CN1322067C - Method for producing iron oxide black - Google Patents
Method for producing iron oxide black Download PDFInfo
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- CN1322067C CN1322067C CNB200510075111XA CN200510075111A CN1322067C CN 1322067 C CN1322067 C CN 1322067C CN B200510075111X A CNB200510075111X A CN B200510075111XA CN 200510075111 A CN200510075111 A CN 200510075111A CN 1322067 C CN1322067 C CN 1322067C
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- CN
- China
- Prior art keywords
- iron oxide
- oxide black
- production method
- ammonia
- oxygen
- 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 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 30
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 15
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims abstract description 9
- 239000001301 oxygen Substances 0.000 claims abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 9
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 6
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 claims abstract description 5
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 7
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 6
- 239000011790 ferrous sulphate Substances 0.000 claims description 6
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 235000010215 titanium dioxide Nutrition 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000012452 mother liquor Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000002699 waste material Substances 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 2
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 abstract description 4
- 239000002440 industrial waste Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000007791 liquid phase Substances 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
- 238000004040 coloring Methods 0.000 abstract 2
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 235000021190 leftovers Nutrition 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 15
- 239000001034 iron oxide pigment Substances 0.000 description 9
- 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 description 9
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000000049 pigment Substances 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 1
Abstract
The present invention relates to a method for producing iron oxide black, which comprises the following steps: ferrous salt water solution is added to a neutralization reaction tank, ammonia is added, and the water solution is stirred so that ferrous hydroxide gelatin is generated by neutralization; the generated gelatin is conveyed to an oxidation reaction tank; oxygen-containing gas is led in the oxidation reaction tank, and the gelatin is simultaneously heated to be oxidized; iron oxide black slurry is obtained after the reaction; iron oxide black and mother liquid in the slurry are separated; the separated iron oxide black is orderly washed by water, sieved, dried and pulverized to obtain a finished product. The method for producing iron oxide black of the present invention is characterized in that a liquid phase method is used to greatly enhance a reaction rate, and the particles of the obtained iron oxide black finished product has the advantages of even particle diameter and high coloring power. The obtained product contains 96.5 % of Fe3O4. Compared with a designated standard sample in industry, the coloring power is from 200 to 250%. In addition, leftovers for producing titanium dioxide are used as the raw material of the producing method of the present invention, which is favorable for cyclic utilization and environmental protection for industrial waste, and production costs are greatly reduced.
Description
Technical field
The present invention relates to a kind of production method of pigment, particularly a kind of production method of high-strength black iron oxide pigment.
Background technology
Black iron oxide pigment is commonly called as the iron oxide black, and main component is a Z 250, and molecular formula is Fe
3O
4, or Fe
2O
3.FeO.The production method of existing black iron oxide pigment generally adopts the direct addition method, this technology is to be raw material with the tankage of producing iron oxide red or iron oxide yellow, add ferrous sulfate and caustic soda, in the pH value is 7～8, temperature is that addition under 90～100 ℃ the situation, dehydration generate the iron oxide black, and the shortcoming of this technology is that the simple particle shape of the iron black product of gained is inconsistent, and particle diameter is big and distribute very inhomogeneous, red partially phase of form and aspect or yellow phase during as 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 is intended to overcome the deficiency of above-mentioned prior art, and a kind of production method of black iron oxide pigment is provided, and the particle diameter of the iron oxide black finished product that it obtains is even, and tinting strength is higher.
The technical solution used in the present invention is:
The production method of iron oxide black, this method may further comprise the steps:
(a) in the neutralization reaction jar, add perferrite solution, add ammonia and stir the aqueous solution and make its neutralization generate the ferrous hydroxide gel, and the pH value that control adds behind the ammonia is 7～10, the gel of generation is delivered to the oxidizing reaction jar;
(b) in the oxidizing reaction jar, feed oxygen-containing gas and adopt the scope of open steam heating method heating gel to 85 ℃～100 ℃ to make the gel oxidation simultaneously, obtain the iron oxide black slurry after the reaction;
(c) iron oxide black in the separating slurry and mother liquor;
(d) iron oxide black after will separating successively through washing, sieve, drying and pulverizing obtain finished product.
Further, preferably in this production method the ferrous salt described in the step (a) be the clear liquor that obtains after water-soluble by the tankage of producing titanium dioxide.
Compared with the prior art the production method of black iron oxide pigment of the present invention has following positively effect: adopt its reactivity of liquid phase method to improve greatly, the particle diameter of the iron oxide black finished product that obtains is even, tinting strength is higher, and the product that obtains through production method involved in the present invention contains Fe after testing
3O
496.5%, specify the standard specimen ratio with industry, tinting strength is 200～250%; Further, produce the raw material of the tankage of titanium dioxide, be beneficial to the recycle and the environment protection of industrial waste as production method involved in the present invention; Greatly reduce production cost.
Embodiment
Further specify the present invention below by embodiment.
The production method of the black iron oxide pigment that the present invention relates to comprises neutralization, oxidation, separation and four steps of aftertreatment.Wherein, neutralization reaction is the aqueous solution that adds ferrous salt in the neutralization reaction jar, add ammonia afterwards and stir the aqueous solution to make it that neutralization reaction take place to generate the ferrous hydroxide gel, with the gel that generates with pump delivery to the oxidizing reaction jar, the reaction formula in this step is Fe
2++ 2NH
3+ 2H
2O==Fe (OH)
2↓+2NH
4 +Oxidizing reaction makes its oxidation for feeding oxygen-containing gas and heat gel simultaneously in the oxidizing reaction jar, obtains the iron oxide black slurry after reaction is finished, and the reaction formula of this step is 2Fe (OH)
2+ 1/2O
2+ H
2O==2Fe (OH)
3, 2Fe (OH)
3+ Fe (OH)
2==2Fe (OH)
3Fe (OH)
2==Fe
3O
4+ 4H
2O; Iron oxide black in the separating slurry and mother liquor afterwards; With the iron oxide black after separating successively through washing, sieve, filter, drying and pulverizing obtain finished product.The finished iron black that aforesaid method obtains shows blue phase mutually, and tinting strength and uniform particle diameter degree all are higher than the iron oxide black that the direct addition method is produced.
Further, in the production method of black iron oxide pigment of the present invention, the ferrous salt described in the step (a) comprises ferrous sulfate, Iron nitrate, iron protochloride; Ammonia described in the step (a) comprises liquid ammonia, gaseous ammonia, ammoniacal liquor; The preferred making method of ferrous salt described in the step (a) is: 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 as the perferrite solution of producing iron oxide black; this makes some industrial waste material to be recycled, and has also protected environment simultaneously.
Further, in the production method of black iron oxide pigment of the present invention, the iron concentration of the ferrous salt solution described in the step (a) is 10～150g/L; PH value in the step (a) behind the control adding ammonia is 7～10; Heating temperature described in the step (b) is 80～100 ℃, adopts the open steam heating; The pot bottom of the oxidizing reaction jar that adopts in the step (b) is a gas distributor, soon steam directly feeds in the oxidizing reaction jar and heats gel, oxygen-containing gas enters by the gas distributor of retort bottom, and oxygen-containing gas upwards moves in jar and through stirring, these can strengthen oxidizing reaction.
The product that obtains through production method involved in the present invention contains Fe after testing
3O
496.5%; Specify the standard specimen ratio with industry, tinting strength is 200～250%, and its production cost reduces greatly.
Embodiment
In the neutralization reaction jar that the 2000L band stirs, adding iron concentration is ferrous iron solution as shown in the table, adds liquefied ammonia under condition of stirring, control pH of latex gel value; The ferrous hydroxide gel that makes is conveyed in the 3000L oxidizing reaction jar, with steam heating and control Heating temperature, feeds 0.6m
3The air of/min is separated the iron oxide black after reaction finishes from slurry, through wash, sieve, filter, dry, pulverizing obtains iron black finished product.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | |
| Ferrous salt iron concentration (g/L) | 50 | 100 | 150 | 10 | 50 | 100 |
| The pH value of neutralization reaction | 10 | 9 | 7 | 9.5 | 7.5 | 8.5 |
| The temperature of oxidizing reaction (℃) | 80 | 90 | 100 | 85 | 95 | 90 |
Claims (6)
1, the production method of iron oxide black, this method may further comprise the steps:
(a) in the neutralization reaction jar, add perferrite solution, add ammonia and stir the aqueous solution and make its neutralization generate the ferrous hydroxide gel, and the pH value that control adds behind the ammonia is 7～10, the gel of generation is delivered to the oxidizing reaction jar;
(b) in the oxidizing reaction jar, feed oxygen-containing gas and adopt the scope of open steam heating method heating gel to 85 ℃～100 ℃ to make the gel oxidation simultaneously, obtain the iron oxide black slurry after the reaction;
(c) iron oxide black in the separating slurry and mother liquor;
(d) iron oxide black after will separating successively through washing, sieve, drying and pulverizing obtain finished product.
2, the production method of iron oxide black according to claim 1 is characterized in that the ferrous salt described in the step (a) comprises ferrous sulfate, Iron nitrate, iron protochloride.
3, the production method of iron oxide black according to claim 2 is characterized in that the ammonia described in the step (a) comprises liquid ammonia, gaseous ammonia, ammoniacal liquor.
4, the production method of iron oxide black according to claim 3, the making method that it is characterized in that perferrite solution described in the step (a) is: the waste particle that contains ferrous sulfate that titanium white production is discharged drops into fully dissolving of heating in the water, after settlement separate, get its clear liquor as the perferrite solution of producing iron oxide black.
5, according to the production method of the described iron oxide black of the arbitrary claim of claim 1-4, the concentration that it is characterized in that the ferrous salt solution described in the step (a) is 10～150g/L.
6, the production method of iron oxide black according to claim 5 is characterized in that the oxygen-containing gas that adopts in the step (b) is air, oxygen or other oxygen-containing gass.
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 CN1709984A (en) | 2005-12-21 |
| CN1322067C true 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) |
Families Citing this family (9)
| 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 |
| CN104828876B (en) * | 2015-05-25 | 2016-08-17 | 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 |
| CN105271432B (en) * | 2015-10-19 | 2017-03-22 | 天津大学 | Method for preparing nano ferroferric oxide particle with steel picking waste liquid |
| 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 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1031985A (en) * | 1987-09-14 | 1989-03-29 | 包头钢铁公司环境保护研究所 | Method with 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 |
| CN1359987A (en) * | 2001-12-28 | 2002-07-24 | 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
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1031985A (en) * | 1987-09-14 | 1989-03-29 | 包头钢铁公司环境保护研究所 | Method with 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 |
| CN1359987A (en) * | 2001-12-28 | 2002-07-24 | 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 |
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| Publication number | Publication date |
|---|---|
| CN1709984A (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.: 2009990000196 Denomination of invention: Method for producing iron oxide black Granted publication date: 20070620 License type: Exclusive license Record date: 20090318 |
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