CN100352866C - Method for producing iron oxide black - Google Patents
Method for producing iron oxide black Download PDFInfo
- Publication number
- CN100352866C CN100352866C CNB2005100751124A CN200510075112A CN100352866C CN 100352866 C CN100352866 C CN 100352866C CN B2005100751124 A CNB2005100751124 A CN B2005100751124A CN 200510075112 A CN200510075112 A CN 200510075112A CN 100352866 C CN100352866 C CN 100352866C
- Authority
- CN
- China
- Prior art keywords
- iron oxide
- oxide black
- ferrous
- oxidized iron
- hydroxide
- 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.)
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000000049 pigment Substances 0.000 claims abstract description 10
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 9
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 9
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 9
- 235000010215 titanium dioxide Nutrition 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 8
- 239000002699 waste material Substances 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010298 pulverizing process Methods 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 8
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims description 7
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000003916 acid precipitation Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 238000007639 printing Methods 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000012847 fine chemical Substances 0.000 abstract description 2
- 229920006395 saturated elastomer Polymers 0.000 abstract description 2
- 238000007873 sieving Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract 2
- 229910000859 α-Fe Inorganic materials 0.000 abstract 2
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000002440 industrial waste Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 238000010186 staining Methods 0.000 abstract 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000004040 coloring Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 241000233855 Orchidaceae Species 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
Abstract
The present invention relates to a method for producing oxidized iron oxide black, which comprises the following contents: preparing a ferrite watery solution; using sodium hydroxide as a neutralizing agent for reacting with a ferrite watery solution to produce hydroxide ferrous; using oxygenous gas as an oxidant for reacting with the hydroxide ferrous to produce iron oxide black; sieving, filtering, washing, drying and pulverizing the prepared iron oxide black to obtain a blue oxidized iron oxide black pigment product. The oxidized iron oxide black produced by the method has the advantages of high purity and thin crystal grain, the grain size of produced pigment particles is thin and uniform, and the produced pigment particles have a saturated blue ink light black color and stable action on light and atmosphere. The present invention having high staining performance and high hiding power can be used for fine chemical engineering products, such as printing ink, carbon powder, etc. In the further scheme of the present invention, waste residues containing ferrous sulfate discharged in the production of titanium white powder are used for producing a ferrous sulfate water solution so as to produce oxidized iron oxide black, industrial waste materials can be fully used for producing high-quality oxidized iron oxide black products, and environmental pollution is reduced.
Description
Technical field
The invention belongs to a kind of production method of pigment, be specifically related to a kind of production method of iron oxide black.
Background technology
Iron oxide black is called for short iron black, and molecular formula is Fe
3O
4, or Fe
2O
3.FeO, chemical name is a Z 250, belongs to spinel type, also can be described as the ferrous and usefulness of ferrous acid
Structural formula is represented.
Iron oxide black is because of opacifying power, strong coloring force, and light fastness is good and be widely used in fields such as paint, building materials, cement industry be painted, is widely used in fields such as printing ink, printing, coloring plastic, polishing and metal defect detection in addition.Prior art is generally used the direct addition method, be raw material promptly with the tankage of producing iron oxide red or iron oxide yellow, addition under certain processing condition, dehydration and generate the iron oxide black, the shortcoming of this technology is that the simple particle shape of the iron black product of gained is inconsistent, particle diameter is big and distribute very inhomogeneous, make red partially phase of form and aspect or yellow phase behind the pigment, fullness of shade and tinting strength are lower.In the existing in addition titanium white production, one ton of titanium dioxide of every production can produce the waste residue that the 3-4 ton contains ferrous sulfate, causes serious environmental to pollute.
Summary of the invention
The technical problem to be solved in the present invention provide a kind of with the titanium white production waste residue be the iron black purity height of raw material, product, particle diameter is thin and evenly, tinting strength is high, has the production method of the iron oxide black of blue phase characteristics.
The technical scheme that addresses the above problem is:
1, the waste particle that contains ferrous sulfate that titanium white production is discharged drops into fully dissolving of heating in the water, and impurity titanyl sulfate wherein is hydrolyzed into the metatitanic acid precipitation, after settlement separate, get its clear liquor and makes perferrite solution;
2, make neutralizing agent and perferrite solution reaction generation ferrous hydroxide with caustic soda;
3, make oxygenant with oxygen-containing gas, generate iron black with above-mentioned hydroxide iron oxidation reaction;
4, sieve in the iron oxide black that will generate, press filtration, rinsing, oven dry, pulverizing promptly get blue phase oxidation iron oxide black pigment product.
Described perferrite solution can be that the ferrous waste residue of sulfur acid that Producing Titanium Dioxide is discharged is made ferrous sulfate aqueous solution through refining and edulcoration;
Described perferrite solution concentration is advisable with 5-50%, and preferred version is that ferrous salt content is 40-50%;
Described neutralizing agent caustic soda comprises liquid base, solid caustic soda, sheet alkali etc., and the gel pH value after the neutralization is 7.5-9;
Described oxygen-containing gas can be air or other oxygen-containing gas.
To be temperature carry out oxidizing reaction to described the 3rd oxidation reaction condition under 90-102 ℃, the condition of pH value at 7.5-9.
The inventive method is a raw material with the titanium white production waste residue, reduced environmental pollution, iron oxide black purity height, the crystal grain produced are thin, the pigment particle size of making is thin and even, and has a blue phase character of the black light black of saturated orchid, very stable to light and atmospheric action, strong coloring force, strong covering power can be used for fine chemical products such as printing ink, carbon dust.
Embodiment
Embodiment 1
The method that this example is produced blue phase oxidation iron oxide black pigment is:
1, the waste residue that contains ferrous sulfate of discharging in the titanium white production is put into dissolving tank, use steam heating, after abundant dissolving, standing sedimentation is got the clear liquor on its top, makes concentration and be 45% ferrous sulfate aqueous solution 2000Kg, puts into reaction vessel;
2, will generate ferrous hydroxide in the about 865Kg adding of the liquid caustic soda of neutralizing agent 30% ferrous sulfate aqueous solution while stirring, the system pH value is 8.5;
3, the ferrous hydroxide that makes is gone into the retort of 5000L with pump delivery, at 95 ℃, pH value is about 8.5 with the steam controlled temperature, and feeding flow while stirring is 0.3m
3The air of/min carries out oxidizing reaction and generates iron black;
The reaction formula in above-mentioned 2,3 steps is:
FeSO
4+2NaOH→Fe(OH)
2+Na
2SO
4
Fe(OH)
2+1/2O
2+H
2O→2Fe(OH)
3
Fe(OH)
2+2Fe(OH)
3→Fe(OH)
2·2Fe(OH)
3→Fe
3O
4+4H
2O
4, wet feed sieves: with the screening of sieving of 3 step gained slurries, sieve number is 320 orders;
5, filter-press water-washing: outsifting is put into water washing tank clean after-filtration;
6,5 gained filtrate are dried;
7, will dry thing and pulverize, make blue phase oxidation iron oxide black pigment.
This routine product contains Fe after testing
3O
496.5%; Specify the standard specimen ratio with industry, tinting strength is 160%.
Be the main technical data of embodiment 2-4 production method below:
| Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| In perferrite solution (concentration) neutralizing agent and back pH value oxidizing reaction temperature oxidizing reaction pH value | 30% solid caustic soda 7.5 90 7.5 | 40% 42% liquid caustic soda 8 95 8 | 50% 30% liquid caustic soda 9 100 9 |
The product that embodiment 2-4 produces all can be obtained effect substantially the same manner as Example 1.
Claims (2)
1, a kind of production method of iron oxide black is characterized in that, comprises following content:
(1), the waste particle that contains ferrous sulfate that titanium white production is discharged drops into fully dissolving of heating in the water, impurity titanyl sulfate wherein is hydrolyzed into the metatitanic acid precipitation, after settlement separate, get its clear liquor and makes perferrite solution;
(2), do the reaction of neutralizing agent and perferrite solution with caustic soda and generate ferrous hydroxide, ferrous hydroxide gel pH value is 7.5-9;
(3), make oxygenant, generate iron blackly with above-mentioned hydroxide iron oxidation reaction, to be temperature carry out oxidizing reaction to oxidation reaction condition under 90-102 ℃, the condition of pH value at 7.5-9 with oxygen-containing gas;
(4), sieve in the iron oxide black that will generate, press filtration, rinsing, oven dry, pulverizing promptly get blue phase oxidation iron oxide black pigment product.
2, the production method of iron oxide black according to claim 1 is characterized in that: described perferrite solution concentration is 40-50%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100751124A CN100352866C (en) | 2005-06-08 | 2005-06-08 | Method for producing iron oxide black |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100751124A CN100352866C (en) | 2005-06-08 | 2005-06-08 | Method for producing iron oxide black |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1709985A CN1709985A (en) | 2005-12-21 |
| CN100352866C true CN100352866C (en) | 2007-12-05 |
Family
ID=35706279
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100751124A Active CN100352866C (en) | 2005-06-08 | 2005-06-08 | Method for producing iron oxide black |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100352866C (en) |
Families Citing this family (12)
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| CN107200359B (en) * | 2016-03-17 | 2019-08-13 | 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 |
Citations (3)
| 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 |
| CN1546385A (en) * | 2003-12-03 | 2004-11-17 | 南京工业大学 | Ferric oxide with high magnetic-hysteresis heat generation ability for the use of tumour thermomagnetic therapy and method for preparing the same |
| CN1590304A (en) * | 2003-09-05 | 2005-03-09 | 李景钞 | Comprehensive utilization method of ferrous sulfate waste water and waste iron scraps |
-
2005
- 2005-06-08 CN CNB2005100751124A patent/CN100352866C/en active Active
Patent Citations (3)
| 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 |
| CN1546385A (en) * | 2003-12-03 | 2004-11-17 | 南京工业大学 | Ferric oxide with high magnetic-hysteresis heat generation ability for the use of tumour thermomagnetic therapy and method for preparing the same |
Non-Patent Citations (2)
| Title |
|---|
| 钛白副产硫酸亚铁制取氧化铁颜料工艺的研究 周宏明.湘潭大学硕士论文 2001 * |
| 钛白副产硫酸亚铁制取氧化铁颜料的工艺研究 熊国宣.华东地质学院学报，第20卷第2期 1997 * |
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| Publication number | Publication date |
|---|---|
| CN1709985A (en) | 2005-12-21 |
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Assignee: Hubei Wan run industry and Trade Development Co., Ltd. Assignor: Liu Shiqi Contract fulfillment period: 2009.2.23 to 2025.6.8 Contract record no.: 2009990000197 Denomination of invention: Method for producing iron oxide black Granted publication date: 20071205 License type: Exclusive license Record date: 20090318 |
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Effective date of registration: 20120131 Address after: 442003 Shiyan City, Hubei province Zhangwan District Huaguo Road No. 111 Patentee after: Hubei Wanrun New Energy Technology Development Co.,Ltd. Address before: 518048 B-607, Futian District International Chamber of Commerce, Shenzhen, Guangdong Patentee before: Liu Shiqi |
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Address after: 442003 Shiyan City, Hubei province Zhangwan District Huaguo Road No. 111 Patentee after: Hubei Wanrun New Energy Technology Co., Ltd Address before: 442003 Shiyan City, Hubei province Zhangwan District Huaguo Road No. 111 Patentee before: HUBEI WANRUN NEW ENERGY TECHNOLOGY DEVELOPMENT Co.,Ltd. |
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