份有限公司 | A kind of method that red soil prepares iron oxide black |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100564267C (en) | 2009-12-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1807263A (en) | Method for producing iron oxide black using desilicified mud cake | |
| US5961941A (en) | Production of precipitated calcium carbonate from papermaking sludge and sludge-derived ash | |
| CN1709985A (en) | Method for producing iron oxide black | |
| CN101434970A (en) | Double decomposition precipitation transformation production method of potassium citrate | |
| CN109647351B (en) | Bagasse loaded iron hydroxide adsorbent and preparation method and application thereof | |
| CN111704143A (en) | Production process for preparing composite calcium silicate by using rice hull ash | |
| CN112520772A (en) | Method for producing high-purity colorless transparent polyaluminum chloride by using aluminum ash | |
| CN1807252A (en) | Preparation method of nanometer grade active calcium carbonate special for sealing material | |
| CN114749148B (en) | Composite modified banana peel biochar and preparation method and application thereof | |
| CN102910676A (en) | Preparation method of high-purity vanadium pentoxide | |
| CN109824076B (en) | Process for preparing calcium carbonate by bubble membrane method and application thereof | |
| CN1923708A (en) | Producing method of iron oxide yellow pigment | |
| CN111874935B (en) | Preparation method of large-particle calcium carbonate | |
| CN1200049C (en) | Method for preparing high-white ness nano calcium carbide | |
| CN110776004B (en) | Method for recovering soluble titanium dioxide in titanium dioxide waste acid | |
| CN1063730C (en) | Technology for producing magnesium sulfate in treatment of titanium white waste sulfuric acid | |
| CN103641145A (en) | High-whiteness barium sulfate and preparation method thereof | |
| CN115652676B (en) | Green liquid silicon removal process for pre-stage silicon removal process | |
| CN110894066A (en) | Method for preparing sheet iron phosphate from titanium dioxide slag | |
| CN103011230B (en) | Low-cost method for preparing nano calcium sulfate | |
| CN115770550A (en) | Modified activated carbon and clay mixed decolorant and application thereof in refining crude oil of lubricating oil | |
| CN1410352A (en) | Comprehensive utilization method of converting chromium slag totally into light magnesium carbonate and fine iron breeze | |
| CN1198402A (en) | Telchnological process of sodium method producing bleaching powder extract | |
| CN113479921A (en) | Preparation method of high-purity calcium hydroxide | |
| CN103523813A (en) | Industrial preparation method of producing nano calcium carbonate by recycling filter-pressing water |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20091202 Termination date: 20110221 |