CN1709984A - Method for producing iron oxide black - Google Patents
Method for producing iron oxide black Download PDFInfo
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- CN1709984A CN1709984A CN 200510075111 CN200510075111A CN1709984A CN 1709984 A CN1709984 A CN 1709984A CN 200510075111 CN200510075111 CN 200510075111 CN 200510075111 A CN200510075111 A CN 200510075111A CN 1709984 A CN1709984 A CN 1709984A
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- CN
- China
- Prior art keywords
- iron oxide
- producing
- black
- oxide black
- ferrous
- 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 40
- 238000004519 manufacturing process Methods 0.000 title claims description 31
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 9
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 6
- 239000002699 waste material Substances 0.000 claims abstract description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000012452 mother liquor Substances 0.000 claims abstract description 4
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 17
- 238000007254 oxidation reaction Methods 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 7
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 6
- 239000011790 ferrous sulphate Substances 0.000 claims description 6
- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 claims description 6
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 6
- 239000004408 titanium dioxide Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 claims description 4
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 3
- 239000002893 slag Substances 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 229960002089 ferrous chloride Drugs 0.000 claims description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims 1
- 238000004062 sedimentation Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 2
- 108010010803 Gelatin Proteins 0.000 abstract 3
- 229920000159 gelatin Polymers 0.000 abstract 3
- 239000008273 gelatin Substances 0.000 abstract 3
- 235000019322 gelatine Nutrition 0.000 abstract 3
- 235000011852 gelatine desserts Nutrition 0.000 abstract 3
- 230000019612 pigmentation Effects 0.000 abstract 2
- 239000010866 blackwater Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 5
- 239000000049 pigment Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- -1 iron ion Chemical class 0.000 description 3
- 235000021190 leftovers Nutrition 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 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
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 1
Landscapes
- Compounds Of Iron (AREA)
Abstract
The invention relates to the producing method of a kind of oxidized iron black. It includes following steps: add ferrite watery solution into neutralization action pot, add ammonia and mix round watery solution to neutralize it to prepare hydroxidized ferrous gelatin, transmit the produced gelatin into oxidizing reaction pot; send oxygenous gas and meanwhile heat gelatin to make it oxidated, after reaction we can get oxidized iron oxide black pulp; separate iron oxide black and mother liquor in pulp; make the separated iron oxide black water washed, sieved, dried and comminuted orderly to get finished products. This method adopts liquid phase method to make its reaction rate greatly improved, the particle granularity of oxidized iron oxide black finished products even; it has higher pigmentation strength, and the obtained product contains 96.5% Fe3O4. Compared with the industry appointed standard sample, its pigmentation strength is 200% - 250%; ulteriorly make offal in producing titanium oxide powder as material of this method, which is beneficial to circulation usage of industry waste material and environmental protection, and can greatly reduce producing cost.
Description
Technical Field
The invention relates to a production method of a pigment, in particular to a production method of an iron oxide black pigment with high tinting strength.
Background
Iron oxide black pigment, commonly called iron black, contains ferroferric oxide as main component and Fe as molecular formula3O4Or Fe2O3FeO. The existing production method of iron oxide black pigment generally adopts a direct addition method, the process uses leftovers for producing iron oxide red or iron oxide yellow as raw materials, ferrous sulfate and caustic soda are added, and iron oxide black is generated by addition and dehydration under the conditions that the pH value is 7-8 and the temperature is 90-100 ℃. In addition, in the existing titanium dioxide production, one ton of titanium dioxide is producedTitanium dioxide can produce 3-4 tons of waste residue containing ferrous sulfate, which causes serious environmental pollution.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art and provide a method for producing iron oxide black, wherein the obtained iron oxide black finished product has uniform particle size and higher tinting strength.
The technical scheme adopted by the invention is as follows:
a method for producing black iron oxide, comprising the steps of:
(a) adding a ferrous salt aqueous solution into a neutralization reaction tank, adding ammonia, stirring the aqueous solution to neutralize the aqueous solution to generate ferrous hydroxide gel, and conveying the generated gel to an oxidation reaction tank;
(b) introducing oxygen-containing gas into the oxidation reaction tank, heating the gel to oxidize the oxygen-containing gas and obtaining iron oxide black slurry after reaction;
(c) separating iron oxide black and mother liquor in the slurry;
(d) and washing, screening, drying and crushing the separated iron oxide black sequentially to obtain a finished product.
Further, the ferrous salt in the step (a) in the production method is preferably a clear solution obtained by dissolving leftovers from the production of titanium dioxide in water.
Compared with the prior art, the production method of the iron oxide black has the following positive effects: the reaction rate is greatly improved by adopting a liquid phase method, the particle diameter of the obtained iron oxide black finished product is uniform, the tinting strength is higher, and the product obtained by the production method related by the invention contains Fe through detection3O496.5 percent, compared with the standard sample specified by the industry, the tinting strength is 200-250 percent; furthermore, the leftovers from the production of titanium dioxide are used as the raw materials of the production method, which is beneficial to the recycling of industrial waste and environmental protection; greatly reducing the production cost.
Detailed Description
The invention is further illustrated by the following examples.
The production method of the iron oxide black comprises four steps of neutralization, oxidation, separation and post-treatment. Wherein the neutralization reaction is that aqueous solution of ferrous salt is added into a neutralization reaction tank, then ammonia is added and the aqueous solution is stirred to generate neutralization reaction to generate ferrous hydroxide gel, the generated gel is conveyed to an oxidation reaction tank by a pump, and the reaction formula of the step is that (ii) a The oxidation reaction is to introduce oxygen-containing gas into the oxidation reaction tank and heat the gel to oxidize the oxygen-containing gas and obtain iron oxide black slurry after the reaction is finished, and the reaction formula of the step is ， (ii) a Then separating iron oxide black and mother liquor in the slurry; and washing, sieving, filtering, drying and crushing the separated iron oxide black in sequence to obtain a finished product. The finished iron black obtained by the method has blue-phase hue and higher tinting strength and grain diameter uniformity than the iron black produced by a direct addition method.
Further, in the method for producing iron oxide black of the present invention, the ferrous salt in the step (a) includes ferrous sulfate, ferrous nitrate, ferrous chloride; the ammonia in the step (a) comprises liquid ammonia, gaseous ammonia and ammonia water; the preferable preparation method of the ferrous salt in the step (a) 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, the impurity titanyl sulfate is hydrolyzed into metatitanic acid precipitate, and after settling separation, clear liquid is taken as ferrous salt aqueous solution for producing iron oxide black, so that certain industrial production waste materials can be recycled, and the environment is protected.
Further, in the production method of the iron oxide black, the iron ion concentration of the ferrite solution in the step (a) is 10-150 g/L; controlling the pH value of the ammonia added in the step (a) to be 7-10; the heating temperature in the step (b) is 80-100 ℃, and direct steam heating is adopted; the bottom of the oxidation reaction tank used in the step (b) is provided with a gas distributor, namely, steam is directly introduced into the oxidation reaction tank to heat the gel, oxygen-containing gas enters through the gas distributor at the bottom of the reaction tank, and the oxygen-containing gas moves upwards in the tank and is stirred, so that the oxidation reaction is enhanced.
The product obtained by the production method related by the invention contains Fe through detection3O496.5 percent; compared with the standard sample specified in the industry, the tinting strength is 200-250%, and the production cost is greatly reduced.
Examples
Adding ferrous solution with iron ion concentration shown in the following table into a 2000L neutralization reaction tank with stirring, adding liquid ammonia under stirring, and controlling the pH value of the gel; conveying the prepared ferrous hydroxide gel into a 3000L oxidation reaction tank, heating with steam, controlling the heating temperature, and introducing 0.6m3And air of/min, separating iron black from the slurry after the reaction is finished, and obtaining the iron black finished product through water washing, sieving, filtering, drying and crushing.
TABLE 1
| Examples 1 | Examples 2 | Examples 3 | Examples 4 | Examples 5 | Examples 6 | |
| Ferrous salt iron ion concentration (g/L) | 50 | 100 | 150 | 10 | 50 | 100 |
| pH value of neutralization reaction | 10 | 9 | 7 | 9.5 | 7.5 | 8.5 |
| Temperature (. degree.C.) of the oxidation reaction | 80 | 90 | 100 | 85 | 95 | 90 |
Claims (8)
1. A method for producing black iron oxide, comprising the steps of:
(a) adding a ferrous salt aqueous solution into a neutralization reaction tank, adding ammonia, stirring the aqueous solution to neutralize the aqueous solution to generate ferrous hydroxide gel, and conveying the generated gel to an oxidation reaction tank;
(b) introducing oxygen-containing gas into the oxidation reaction tank, heating the gel to oxidize the oxygen-containing gas and obtaining iron oxide black slurry after reaction;
(c) separating iron oxide black and mother liquor in the slurry;
(d) and washing, screening, drying and crushing the separated iron oxide black sequentially to obtain a finished product.
2. The method for producing iron oxide black according to claim 1, wherein the ferrous salt in the step (a) comprises ferrous sulfate, ferrous nitrate, ferrous chloride.
3. The method for producing black iron oxide according to claim 2, wherein the ammonia in the step (a) comprises liquid ammonia, gaseous ammonia, aqueous ammonia.
4. The method for producing black iron oxide according to claim 3, wherein the method for producing the aqueous solution of ferrous salt in the step (a) comprises: waste slag particles containing ferrous sulfate discharged from titanium dioxide production are put into water to be heated and fully dissolved, and after sedimentation separation, clear liquid of the waste slag particles is taken as ferrous salt water solution for producing iron oxide black.
5. The method for producing iron oxide black according to any one of claims 1 to 4, wherein the concentration of the ferrous salt solution in the step (a) is 10 to 150 g/L.
6. The method for producing black iron oxide according to claim 5, wherein the pH value after the addition of ammonia in the step (a) is controlled to 7 to 10.
7. The method for producing iron oxide black according to any one of claims 1 to 4, wherein the heating temperature in the step (b) is 80 to 100 ℃ and direct steam heating is employed.
8. The method for producing black iron oxide according to claim 7, wherein the oxygen-containing gas used in the step (b) is air, oxygen or other oxygen-containing gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510075111XA CN1322067C (en) | 2005-06-08 | 2005-06-08 | Method for producing iron oxide black |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510075111XA CN1322067C (en) | 2005-06-08 | 2005-06-08 | Method for producing iron oxide black |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1709984A true CN1709984A (en) | 2005-12-21 |
| CN1322067C CN1322067C (en) | 2007-06-20 |
Family
ID=35706278
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200510075111XA Active CN1322067C (en) | 2005-06-08 | 2005-06-08 | Method for producing iron oxide black |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1322067C (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101746836B (en) * | 2009-12-25 | 2012-05-23 | 浙江工业大学 | Method for preparing iron oxide black pigment by carrying out resourceful treatment on pyrite wastewater |
| 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 |
| CN102633308A (en) * | 2012-05-19 | 2012-08-15 | 河南佰利联化学股份有限公司 | Method for producing iron oxide black by ferrous sulfate mother liquor |
| CN104828876A (en) * | 2015-05-25 | 2015-08-12 | 北京矿冶研究总院 | Method for producing ferroferric oxide by using iron scale |
| 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 |
| CN105271432A (en) * | 2015-10-19 | 2016-01-27 | 天津大学 | Method for preparing nano ferroferric oxide particle with steel picking waste liquid |
| CN106629862A (en) * | 2016-12-22 | 2017-05-10 | 广州市群笑化工颜料有限公司 | Method for producing black iron oxide by adopting fluorine titanium mother solution |
| CN112551593A (en) * | 2020-12-07 | 2021-03-26 | 太原理工大学 | Preparation method of magnetite micro-nano material |
| 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 (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1013102B (en) * | 1987-09-14 | 1991-07-10 | 包头钢铁公司环境保护研究所 | Method for producing iron oxide red from iron borne soot of steel smelting |
| CN1040565A (en) * | 1988-08-17 | 1990-03-21 | 李剑池 | The combine production method of polyiron sulfate and iron oxide black |
| CN1226354C (en) * | 2001-12-28 | 2005-11-09 | 中山大学 | Composite gaolinite/rare-earth/iron oxide-base nano pigment and its microwave process for synthesizing it |
| CN1536031A (en) * | 2003-04-11 | 2004-10-13 | 陈书怡 | Polycrystalline state composite and its preparation method |
| 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 CNB200510075111XA patent/CN1322067C/en active Active
Cited By (11)
| 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 |
| CN101746836B (en) * | 2009-12-25 | 2012-05-23 | 浙江工业大学 | Method for preparing iron oxide black pigment by carrying out resourceful treatment on pyrite wastewater |
| CN102633308A (en) * | 2012-05-19 | 2012-08-15 | 河南佰利联化学股份有限公司 | Method for producing iron oxide black by ferrous sulfate mother liquor |
| 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 |
| CN104828876A (en) * | 2015-05-25 | 2015-08-12 | 北京矿冶研究总院 | Method for producing ferroferric oxide by using iron scale |
| 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 |
| CN105271432A (en) * | 2015-10-19 | 2016-01-27 | 天津大学 | Method for preparing nano ferroferric oxide particle with steel picking waste liquid |
| CN106629862A (en) * | 2016-12-22 | 2017-05-10 | 广州市群笑化工颜料有限公司 | Method for producing black iron oxide by adopting fluorine titanium mother solution |
| CN106629862B (en) * | 2016-12-22 | 2019-03-19 | 广州市群笑化工颜料有限公司 | With the method for fluorine titanium mother liquor production iron oxide black |
| CN112551593A (en) * | 2020-12-07 | 2021-03-26 | 太原理工大学 | Preparation method of magnetite micro-nano material |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1322067C (en) | 2007-06-20 |
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