CN104556244A - Method for preparing superfine iron oxide yellow through sodium chlorate oxidation - Google Patents
Method for preparing superfine iron oxide yellow through sodium chlorate oxidation Download PDFInfo
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- CN104556244A CN104556244A CN201410821967.6A CN201410821967A CN104556244A CN 104556244 A CN104556244 A CN 104556244A CN 201410821967 A CN201410821967 A CN 201410821967A CN 104556244 A CN104556244 A CN 104556244A
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- sodium chlorate
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Abstract
The invention discloses a method for preparing superfine iron oxide yellow through sodium chlorate oxidation. The method comprises the following steps: under a stirring condition, dropwise adding sulfuric acid into a FeSO4 solution, adding NaClO3, enabling Fe2+ to be completely oxidized at a constant temperature, raising the temperature, and performing thermostatic reaction to enable the superfluous sodium chlorate to be completely decomposed, diluting by adding water, dropwise adding ammonia water under the stirring condition to obtain brown red colloidal ferric hydroxide, diluting by adding water, stirring, raising the temperature, adding an iron persulfate solution, then adding reduced iron powder, keeping the temperature until the pH value of the slurry is up to a conversion end point, washing until SO4<2-> cannot be detected, adding SDBS into the slurry, keeping the temperature, adding diphenylguanidine, slurrying, filtering, washing, drying and crushing to obtain the superfine iron oxide yellow. The method for preparing superfine iron oxide yellow through sodium chlorate oxidation, disclosed by the invention, is easier in rinsing operation, low in production cost, and low in pollution; the sedimentation filtering performance of the particle can be improved; the agglomeration phenomenon does not exist and monodispersion is good.
Description
Technical field
The invention belongs to pigment technology field, relate to the method that superfine iron oxide Huang is prepared in the oxidation of a kind of sodium chlorate.
Background technology
Iron oxide yellow is also known as iron carbonyl, and be called for short iron oxide yellow, chemical molecular formula is Fe
2o
3h
2o or alpha-feooh, in yellow powder.Superfine iron oxide is yellow has the surface effects of nano material, volume effect and quantum size effect because of its particle diameter little (nano level), performance is better than common iron oxide yellow, have good weathering resistance, photostabilization and its to ultraviolet, there is good absorption and shielding effect.It is mainly used in high-grade automobile finish and woodstain, has a wide range of applications in plastics, rubber, ink and makeup, food, medicine etc. simultaneously.
The preparation method preparing superfine iron oxide Huang is a lot, can be divided into wet method (wet method) and dry method (dry method) generally.Wet method can be divided into oxidation-precipitation method and colloid chemistry methods again.Sodium chlorate oxidation style is the one in oxidation-precipitation method, and this method technique is simple, is easy to industrialization and amplifies, but be mostly sodium hydroxide in high ferro to alkali used in iron glue conversion process.
Summary of the invention
In view of this, a kind of sodium chlorate is the object of the present invention is to provide to be oxidized the method preparing superfine iron oxide Huang.
For achieving the above object, the invention provides following technical scheme:
A method for superfine iron oxide Huang is prepared in sodium chlorate oxidation, comprises the steps:
Under stirring, toward FeSO
4drip sulfuric acid acidation in solution, 50 ~ 60 DEG C add NaClO
3, constant temperature makes Fe
2+oxidation completely, is finally warming up to 80 ~ 90 DEG C, isothermal reaction 2 ~ 3h, and excessive sodium chlorate is decomposed completely, and thin up, drips ammoniacal liquor under stirring, when pH rises to 7.2 ~ 7.4, stops adding, obtains red-brown colloidal iron hydroxide, thin up, make Fe
3+concentration is 0.1 ~ 0.15mol/L, stirs, is warming up to 80 ~ 90 DEG C, adds the ferric sulphate solution that concentration is 0.7 ~ 0.8mol/L, then add reduced iron powder, insulation, and the pH to slurries reaches 3.5 ~ 4.0 for inversion end-point, washing, until inspection does not measure SO
4 2-, add 0.6 ~ 0.8wt%SDBS, at 80 ~ 90 DEG C of insulation 2 ~ 3h, add 30 ~ 50wt% vulkacit D, pulp, filtration, washing, drying, pulverize that to obtain superfine iron oxide yellow.
Preferably, 55 DEG C add NaClO
3, constant temperature makes Fe
2+oxidation completely.
Preferably, be warming up to 85 DEG C, isothermal reaction 2.5h.
Preferably, thin up, makes Fe
3+concentration is 0.12mol/L.
Preferably, be warming up to 85 DEG C, add the ferric sulphate solution that concentration is 0.75mol/L.
Preferably, add 0.7wt%SDBS, at 85 DEG C of insulation 2.5h.
Preferably, add 40wt% vulkacit D, pulp, filtration, washing, drying, pulverize that to obtain superfine iron oxide yellow.
The method of superfine iron oxide Huang is prepared in sodium chlorate oxidation of the present invention, and rising operation ratio is easier to, and production cost low stain is little, and improve the sedimentation filtration performance of particle, soilless sticking phenomenon, monodispersity is good.
Embodiment
Be described in detail to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite not making creative work, all belongs to the scope of protection of the invention.
Embodiment 1
Under stirring, toward FeSO
4drip sulfuric acid acidation in solution, 50 DEG C add NaClO
3, constant temperature makes Fe
2+oxidation completely, is finally warming up to 80 DEG C, isothermal reaction 3h, and excessive sodium chlorate is decomposed completely, and thin up, drips ammoniacal liquor under stirring, when pH rises to 7.2 ~ 7.4, stops adding, obtains red-brown colloidal iron hydroxide, thin up, make Fe
3+concentration is 0.1mol/L, stirs, is warming up to 80 DEG C, adds the ferric sulphate solution that concentration is 0.7mol/L, then add reduced iron powder, insulation, and the pH to slurries reaches 3.5 ~ 4.0 for inversion end-point, washing, until inspection does not measure SO
4 2-, add 0.6wt%SDBS, at 80 DEG C of insulation 3h, add 30wt% vulkacit D, pulp, filtration, washing, drying, pulverize that to obtain superfine iron oxide yellow.
Embodiment 2
Under stirring, toward FeSO
4drip sulfuric acid acidation in solution, 60 DEG C add NaClO
3, constant temperature makes Fe
2+oxidation completely, is finally warming up to 90 DEG C, isothermal reaction 2h, and excessive sodium chlorate is decomposed completely, and thin up, drips ammoniacal liquor under stirring, when pH rises to 7.2 ~ 7.4, stops adding, obtains red-brown colloidal iron hydroxide, thin up, make Fe
3+concentration is 0.15mol/L, stirs, is warming up to 90 DEG C, adds the ferric sulphate solution that concentration is 0.8mol/L, then add reduced iron powder, insulation, and the pH to slurries reaches 3.5 ~ 4.0 for inversion end-point, washing, until inspection does not measure SO
4 2-, add 0.8wt%SDBS, at 90 DEG C of insulation 2h, add 50wt% vulkacit D, pulp, filtration, washing, drying, pulverize that to obtain superfine iron oxide yellow.
Embodiment 3
Under stirring, toward FeSO
4drip sulfuric acid acidation in solution, 55 DEG C add NaClO
3, constant temperature makes Fe
2+oxidation completely, is finally warming up to 85 DEG C, isothermal reaction 2.5h, and excessive sodium chlorate is decomposed completely, and thin up, drips ammoniacal liquor under stirring, when pH rises to 7.2 ~ 7.4, stops adding, obtains red-brown colloidal iron hydroxide, thin up, make Fe
3+concentration is 0.12mol/L, stirs, is warming up to 85 DEG C, adds the ferric sulphate solution that concentration is 0.75mol/L, then add reduced iron powder, insulation, and the pH to slurries reaches 3.5 ~ 4.0 for inversion end-point, washing, until inspection does not measure SO
4 2-, add 0.7wt%SDBS, at 85 DEG C of insulation 2.5h, add 40wt% vulkacit D, pulp, filtration, washing, drying, pulverize that to obtain superfine iron oxide yellow.
In those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (7)
1. a method for superfine iron oxide Huang is prepared in sodium chlorate oxidation, it is characterized in that, comprises the steps:
Under stirring, toward FeSO
4drip sulfuric acid acidation in solution, 50 ~ 60 DEG C add NaClO
3, constant temperature makes Fe
2+oxidation completely, is finally warming up to 80 ~ 90 DEG C, isothermal reaction 2 ~ 3h, and excessive sodium chlorate is decomposed completely, and thin up, drips ammoniacal liquor under stirring, when pH rises to 7.2 ~ 7.4, stops adding, obtains red-brown colloidal iron hydroxide, thin up, make Fe
3+concentration is 0.1 ~ 0.15mol/L, stirs, is warming up to 80 ~ 90 DEG C, adds the ferric sulphate solution that concentration is 0.7 ~ 0.8mol/L, then add reduced iron powder, insulation, and the pH to slurries reaches 3.5 ~ 4.0 for inversion end-point, washing, until inspection does not measure SO
4 2-, add 0.6 ~ 0.8wt%SDBS, at 80 ~ 90 DEG C of insulation 2 ~ 3h, add 30 ~ 50wt% vulkacit D, pulp, filtration, washing, drying, pulverize that to obtain superfine iron oxide yellow.
2. the method for superfine iron oxide Huang is prepared in sodium chlorate oxidation according to claim 1, it is characterized in that: 55 DEG C add NaClO
3, constant temperature makes Fe
2+oxidation completely.
3. the method for superfine iron oxide Huang is prepared in sodium chlorate oxidation according to claim 1, it is characterized in that: be warming up to 85 DEG C, isothermal reaction 2.5h.
4. the method for superfine iron oxide Huang is prepared in sodium chlorate oxidation according to claim 1, it is characterized in that: thin up, makes Fe
3+concentration is 0.12mol/L.
5. the method for superfine iron oxide Huang is prepared in sodium chlorate oxidation according to claim 1, it is characterized in that: be warming up to 85 DEG C, adds the ferric sulphate solution that concentration is 0.75mol/L.
6. the method for superfine iron oxide Huang is prepared in sodium chlorate oxidation according to claim 1, it is characterized in that: add 0.7wt%SDBS, at 85 DEG C of insulation 2.5h.
7. the method for superfine iron oxide Huang is prepared in sodium chlorate according to claim 1 oxidation, it is characterized in that: add 40wt% vulkacit D, pulp, filtration, washing, drying, pulverizes that to obtain superfine iron oxide yellow.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108455681A (en) * | 2018-02-05 | 2018-08-28 | 吉林建筑大学 | A method of preparing iron oxide yellow using iron content, aluminum i ndustry waste water |
| CN116410616A (en) * | 2023-03-03 | 2023-07-11 | 浙江正奇世荣科技有限公司 | Production process of nano ferric oxide pigment |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319099A (en) * | 2008-04-07 | 2008-12-10 | 王建民 | Method for preparing transparent iron oxide pigment with microemulsion method |
-
2014
- 2014-12-26 CN CN201410821967.6A patent/CN104556244A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319099A (en) * | 2008-04-07 | 2008-12-10 | 王建民 | Method for preparing transparent iron oxide pigment with microemulsion method |
Non-Patent Citations (2)
| Title |
|---|
| 肖曙阳等: "纳米氧化铁黄颜料的制备和表征", 《上海大学学报（自然科学版）》 * |
| 黄坚等: "氯酸钠氧化法制备超细氧化铁黄的研究", 《广州化学》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108455681A (en) * | 2018-02-05 | 2018-08-28 | 吉林建筑大学 | A method of preparing iron oxide yellow using iron content, aluminum i ndustry waste water |
| CN116410616A (en) * | 2023-03-03 | 2023-07-11 | 浙江正奇世荣科技有限公司 | Production process of nano ferric oxide pigment |
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Application publication date: 20150429 |