CN105439211A - Energy-saving environmental-protection production method for iron oxide black pigment - Google Patents
Energy-saving environmental-protection production method for iron oxide black pigment Download PDFInfo
- Publication number
- CN105439211A CN105439211A CN201510948055.XA CN201510948055A CN105439211A CN 105439211 A CN105439211 A CN 105439211A CN 201510948055 A CN201510948055 A CN 201510948055A CN 105439211 A CN105439211 A CN 105439211A
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- China
- Prior art keywords
- iron oxide
- energy
- production method
- oxide pigment
- conserving
- 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 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 239000000049 pigment Substances 0.000 title abstract 5
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 29
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 17
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 17
- 239000012452 mother liquor Substances 0.000 claims abstract description 13
- 238000005273 aeration Methods 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 239000006227 byproduct Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 36
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 32
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 239000001034 iron oxide pigment Substances 0.000 claims description 24
- 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 24
- 230000001590 oxidative effect Effects 0.000 claims description 19
- 235000017550 sodium carbonate Nutrition 0.000 claims description 16
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 16
- 229910052742 iron Inorganic materials 0.000 claims description 13
- 238000010792 warming Methods 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000005189 flocculation Methods 0.000 claims description 8
- 230000016615 flocculation Effects 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 235000010215 titanium dioxide Nutrition 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000002699 waste material Substances 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 abstract 1
- 238000004040 coloring Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241001062009 Indigofera Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses an energy-saving environmental-protection production method for an iron oxide black pigment, wherein the method includes the following steps: (1) removal of impurities of ferrous sulfate; (2) aeration treatment of iron oxide yellow mother liquor; (3) oxidation reaction; (4) iron oxide black pigment obtaining. According to the energy-saving environmental-protection production method for the iron oxide black pigment, with the waste by-product as the raw material, and through reasonable design of oxidation conditions, the excellent-performance iron oxide black pigment is produced, and new industrial three wastes are no longer produced. The conventional waste is turned into treasure, the utilization rate of resources is increased, and the method has the advantages of energy saving and environmental protection and is conducive to social sustainable development.
Description
Technical field
The present invention relates to chemical color field, particularly relate to a kind of energy-conserving and environment-protective production method of black iron oxide pigment.
Background technology
Iron oxide black is called for short iron black, and molecular formula is Fe
3o
4or Fe
2o
3feO, chemical name Z 250, has saturated indigo plant ink light black.Iron oxide black is because of opacifying power, strong coloring force, and light fastness is good and be applied to coating industry, due to alkaline-resisting and be widely used in building trade Cement Colouring.In addition, be also employed in ink, printing, coloring plastic, polishing and metal defect detection etc.
The production of current iron oxide yellow because of the requirement of processing condition, FeSO in its mother liquor
47H
2o content is 60 ~ 70g/t, if be not used, not only increase enterprise's cost of sewage disposal, also result in the serious waste of iron resources.Conventional oxidation iron oxide black produces based on ferrous hydroxide oxidation style, require higher to material quality, require the background of increasingly stringent at resources and environment under, the need of production of existing iron oxide black is produced from resource-hungry and is turned to resource reclaim recycling type to produce, to improve the utilization ratio of resource, realize the production requirement of energy-conserving and environment-protective.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of energy-conserving and environment-protective production method of black iron oxide pigment, iron oxide yellow mother liquor effectively can be utilized to produce high quality iron oxide black, improve resource utilization, reduce environmental pollution.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: the energy-conserving and environment-protective production method providing a kind of black iron oxide pigment, comprises the steps:
(1) ferrous sulfate removal of impurities: by-product ferrous sulfate during production of titanium white powder is dissolved in clear water with the ratio of mass ratio 1:10, add scrap iron powder and flocculation agent again, then after intensification stirring reaction certain hour, staticly settle, solids removed by filtration, the copperas solution after being purified;
(2) iron oxide yellow mother liquor Air Exposure: add in aeration tank by the iron oxide yellow mother liquor of certain proportioning and soda ash solution, after intensification, is uniformly mixed while pass into air to carry out Air Exposure, filters after process terminates, and removes filtrate, obtains iron mud;
(3) oxidizing reaction: add in oxidizing reaction pond obtain in a certain amount of step (1) copperas solution, iron mud in step (2) after Air Exposure, with the soda ash solution of same concentrations in step (2) and appropriate amount of deionized water, be warming up to 80 ~ 90 DEG C, adjust ph, passes into oxygen while stirring and carries out oxidizing reaction under constant temperature;
(4) black iron oxide pigment is obtained: by the mixture after oxidizing reaction in step (3) through press filtration, washing, drying, pulverizing, obtain described black iron oxide pigment.
In a preferred embodiment of the present invention, in described step (1), the mol ratio of described scrap iron powder and described ferrous sulfate is 1:2; The add-on of described flocculation agent is 0.1 ~ 0.3 times of described ferrous sulfate quality.
In a preferred embodiment of the present invention, in described step (1), the temperature of described reaction is 30 ~ 50 DEG C, and the reaction times is 0.5 ~ 2h.
In a preferred embodiment of the present invention, in described step (2), the concentration of described soda ash solution is 30 ~ 40%, and the volume ratio of described iron oxide yellow mother liquor and soda ash solution is 1:3 ~ 5.
In a preferred embodiment of the present invention, in described step (2), described warming temperature is 30 ~ 50 DEG C, and described air flow is 3 ~ 5m
3/ h, aeration time is 1 ~ 2h.
In a preferred embodiment of the present invention, in described step (3), the mol ratio of described copperas solution, iron mud and soda ash solution is 1:1.5 ~ 2:1 ~ 1.2.
In a preferred embodiment of the present invention, in described step (3), described pH value is 6.5 ~ 7.5, and thermostat temperature is 90 ~ 100 DEG C, and oxygen intake is 5 ~ 9m
3/ h, the reaction times is 1 ~ 3h.
The invention has the beneficial effects as follows: the energy-conserving and environment-protective production method of a kind of black iron oxide pigment of the present invention, with useless by product for raw material, designed by rational oxidizing condition, produce the black iron oxide pigment of excellent performance, and no longer produce new three industrial wastes.Existing waste is turned waste into wealth by the present invention, improves the utilization ratio of resource, energy-conserving and environment-protective, is conducive to the Sustainable development of society.
Embodiment
Below preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
The embodiment of the present invention comprises:
Embodiment 1
An energy-conserving and environment-protective production method for black iron oxide pigment, comprises the steps:
(1) ferrous sulfate removal of impurities: by-product ferrous sulfate during production of titanium white powder is dissolved in clear water with the ratio of mass ratio 1:10, add scrap iron powder and flocculation agent again, the mol ratio of scrap iron powder and described ferrous sulfate is made to be 1:2, the add-on of flocculation agent is 0.1 times of ferrous sulfate quality, then be warming up to 30 ~ 50 DEG C, the speed stirring reaction 2h of 50r/min, staticly settles, solids removed by filtration impurity, the copperas solution after being purified;
(2) iron oxide yellow mother liquor Air Exposure: to be the iron oxide yellow mother liquor of 1:3 and mass concentration by volume ratio be 30% soda ash solution add in aeration tank, be warming up to 30 DEG C, be uniformly mixed while pass into 3m
3the air of/h carries out Air Exposure 2h, filters, and removes filtrate, obtains iron mud;
(3) oxidizing reaction: add in oxidizing reaction pond obtain in step (1) copperas solution, iron mud in step (2) after Air Exposure, with the soda ash solution of same concentrations in step (2) and appropriate amount of deionized water, the mol ratio of copperas solution in oxidizing reaction pond, iron mud and soda ash solution is made to be 1:1.5:1, then 80 ~ 90 DEG C are warming up to, adjust ph is pass into 5m while stirring under 6.5,90 DEG C of constant temperature
3the oxygen of/h carries out oxidizing reaction 3h;
(4) black iron oxide pigment is obtained: by the mixture after oxidizing reaction in step (3) through press filtration, washing, drying, pulverizing, obtain described black iron oxide pigment.
Embodiment 2
An energy-conserving and environment-protective production method for black iron oxide pigment, comprises the steps:
(1) ferrous sulfate removal of impurities: by-product ferrous sulfate during production of titanium white powder is dissolved in clear water with the ratio of mass ratio 1:10, add scrap iron powder and flocculation agent again, the mol ratio of scrap iron powder and described ferrous sulfate is made to be 1:2, the add-on of flocculation agent is 0.3 times of ferrous sulfate quality, then be warming up to 50 DEG C, the speed stirring reaction 0.5h of 80r/min, staticly settles, solids removed by filtration impurity, the copperas solution after being purified;
(2) iron oxide yellow mother liquor Air Exposure: to be the iron oxide yellow mother liquor of 1:5 and mass concentration by volume ratio be 40% soda ash solution add in aeration tank, be warming up to 50 DEG C, be uniformly mixed while pass into 5m
3the air of/h carries out Air Exposure 1h, filters, and removes filtrate, obtains iron mud;
(3) oxidizing reaction: add in oxidizing reaction pond obtain in a certain amount of step (1) copperas solution, iron mud in step (2) after Air Exposure, with the soda ash solution of same concentrations in step (2) and appropriate amount of deionized water, the mol ratio of copperas solution in oxidizing reaction pond, iron mud and soda ash solution is made to be 1:2:1.2, then 90 DEG C are warming up to, adjust ph is pass into 9m while stirring under 7.5,100 DEG C of constant temperature
3the oxygen of/h carries out oxidizing reaction 1h;
(4) black iron oxide pigment is obtained: by the mixture after oxidizing reaction in step (3) through press filtration, washing, drying, pulverizing, obtain described black iron oxide pigment.
The preparation method of above-mentioned iron oxide black, the transformation efficiency of raw material is 70 ~ 75%, and gained black iron oxide pigment complies with the national standard requirements, and has excellent opacifying power and stability.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (7)
1. an energy-conserving and environment-protective production method for black iron oxide pigment, is characterized in that, comprise the steps:
(1) ferrous sulfate removal of impurities: by-product ferrous sulfate during production of titanium white powder is dissolved in clear water with the ratio of mass ratio 1:10, add scrap iron powder and flocculation agent again, then after intensification stirring reaction certain hour, staticly settle, solids removed by filtration, the copperas solution after being purified;
(2) iron oxide yellow mother liquor Air Exposure: add in aeration tank by the iron oxide yellow mother liquor of certain proportioning and soda ash solution, after intensification, is uniformly mixed while pass into air to carry out Air Exposure, filters after process terminates, and removes filtrate, obtains iron mud;
(3) oxidizing reaction: add in oxidizing reaction pond obtain in a certain amount of step (1) copperas solution, iron mud in step (2) after Air Exposure, with the soda ash solution of same concentrations in step (2) and appropriate amount of deionized water, be warming up to 80 ~ 90 DEG C, adjust ph, passes into oxygen while stirring and carries out oxidizing reaction under constant temperature;
(4) black iron oxide pigment is obtained: by the mixture after oxidizing reaction in step (3) through press filtration, washing, drying, pulverizing, obtain described black iron oxide pigment.
2. the energy-conserving and environment-protective production method of black iron oxide pigment according to claim 1, is characterized in that, in described step (1), the mol ratio of described scrap iron powder and described ferrous sulfate is 1:2; The add-on of described flocculation agent is 0.1 ~ 0.3 times of described ferrous sulfate quality.
3. the energy-conserving and environment-protective production method of black iron oxide pigment according to claim 1, is characterized in that, in described step (1), the temperature of described reaction is 30 ~ 50 DEG C, and the reaction times is 0.5 ~ 2h.
4. the energy-conserving and environment-protective production method of black iron oxide pigment according to claim 1, is characterized in that, in described step (2), the concentration of described soda ash solution is 30 ~ 40%, and the volume ratio of described iron oxide yellow mother liquor and soda ash solution is 1:3 ~ 5.
5. the energy-conserving and environment-protective production method of black iron oxide pigment according to claim 1, is characterized in that, in described step (2), described warming temperature is 30 ~ 50 DEG C, and described air flow is 3 ~ 5m
3/ h, aeration time is 1 ~ 2h.
6. the energy-conserving and environment-protective production method of black iron oxide pigment according to claim 1, is characterized in that, in described step (3), the mol ratio of described copperas solution, iron mud and soda ash solution is 1:1.5 ~ 2:1 ~ 1.2.
7. the energy-conserving and environment-protective production method of black iron oxide pigment according to claim 1, is characterized in that, in described step (3), described pH value is 6.5 ~ 7.5, and thermostat temperature is 90 ~ 100 DEG C, and oxygen intake is 5 ~ 9m
3/ h, the reaction times is 1 ~ 3h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510948055.XA CN105439211A (en) | 2015-12-17 | 2015-12-17 | Energy-saving environmental-protection production method for iron oxide black pigment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510948055.XA CN105439211A (en) | 2015-12-17 | 2015-12-17 | Energy-saving environmental-protection production method for iron oxide black pigment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105439211A true CN105439211A (en) | 2016-03-30 |
Family
ID=55549931
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510948055.XA Pending CN105439211A (en) | 2015-12-17 | 2015-12-17 | Energy-saving environmental-protection production method for iron oxide black pigment |
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| CN (1) | CN105439211A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107986337A (en) * | 2017-11-03 | 2018-05-04 | 浙江华源颜料股份有限公司 | A kind of easily scattered high coloring power iron oxide black and preparation method thereof |
| CN109850951A (en) * | 2019-04-01 | 2019-06-07 | 中钢集团南京新材料研究院有限公司 | A method of iron oxide black is prepared using titanium white by product object |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1441043A (en) * | 1974-02-21 | 1976-06-30 | Laporte Industries Ltd | Process for the production of iron oxide |
| JPS59102824A (en) * | 1982-11-30 | 1984-06-14 | Dowa Teppun Kogyo Kk | Production of black iron oxide powder |
| CN1807263A (en) * | 2006-02-21 | 2006-07-26 | 上海宝齐氧化铁有限公司 | Method for producing iron oxide black using desilicified mud cake |
| CN101560336A (en) * | 2008-04-18 | 2009-10-21 | 上海宝齐氧化铁有限公司 | Spherical iron oxide black and preparation technology thereof |
-
2015
- 2015-12-17 CN CN201510948055.XA patent/CN105439211A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1441043A (en) * | 1974-02-21 | 1976-06-30 | Laporte Industries Ltd | Process for the production of iron oxide |
| JPS59102824A (en) * | 1982-11-30 | 1984-06-14 | Dowa Teppun Kogyo Kk | Production of black iron oxide powder |
| CN1807263A (en) * | 2006-02-21 | 2006-07-26 | 上海宝齐氧化铁有限公司 | Method for producing iron oxide black using desilicified mud cake |
| CN101560336A (en) * | 2008-04-18 | 2009-10-21 | 上海宝齐氧化铁有限公司 | Spherical iron oxide black and preparation technology thereof |
Non-Patent Citations (1)
| Title |
|---|
| 孙晓庆等: "加成氧化法氧化铁黑合成技术研究", 《广东化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107986337A (en) * | 2017-11-03 | 2018-05-04 | 浙江华源颜料股份有限公司 | A kind of easily scattered high coloring power iron oxide black and preparation method thereof |
| CN107986337B (en) * | 2017-11-03 | 2020-05-05 | 浙江华源颜料股份有限公司 | Easily-dispersible high-tinting-strength iron oxide black and preparation method thereof |
| CN109850951A (en) * | 2019-04-01 | 2019-06-07 | 中钢集团南京新材料研究院有限公司 | A method of iron oxide black is prepared using titanium white by product object |
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Application publication date: 20160330 |